UNIVERSITY OF KHATOUM

FACULTY OF ENGINEERING

CHEMICAL ENGINEERING DEPARTMENT

A PROJECT SUBMITTED IN PARTIAL FULLFILMENT OF THE REQUIREMENTS FOR

THE DEGREE OF B.S.C. (HONORS) IN CHEMICAL ENGINEERING

PRODUCTION OF PHENOL FROM CUMENE

Submitted by:
Bashayer Suliman Abass 142016

Essra Rabei Omer 142008

Mohamed Merghani Mohamedgaili 132045

SUPERVISED BY:

Dr. Bashir Mohamed Alhassan

OCTOBER 2020
 ||PHENOL

Word of wisdom
If at first you don’t succeed,
Try..
Try..
and try again.

II
 ||PHENOL

Dedication
It is our genuine gratefulness and warmest regard
that we dedicate this work to our beloved parents,
Who educated us and enabled us to reach at this
level.

To all of people that we love and respect and

helped us, we are very thankful to all the people
who supported us with their attitude and
unlimited help.

III
 ||PHENOL

Acknowledgement
Firstly, we thank Allah almighty for His blessings and for
providing us with the strength and power to succeed.

Independently on the nature of their contribution (intellectual

or/and emotional), many people have pushed toward the
completion of this work. To all of them we are deeply and
sincerely indebted.

Our words of thanks go to our supervisor Dr. Bashir Mohamed

Alhassan; we thank him for his continuous guidance, unlimited
support, grateful efforts, continuous encouragement and
scientific insight during this project.

We would like to thank also to Eng. Omnia Babiker Hassan and

Eng. Sidig Mohamed for their continuous strong support and
knowledge.

Finally, we would like to thank all the people who supported our
project. Foremost have been our families who encouraged us to
work hard and to continue this work and our colleagues for their
kindness and support.

IV
 ‫‪||PHENOL‬‬

‫المستخلص‬
‫يحتوي هذا التقرير على تصميم عملية إلنتاج الفينول من الكيومين بنا ًء على التجارب المعملية واألبحاث‬
‫العلمية‪ .‬يصف طريقة إلنتاج الفينول باستخدام أكسدة وانقسام الكيومين ‪ ،‬بمعدل إنتاج للفينول ‪ 252‬مليون رطل‬
‫سنويًا (‪ 126‬ألف طن سنويًا) مع األسيتون و الوقود كمنتجات ثانوية لعملية التصنيع‪.‬‬

‫عا بالتحلل‬
‫يتأكسد الكيومين باألكسجين (من الهواء) لتكوين هيدروبيروكسيد الكيومين )‪ ، (CHP‬متبو ً‬
‫المحفز بالحمض (االنقسام) لـ ‪ CHP‬إلى الفينول واألسيتون‪ .‬يتم بعد ذلك تقطير الفينول واألسيتون والكيومين‬
‫غير المحول والمنتجات الثانوية في سلسلة من أبراج التقطير الستعادة الفينول عالي النقاء (‪ )٪98‬ومنتجات‬
‫األسيتون واستعادة الكيومين إلعادة تدويره للتفاعل‪.‬‬

‫تم استخدام طريقتين في هذه الدراسة ؛ الحسابات اليدوية المعتمدة على مراجع الهندسة الكيميائية والميكانيكية‬
‫كطريقة أولى ‪ ،‬وبرامج المحاكاة‪ "Aspen HYSYS v10".‬كطريقة ثانية‪.‬‬

‫اجريت موازنات المادة والطاقة وتكامل الحرارة على العملية‪ ,‬كما تم تصميم كل االجهزة الرئيسية واالجهزة‬
‫الملحقة تصميما تفصيليا‪ .‬باإلضافة الى دراسات تتضمن اجراءات السالمة الالزمة وتطوير نظام تحكم لكل‬
‫واقتصاديا‪.‬‬ ‫عمليا‬ ‫المشروع‬ ‫هذا‬ ‫تطبيق‬ ‫قابلية‬ ‫من‬ ‫للتحقق‬ ‫وذلك‬ ‫جهاز‬
‫استثمارا رأسماليًا قدره ‪ 13.7‬مليون دوالر أمريكي بمعدل عائد داخلي ‪ 31‬بالمائة وعائد‬‫ً‬ ‫يتطلب المصنع‬
‫استثمار بنسبة ‪ 31.91‬بالمائة‪.‬‬

‫قد تأخذ الدولة صناعة الفينول في االعتبار باستخدام عملية الكيومين التي تعطي إنتاجية عالية ‪ ،‬ونقاء المنتج ‪،‬‬
‫واألسيتون كمنتج ثانوي ومنتج ثانوي أخر أال وهو الوقود الذي يمكن استخدامه في توليد الطاقة‪.‬‬

‫‪V‬‬
 ||PHENOL

Abstract
This report contains a process design for production of phenol from Cumene based on
laboratories experiments and scientific researches. It describes a method to produce phenol using
a oxidation and cleavage of Cumene. Acetone and fuel is a byproducts of this manufacturing
process. The resulting design produces the desired 252 million pounds per year (126 thousand tons
per year) of phenol. Cumene is oxidized with oxygen (from air) to form Cumene Hydroperoxide
(CHP), followed by acid-catalyzed decomposition (cleavage) of CHP to phenol and acetone.
Phenol, acetone, unconverted Cumene, and by-products are then distilled in a series of distillation
towers to recover high purity phenol (98%) and acetone products and to recover Cumene to be
recycled to reaction.

Two methods were used in this plant study; hand calculations based on chemical and
mechanical engineering references and simulation software “Aspen HYSYS v10”.

Material and energy balances, heat integration, Detailed design for all of the major equipment
and the ancillary equipment, HAZOP studies and basic control schemes; all were conducted in
order to verify the economic feasibility of the project.

The plant requires a capital investment of 13.7 million USD with an internal rate of return of
31 percent and return on investment of 31.91 percent.

The country may take the phenol industry in consideration using Cumene process that gives
high yields, purities of the product, acetone as byproduct and fuel byproduct that can be used
in energy generation.

VI
 ||PHENOL

Table of Contents
Word of wisdom .......................................................................................................... II
Dedication .................................................................................................................. III
Acknowledgement ..................................................................................................... IV
Abstract in Arabic....................................................................................................... V
Abstract ...................................................................................................................... VI
Table of Contents ..................................................................................................... VII
List of Tables ............................................................................................................ XII
List of Figures ......................................................................................................... XVI
Chapter 1: Introduction and Literature review ............................................... 1
Introduction .................................................................................................... 1
Literature review ............................................................................................ 2
Sources of phenol........................................................................ 3
Physical properties ...................................................................... 4
Reactions of phenol .................................................................... 4
Effects of phenol ......................................................................... 5
Uses of phenol ............................................................................ 7
Production of phenol ................................................................... 7
References ................................................................................................................. 12
Chapter 2: Process Description ........................................................................ 13
Brief Description .......................................................................................... 13
Detailed Description .................................................................................... 14
Liquid Phase Cumene Oxidation .............................................. 14
Acid-Cleavage .......................................................................... 14
Separation ................................................................................. 15
Hydrogenation of AMS ............................................................ 15
References ................................................................................................................. 16
Chapter 3: Materials balance ........................................................................... 17
Introduction .................................................................................................. 17
General balance equation .......................................................... 17
Reactor (1) – Oxidation Reactor .................................................................. 18
Chemical Reactions .................................................................. 18
Assumptions.............................................................................. 18
Material Balance ....................................................................... 19
Reactor (2) - Cleavage Unit ......................................................................... 20
Chemical Reactions .................................................................. 20
Assumptions.............................................................................. 20
Material Balance ....................................................................... 21
Distillation Unit 1: Acetone separation........................................................ 22
Assumptions.............................................................................. 22
Material Balance ....................................................................... 23
Distillation Unit 2: cumene separation ........................................................ 24
Assumptions.............................................................................. 24
Material Balance ....................................................................... 25
Distillation Unit 3: AMS separation ............................................................ 26
Assumptions.............................................................................. 26

VII
 ||PHENOL

Material Balance ....................................................................... 27

Distillation Unit 4: phenol separation .......................................................... 28
Assumptions.............................................................................. 28
Material Balance ....................................................................... 29
Reactor 3 – Pre - Purification Reactor ......................................................... 30
Chemical Reaction Involved In Pre – Purification Reactor ...... 30
Material Balance ....................................................................... 31
Mixer 1 ......................................................................................................... 32
Material Balance ....................................................................... 32
Mixer 2 ......................................................................................................... 33
Material Balance ..................................................................... 33
Overall Material Balance ............................................................................. 34
Material Balance ..................................................................... 34
References ................................................................................................................. 35
Chapter 4: Energy Balance .............................................................................. 36
Introduction .................................................................................................. 36
Energy balance fundamentals ...................................................................... 36
Calculation of specific enthalpy (H) ............................................................ 36
Equipment energy balance ........................................................................... 38
Mixer M-(101): ......................................................................... 38
Mixer M-(102): ......................................................................... 39
Heater E-(101): ......................................................................... 40
Reactor R-(101): ....................................................................... 41
Cooler E-(102): ......................................................................... 43
Reactor R-(102): ....................................................................... 44
Heater E-(103): ......................................................................... 46
Distillation column T-(101): ..................................................... 47
Distillation column T-(102): ..................................................... 48
Distillation column T-(103): ................................................... 50
Distillation column T-(104): ................................................... 52
Reactor R-(103): ..................................................................... 54
References ................................................................................................................. 56
Chapter 5: Heat Integration ............................................................................. 57
Introduction .................................................................................................. 57
Minimum utility targets using the algebraic cascade diagram..................... 58
Cascade diagram: ...................................................................... 61
Revised cascade diagram: ......................................................... 62
Stream matching and synthesis of heat-exchange networks ........................ 62
Stream population rules ............................................................ 62
LINGO Code............................................................................. 64
Matlab code............................................................................... 68
References ................................................................................................................. 70
Chapter Six: Equipment Design ...................................................................... 71
Bubble Column Reactor ............................................................................... 71
Introduction ............................................................................... 71
Fluid-Fluid Reactors ................................................................. 73

VIII
 ||PHENOL

Bubble Column Reactor............................................................ 74

Cleavage reactor design ............................................................................... 82
Introduction ............................................................................... 82
Stirred tank reactors .................................................................. 82
Continuous stirred tank reactor design ..................................... 84
Hydrogenation Reactor ................................................................................ 91
Assumptions.............................................................................. 91
Reaction kinetics: ...................................................................... 91
Reactor’s volume ...................................................................... 91
Acetone distillation column ......................................................................... 92
Introduction ............................................................................... 92
Step 1: Product specifications ................................................... 93
Step 2: Selection of operating conditions ................................. 93
Step 3: Selection of the contacting device ................................ 96
Step 4: Determination of the stage and reflux requirements .... 97
Step 5: Column sizing ............................................................. 105
Step 6: Detailed column sizing and internals design .............. 109
Step 7: Mechanical design of Acetone distillation column .... 127
Checking the buckling pressure: ...................................................................... 131
Cumene Distillation ................................................................................... 135
AMS Distillation ........................................................................................ 142
Phenol Distillation ..................................................................................... 148
References ............................................................................................................... 153
Chapter 7: Ancillaries Design ........................................................................ 154
Mixing and storage facilities ...................................................................... 154
Sizing of storage and mixing tanks ......................................... 154
Cumene storage tank ............................................................... 155
Acetone storage tank ............................................................... 156
Phenol storage tank ................................................................. 156
Cumene mixing tank 1 ............................................................ 157
Cumene mixing tank 2 ............................................................ 157
Heat exchangers ......................................................................................... 158
Introduction ............................................................................. 158
Heat Exchanger 1 (E-101) ...................................................... 166
Cooler 1 (E- 102) .................................................................... 172
Boiler 1 (E- 103) ..................................................................... 173
Heat Exchanger 2 (E- 104) ..................................................... 174
Boiler 2 (E- 105) ..................................................................... 176
Pumps......................................................................................................... 176
Pump Selection ....................................................................... 176
Power requirement ............................................................................................. 177
Pump P-101 (Cumene)............................................................ 179
Pump P-102 (Cleavage) .......................................................... 179
Compressor ................................................................................................ 179
Centrifugal compressor (C-101) ............................................. 180
References .............................................................................................................. 182

IX
 ||PHENOL

Chapter 8: Process Simulation ....................................................................... 183

Building the Simulation ............................................................................. 183
Part (1): .................................................................................. 185
Part (2): .................................................................................. 187
Comments ................................................................................................. 188
Equipment Work .................................................................. 188
Chapter 9: Process Control ............................................................................ 189
Introduction ................................................................................................ 189
Importance and objectives of control.................................. 189
Process control terms............................................................ 189
Control loop .............................................................................................. 189
Controlled process variables ................................................................... 189
Input Variable .......................................................................................... 190
Output variable........................................................................................... 190
Types of Instrument ................................................................................... 190
Line and function symbols ......................................................................... 191
Types of Controllers' Actions .................................................................... 191
Process equipment control ......................................................................... 192
Heaters control E (102) ........................................................... 192
E (105) .................................................................................... 193
Coolers control E (102)........................................................... 194
Control of heat exchangers E (101) ........................................ 195
E (104) .................................................................................... 195
Control of reactors R (101), R (102), R (103) ........................ 196
Control of distillation columns T (101), T (102), T (103), T (104) 199
References ............................................................................................................... 207
Chapter 10: Safety, Health and Environment ............................................. 208
Safety ......................................................................................................... 208
Hazard Introduction .............................................................. 208
Handling and Storage of Hazardous Chemical: .................... 208
Hazard and Operability Studies (HAZOP) ........................... 210
Health ......................................................................................................... 214
Effect to Human .................................................................... 214
Effect to Environment ................................................................................ 216
References ............................................................................................................... 218
Chapter 11 : Plant location and layout .......................................................... 219
Introduction ................................................................................................ 219
Plant Location and Site Selection .............................................................. 219
Marketing Area ..................................................................... 219
Raw materials ....................................................................... 219
Transport ............................................................................... 220
Availability of labor .............................................................. 220
Utilities (services) ................................................................. 220
Environmental impact and effluent disposal: ....................... 221
Local community considerations: ......................................... 221
Availability of suitable land .................................................. 221

X
 ||PHENOL

Climate .................................................................................. 221

Political and strategic considerations:................................. 221
Site Layout ................................................................................................. 222
Plant Layout ............................................................................................... 223
Economic considerations: construction and operating costs 223
Process requirements ............................................................ 223
Operation .............................................................................. 223
Maintenance .......................................................................... 223
Safety .................................................................................... 223
Plant expansion ..................................................................... 224
Modular construction ............................................................ 224
Other services ....................................................................... 224
General considerations .......................................................... 224
Phenol plant layout: ................................................................................... 225
References: .............................................................................................................. 227
Chapter 12: Cost and Economical Evaluation.............................................. 228
Introduction [1] ............................................................................................ 228
The specifications of plant ......................................................................... 228
Cost estimation........................................................................................... 229
Methods used in capital estimation:...................................... 229
Cost estimation by Capcost: ................................................. 230
Cost Estimation by hand calculation (Excel sheet): [2] ......... 235
Project evaluation....................................................................................... 241
Net present value of the plant ............................................... 241
Internal Rate of Return (IRR) ............................................... 242
Profitability Index: ................................................................ 242
Payback period:..................................................................... 242
Accounting rate of return: ..................................................... 242
Cost of labor: ........................................................................ 243
References: .............................................................................................................. 245
Chapter 13: Equipment Specification Sheets ............................................... 246
Chapter 14: Conclusion and Recommendation ............................................ 260
Conclusion ................................................................................................. 260
Recommendation ....................................................................................... 261
Appendix A. Estimation of Physical Properties .................................................... 262
A.1 Acetone distillation column T-(101) ................................................................ 262
A.1.1 Dynamic viscosity ...................................................................................... 262
A.1.2 Gas density ................................................................................................. 263
A.1.3 Liquid density ............................................................................................. 264
A.2 Energy balance ................................................................................................. 267
A.2.1 Heat capacity .............................................................................................. 267
Appendix B. Economic indicators (CEPCI) .......................................................... 270
Appendix C. MSDA ................................................................................................. 271

XI
 ||PHENOL

List of Tables
[3]
Table 1-1:Physical Properties of Phenol ...................................................................................... 4
Table 1-2: The Toxic Effects on Humans, Animals and Fish [5]..................................................... 5
Table 1-3:Annual Production of Phenol[4] ...................................................................................... 7
Table 1-4:Compositions of Products[1] ........................................................................................... 8
Table 1-5:Summery to all the Above Methods[1] .......................................................................... 11
Table 3-1:Component’s molar flow and Composition of R-(101). .............................................. 19
Table 3-2:Component’s molar flow and Composition of R-(102). .............................................. 21
Table 3-3:Component’s molar flow and Composition of T-(101) ................................................ 23
Table 3-4:Component’s molar flow and Composition of T-(102). ............................................... 25
Table 3-5:Component’s molar flow and Composition of T-(103). ............................................... 27
Table 3-6:Component’s molar flow and Composition of T-(104). ............................................... 29
Table 3-7:Component’s molar flow and Composition of R-(103). .............................................. 31
Table 3-8:Component’s molar flow and Composition of M-(101)............................................... 32
Table 3-9:Component’s molar flow and Composition of M-(102)............................................... 33
Table 4-1:Component’s molar flow, enthalpy and temperature of M-(101). ............................... 38
Table 4-2:Component’s molar flow, enthalpy and temperature of M-(102). ............................... 39
Table 4-3: Component’s molar flow, enthalpy and temperature of E-(101). ............................... 40
Table 4-4:Component’s molar flow, enthalpy and temperature of R-(101). ................................ 42
Table 4-5:Component’s molar flow, enthalpy and temperature of E-(102). ................................ 43
Table 4-6: Component’s molar flow, enthalpy and temperature of R-(102). .............................. 45
Table 4-7: Component’s molar flow, enthalpy and temperature of E-(103). ............................... 46
Table 4-8:Component’s molar flow, enthalpy and temperature of T-(101). ................................ 47
Table 4-9:Q of T-(101). ................................................................................................................ 48
Table 4-10:Component’s molar flow, enthalpy and temperature of T-(102). .............................. 49
Table 4-11:Q of T-(102). .............................................................................................................. 50
Table 4-12:Component’s molar flow, enthalpy and temperature of T-(103). .............................. 51
Table 4-13:Q of T-(103). .............................................................................................................. 52
Table 4-14:Component’s molar flow, enthalpy and temperature of T-(104). .............................. 53
Table 4-15:Q of T-(104). .............................................................................................................. 54
Table 4-16:Component’s molar flow, enthalpy and temperature of R-(103). .............................. 55
Table 5-1:Heat integration calculations ........................................................................................ 59
Table 5-2: Temperature -interval diagram. ................................................................................... 59
Table 5-3:TEHL for hot streams. .................................................................................................. 60
Table 5-4:TEHL for cold streams. ................................................................................................ 60
Table 6-1 : properties of reactor inlet............................................................................................ 76
Table 6-2: specification sheet ....................................................................................................... 81
Table 6-3 : Typical design stresses for plate thickness.. ............................................................... 86
Table 6-4 : Design summary for R-(102)...................................................................................... 89
Table 6-5: Product specifications. ................................................................................................. 93
Table 6-6 : Initial compositions and molar flow rates of the product streams.............................. 98

XII
 ||PHENOL

Table 6-7: Dew point (top temperature). ...................................................................................... 99

Table 6-8: Bubble point (bottom temperature). .......................................................................... 100
Table 6-9: Relative volatilities. ................................................................................................... 100
Table 6-10: Feed compositions. .................................................................................................. 102
Table 6-11:Flash calculation results ........................................................................................... 102
Table 6-12 : Summary on conceptual design calculations. ........................................................ 105
Table 6-13: other ratios of active area corrections .................................................................... 111
Table 6-14:Plate specifications. .................................................................................................. 127
Table 6-15:Design stress factors. ................................................................................................ 129
Table 6-16:Provisional plate design specification. ..................................................................... 134
Table 6-17:Mechanical design of plate column. ......................................................................... 135
Table 6-18:Design summery for Cumene distillation column. ................................................... 135
Table 6-19: Design summery for AMS distillation column. ...................................................... 142
Table 6-20 :. Design summery for Phenol distillation column. .................................................. 148
Table 7-1:Nominal capacities of standard vertical cylindrical tanks, m3. .................................. 155
Table 7-2: Constants used in equation (7.13). ............................................................................ 163
Table 7-3: Physical properties for liquid mixture in shell-side. .................................................. 167
Table 7-4:Physical properties for liquid mixture in tube-side. ................................................... 167
Table 7-5: Design summary for E-(101). .................................................................................... 171
Table 7-6: Design summary for E-(102). .................................................................................... 172
Table 7-7:Design summary for E-(103). ..................................................................................... 173
Table 7-8: Design summary for E-(104). .................................................................................... 174
Table 7-9:Design summary for E-(105). ..................................................................................... 176
Table 8-1:Comparison between simulation and hand calculation ............................................. 185
Table 8-2: Comparison between simulation and hand calculation ............................................ 187
Table 9-1:Types of controllers suitable for the common variables. ........................................... 190
Table 9-2:Symbols used in P&IDs.............................................................................................. 191
Table 9-3:Basic features of control actions. ................................................................................ 192
Table 9-4:Elements of control loop for heater temperature. ....................................................... 192
Table 9-5: Elements of control loop for heater temperature. ...................................................... 193
Table 9-6:Elements of control loop for cooler temperature. ....................................................... 194
Table 9-7: Elements of control loop for heat exchangers temperature. ...................................... 196
Table 9-8:Elements of control loop for reactor temperature....................................................... 197
Table 9-9: Elements of control loop for reactor pressure. .......................................................... 198
Table 9-10:Elements of control loop for distillations pressure. .................................................. 200
Table 9-11:Elements of control loop for distillations temperature. ............................................ 202
Table 9-12:Elements of control loop for distillations drum level. .............................................. 203
Table 9-13: Elements of control loop for distillations base level. .............................................. 204
Table 10-1:A List of Guide Words and Their Meaning.............................................................. 211
Table 10-2: Compressor HAZOP ............................................................................................... 212
Table 10-3: Reactor HAZOP ...................................................................................................... 212
Table 10-4: Cooler HAZOP ........................................................................................................ 213

XIII
 ||PHENOL

Table 10-5: Distillation HAZOP ................................................................................................. 214

Table 12-1:Materials prices. ....................................................................................................... 229
Table 12-2: List of equipments. .................................................................................................. 234
Table 12-3: List of utilities costs................................................................................................. 235
Table 12-4:Direct cost ................................................................................................................. 238
Table 12-5:Indirect cost .............................................................................................................. 239
Table 12-6:Working capital ........................................................................................................ 239
Table 12-7:Manufacturing cost. .................................................................................................. 240
Table 12-8:General expenses ...................................................................................................... 241
Table 12-9:Detailed about direct production cost. ...................................................................... 241
Table 13-1: Pump -101 Specification sheet ................................................................................ 246
Table 13-2:Pump -102 Specification sheet ................................................................................. 246
Table 13-3: E-101 Specification sheet ........................................................................................ 247
Table 13-4: E-102 Specification sheet ........................................................................................ 247
Table 13-5: E-103 Specification sheet ........................................................................................ 248
Table 13-6:E-104 Specification sheet ......................................................................................... 248
Table 13-7:E-105 Specification sheet ......................................................................................... 249
Table 13-8:R-101 Specification sheet ......................................................................................... 250
Table 13-9:R-102 Specification sheet ......................................................................................... 251
Table 13-10:R-103 Specification sheet ....................................................................................... 252
Table 13-11:T-101 Specification sheet ....................................................................................... 253
Table 13-12:T-102 Specification sheet ....................................................................................... 254
Table 13-13:T-103 Specification sheet. ...................................................................................... 255
Table 13-14:T-104 Specification sheet. ...................................................................................... 256
Table 13-15:Compressor -101 Specification sheet. .................................................................... 257
Table 13-16:Cumene storage tank TK-(101). ............................................................................. 257
Table 13-17:Acetone storage tank TK-(102). ............................................................................. 258
Table 13-18:phenol storage tank TK-(103). ............................................................................... 258
Table 13-19:Cumene mixing tank MIX-(101). ........................................................................... 259
Table 13-20:Cumene mixing tank MIX-(102). ........................................................................... 259
Table A-1:Regression coefficients for viscosity calculations. .................................................... 262
Table A-2: Estimation of viscosity of benzene distillation column T-(101) feed. ..................... 262
Table A-3: Data needed for gas density estimation. ................................................................... 263
Table A-4: Gas density estimation on top of T-(101). ................................................................ 263
Table A-5: Gas density estimation on bottom of T-(101). .......................................................... 264
Table A-6: Data needed for liquid density estimation. ............................................................... 265
Table A-7:Liquid density estimation on top of T-(101). ............................................................ 265
Table A-8: Liquid density estimation on bottom of T-(101). ..................................................... 266
Table A-9: Estimation of surface tension on top and bottom of T-(101). .................................. 266
Table A-10: Heat capacity constants for gases. .......................................................................... 267
Table A-11: Heat capacity constants for liquids. ........................................................................ 268
Table A-12: Vapor pressure constants. ....................................................................................... 268

XIV
 ||PHENOL

Table A-13: Components’ formulas and molecular weights. ..................................................... 269

XV
 ||PHENOL

List of Figures
Figure 1-1: Phenol chemical structure and its 3D conformer [3,1] ................................................... 1
Figure 1-2:Sources of Phenol[5]....................................................................................................... 3
Figure 1-3:Uses of Phenol[4] ........................................................................................................... 7
Figure 2-1: Production of phenol from cumene block diagram .................................................... 13
Figure 2-2: Production of phenol from cumene flow sheet .......................................................... 15
Figure 4-1:Mixer M-(101) ............................................................................................................ 38
Figure 4-2:Mixer M-(102) ............................................................................................................ 39
Figure 4-3:Heater E-(101) ............................................................................................................. 40
Figure 4-4: Reactor R-(101) .......................................................................................................... 41
Figure 4-5:Cooler E-(102) ............................................................................................................ 43
Figure 4-6:Reactor R-(102) ........................................................................................................... 44
Figure 4-7: Heater E-(103) ............................................................................................................ 46
Figure 4-8:Distillation column T-(101) ........................................................................................ 47
Figure 4-9:Distillation column T-(102) ........................................................................................ 48
Figure 4-10:Distillation column T-(103) ...................................................................................... 50
Figure 4-11:Distillation column T-(104) ..................................................................................... 52
Figure 4-12:Reactor R-(103) ......................................................................................................... 54
Figure 5-1: Synthesis of HENs ..................................................................................................... 57
Figure 5-2: Cascade diagram of the phenol process. .................................................................... 61
Figure 5-3: Revised cascade diagram of the phenol process. ....................................................... 62
Figure 5-4 : Stream matching above the pinch. ........................................................................... 63
Figure 5-5 : Stream matching below the pinch. ............................................................................ 63
Figure 6-1: Information needed to predict what a reactor can do.(1) ........................................... 71
Figure 6-2:Broad classification of reactor types. (a) The batch reactor. (b) The steady-state flow
reactor. (c), (d), and (e) Various forms of the semibatch reactor. (1) ........................................... 72
Figure 6-3: Material balance for an element of volume of the reactor. (1)................................... 72
Figure 6-4: Energy balance for an element of volume of the reactor. (1)..................................... 73
Figure 6-5: Tower and tank contactors for G/L reactions. (1) ...................................................... 74
Figure 6-6: Scheme of a bubble column (5) ................................................................................ 75
Figure 6-7 : Porous plate sparger. (4) ........................................................................................... 79
Figure 6-8 : Design stress chart (3) ............................................................................................... 80
Figure 6-9 : CSTR ......................................................................................................................... 83
Figure 6-10 : Distillation column. ................................................................................................. 94
Figure 6-11: Plate contractors. .................................................................................................... 107
Figure 6-12: Flooding velocity, sieve plates. .............................................................................. 110
Figure 6-13: Liquid flow pattern on cross-flow tray. .................................................................. 112
Figure 6-14: Selection of liquid-flow arrangement..................................................................... 113
Figure 6-15:The relation between downcomer area and weir length. ......................................... 114
Figure 6-16:Weep-point correlation............................................................................................ 117

XVI
 ||PHENOL

Figure 6-17:Discharge coefficient, sieve plates. ......................................................................... 119

Figure 6-18: Downcomer backup. .............................................................................................. 120
Figure 6-19:Entrainment correlation for sieve plates. ................................................................ 123
Figure 6-20:Typical sectional plate construction. ....................................................................... 124
Figure 6-21:Segment (chord) downcomer designs. .................................................................... 125
Figure 6-22:Relation between hole area and pitch. ..................................................................... 126
Figure 6-23: Collapse coefficient for cylindrical shells. ............................................................. 131
Figure 7-1:Temperature correction factor: one shell pass; two or more even tube passes. ........ 160
Figure 7-2: Tube-side heat transfer factor. .................................................................................. 161
Figure 7-3:Tube-side friction factors. ......................................................................................... 162
Figure 7-4: Shell-bundle clearance. ............................................................................................ 163
Figure 7-5: Shell-side heat transfer factor................................................................................... 165
Figure 7-6:Shell-side friction factors. ......................................................................................... 166
Figure 7-7: Centrifugal pump selection guide. *Single-stage >1750 rpm, multi-stage 1750 rpm(1)
..................................................................................................................................................... 177
Figure 7-8:Centrifugal pump efficiency ..................................................................................... 178
Figure 7-9:Compressor coverage chart based on the normal range of operation of commercially
available types shown. Solid lines: use left ordinate, head. Broken lines: use right ordinate,
pressure. To convert cubic feet per minute to cubic meters per hour, multiply ......................... 180
Figure 8-1:PFD in hysys for phenol production process ............................................................ 184
Figure 9-1:Different types of lines .............................................................................................. 191
Figure 9-2:Heater temperature control loop. ............................................................................... 193
Figure 9-3:Heater temperature control loop. ............................................................................... 194
Figure 9-4:cooler temperature control loop. ............................................................................... 195
Figure 9-5:Heat exchangers temperature control loop. ............................................................... 196
Figure 9-6:reactors temperature control loop,(a)oxidation tower,(b)cleavage
reactor,(c)hydrogenation reactor . .............................................................................................. 198
Figure 9-7:Reactors pressure control loop,(a)oxidation tower,(b)cleavage reactor,(c)hydrogenation
reactor . ...................................................................................................................................... 199
Figure 9-8:Distillation column pressure control loop. ................................................................ 201
Figure 9-9:Distillation column temperature control loop. .......................................................... 202
Figure 9-10:Distillation column drum level control loop. .......................................................... 203
Figure 9-11:Distillation column base level control loop. ........................................................... 205
Figure 9-12:Distillation column control loop. ............................................................................ 205
Figure 9-13:PID. ......................................................................................................................... 206
Figure 11-1:Plant layout.............................................................................................................. 226
Figure 12-1:cash flow diagram. .................................................................................................. 244
Figure B-1:Economic Indicators ................................................................................................. 270

XVII
||PHENOL

XVIII
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

Chapter 1: Introduction and Literature review

Introduction
Phenol is an aromatic organic compound with the molecular formula C6H5OH and with the
chemical structure and its 3D conformer shown in figure (1.1).It also has other names : Carbolic
acid Benzenol , Phenylic acid , Hydroxybenzene and Phenic acid and more other names. It is a
toxic, colourless crystalline solid with a sweet tarry odor that resembles a hospital smell. [3]

Figure 1-1: Phenol chemical structure and its 3D conformer [3,1]

The word phenol is also used to refer to any compound that contains a six-membered aromatic
ring, bonded directly to a hydroxyl group (-OH). Thus, phenols are a class of organic compounds
of which the phenol discussed in this article is the simplest member. It is mildly acidic and requires
careful handling due to its propensity to cause chemical burns.[6]
Phenol can be found in areas with high levels of motor traffic, therefore, people living in
crowded urban areas are frequently exposed to traffic-derived phenol vapor. The average (mean
+/- SD) phenol concentration in urine among normal individuals living in urban areas is 7.4 +/- 2.2
mg/g of creatinine. Exposure of the skin to concentrated phenol solutions causes chemical burns
which may be severe; in laboratories where it is used, it is usually recommended that polyethylene
glycol solution is kept available for washing off splashes. Notwithstanding the effects of
concentrated solutions, it is also used in cosmetic surgery as an exfoliant, to remove layers of dead
skin. In some bacteria phenol can be directly synthesized from tyrosine via the enzyme tyrosine
phenollyase. [3]
Phenol was first extracted from coal tar, but today is produced on a large amounts from
petroleum. Phenol is a key chemical intermediate utilized in the production of many compounds
and materials such as bisphenol-A and phenolic resins. It is commonly used as an antiseptic and
disinfectant. It is active against a wide range of micro-organisms including some fungi and viruses,
but is only slowly effective against spores. It has been used to disinfect skin and to relieve itching.
Phenol is also used in the preparation of cosmetics including sunscreens hair dyes, and skin
lightening preparations. It is also used in the production of drugs (it is the starting material in the
industrial production of aspirin), weed killers, and synthetic resins. [3] Because of its versatility and
importance to a variety of applications, phenol is in high demand. Phenol and its chemical
derivatives are also essential for production of polycarbonates, epoxies, Bakelite, nylon,
detergents, herbicides such as phenoxy herbicide and numerous pharmaceutical drugs.[6]

1
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

The global phenolic industry has undergone some key changes over the last few years. During
2012-17, a very large amount of phenol capacity was brought online in Asia and the
Middle East, resulting in decreased operating rates and an oversupplied market. The United States
of America currently produces approximately 3.2 million tons of phenol per year. The strongest
consumption growth is in Northeast Asia, especially China. Growth in North America and Western
Europe is either stagnant or low, while growth in South America will be strong, but from a small
base.

The Middle East will have strong consumption growth, driven by production of BPA, which is
being produced primarily for export to other regions.[6,2]
Phenol was discovered in 1834 by Friedlieb Ferdinand Runge, who extracted it (in impure form)
from coal tar. Runge called phenol "Karbolsäure" (coal-oil-acid, carbolic acid). Coal tar remained
the primary source until the development of the petrochemical industry. In 1841, the French
chemist Auguste Laurent obtained phenol in pure form.
Auguste Laurent coined the name "phène" for benzene this is the root of the word "phenol" and
"phenyl". In 1843, French chemist Charles Gerhardt coined the name "phénol".
Since the 1840s, phenol became a subject of numerous studies. Victor Meyer studied
desoxybenzoin, benzyl cyanide and phenyl-substituted methylene groups and showed that they
have similar reactivities. He subsequently published a paper on ‘the negative nature of the phenyl
group’, where he noted how phenyl together with other ‘negative groups’ can make the hydrogen
atoms in methylene groups more reactive. In 1867, Heinrich von Brunck defended his Ph.D. thesis
in Tübingen under Adolph Friedrich Ludwig Strecker and Wilhelm
Staedel on the theme ‘About Derivatives of Phenol’, where he particularly studied the isomers of
nitrophenol.
The Raschig–Dow process of manufacturing phenol by cumene was discovered by Wurtz and
Kekule in 1867, although the earlier synthesis was recorded by Hunt in 1849. Interestingly,
Friedrich Raschig, working earlier as a chemist at BASF and known for his work on the synthesis
of phenol and production of phenol formaldehyde adduct, later established his own company in
Ludwigshafen. It is also interesting to mention in this regard that in 1905, the BAAS subcommittee
on ‘dynamic isomerism’ was established and included Armstrong (chairman), Lowry(secretary)
and Lapworth. In the 1909 report, Lowry summarized that one of the types of isomerism involves
the ‘oscillatory transference’ of the hydrogen atom from carbon to oxygen, as in ethyl acetoacetate
(acetoacetic ester), or from oxygen to nitrogen, as in isatin, or from one oxygen atom to the other
one, as in paranitrosophenol.[7]

Literature review
Phenol and its higher homologues are aromatic molecules containing hydroxyl, methyl, amide
or sulphonic groups attached to the benzenoid ring structure. The origin of phenol in the
environment is both industrial and natural. Natural sources include forest fires, natural run off from
urban area where asphalt is used as binding material and natural decay of lignocellulosic material.
Phenol is one among the most prevalent forms of chemical pollutants, because it is toxic even at
low concentrations, and also its presence in natural waters can lead further to the formation of
substituted compounds during disinfection and oxidation processes. It is an important industrial
chemical of environmental concern widely used in many industries such as coke, refineries,

2
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

manufacturers of resin, pharmaceuticals, pesticides, dyes, plastics, explosives and herbicides, and
can also occur in their wastewaters (Lenke et al 1992, Marvin-Sikkema and de Bont 1994, Yang
et al 1998). Phenols are the dominant organic contaminants in wastewater from coal conversion
and coal coking processes, and they generally comprise 40- 80% of the chemical oxygen demand
(COD) (Giabbai et al 1985). Phenols are produced in very large quantities for use as solvents, and
starting materials for chemical synthesis (Budavari 1996).[5]
Sources of phenol
The origin of phenol in the environment is from natural, man-made and endogenous sour- ces.
Phenol is released primarily to the air and water as a result of its manufacture and use, wood
burning and auto exhaust. Phenol mainly enters waters from industrial effluent discharges. Phenol
is a monohydroxy derivative of benzene and the substituents with chloro, nitro, methyl etc., are
named as derivatives of phenols or collectively as phenolics in wastewater The sources of phenol
in the environment are shown in Figure (1.2)[5]:

Figure 1-2:Sources of Phenol[5]

3
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

Physical properties
Table 1-1:Physical Properties of Phenol[3]

Properties Data
Synonyms Hydroxyl benzene, carbolic acid
Chemical formula C6H6O
Appearance Transparent crystalline solid
Density 1.06 g/cm3
Melting point 40.9 0C
Boiling point 181.8 0C
Vapor pressure 0.35 mmHg (250C)
Flash point 790C
Molecular weight 94.113 g/mol
Viscosity 3.49 mPa.s (500C)
1.78mPa.s (750C)
1.099 mPa.s (1000C)
LogP 1.46
LogS 0
Auto-Ignition 7150C
Corrosivity Caustic
Heat of combustion 3053.5kj/mol(solid)
Heat of vaporization 57.82kj/mole(250C)
pH 6(aq.soln)
Surface tension 38.2 mN/m(500C)
35.53mN/m(750C)
32.86 mN/m(1000C)
Ionization potential 8.50 eV
pKa 9.99(250C)

Phenol is an organic compound appreciably soluble in water, with about 842.8 g dissolving in 1000
mL (250C). Homogeneous mixtures of phenol and water at phenol to water mass ratios of ~2.6 and
higher are possible. The sodium salt of phenol, sodium phenoxide, is far more water-soluble.
Phenol is a mono-hydroxylated benzene ring and is a colorless solid at room temperature.[3]
Phenol is weakly acidic, Compared to aliphatic alcohols, is about 1 million times more acidic. And
at high pHs gives the phenolate anion (phenoxide) C6H5O-. It reacts completely with aqueous
(NaOH) to loss H+, whereas most alcohols react only partially.

Reactions of phenol
• Neutralization of phenol with caustic soda and produce sodium phenate or phenolate :

C6H5OH + NaOH →C6H5ONa +H2O (1.1)

• Phenyl benzoate production :
when a mixture of phenol and benzoyl chloride are shaken in presence of dilute sodium hydroxide
solution , Phenyl benzoate is formed .

4
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

C6H5OH +C6H5COCl →C6H5OCOC6H5 +HCl (1.2)

• Benzene production :
when phenol distilled with zinc dust benzene is formed .

C6H5OH +Zn →C6H6 +ZnO (1.3)

• Anisole production :
when phenol reacted with diazomethane in the presence of borontrifluoride (BF3) , Anisole is
obtained as the main product and Nitrogen gas as a byproduct .

C6H5OH +CH2N2 →C6H5OCH3 +N2 (1.4)

Effects of phenol
Phenols have relatively high water solubility and widely known to be acutely toxic to a range
of organisms. It produces undesirable taste, odour, colour to water and is considered toxic
(Klibanov 1982). Continuous ingestion of phenol for prolonged period of time causes mouth sore,
diarrhea, excretion of dark urine and impaired vision at concentrations levels ranging between 10
and 240 mg/L (Barker et al 1978). Phenols are toxic to several biochemical functions (Kumaran
1986) and to fish life (Sufit 1978). It acts as substrate inhibitor in the biotransformation (Hill and
Robinson 1975). Lethal blood concentration for phenol is around 4.7 to 130 mg/100 ml. Phenol
affects the nervous system and key organs, i.e. spleen, pancreas and kidneys (Manahan 1994).
Phenol also contributes to off-flavours in drinking and food processing waters (Hill and Robinson
1975, Yang and Humphery 1975). Although not found to be bioaccumulative (Loehr and
Krishnamoorthy 1988), humans exposed to phenol in well water at concentrations of 1300 mg/L
exhibited a statistically significant increase in diarrhoea, mouth sores, dark urine and burning of
the mouth (USEPA 1980). The toxic effects of phenol on humans, animals and fishes are presented
in the Table (1.2)[5].
Table 1-2: The Toxic Effects on Humans, Animals and Fish [5]

Toxic effects Effects studied Reference

Effects on Acute exposure IPCS
Humans Anorexia, weight loss, headache, vertigo, 1994,1999
Route –Inhalation salivation and dark urine indicative of
nephrotoxicity

Cardiovascular effects, respiratory distress, IPCS

Route-Ingestion metabolic acidosis, renal failure, 1994,1999
neurological effects, shock, coma and death

Dermal inflammation, erythema, anaesthetic, IPCS

Dermal exposure painless blanching, burns, corrosion and necrosis 1994,ATSDR
1998

5
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

Route –Inhalation Chronic exposure

Gastrointestinal effects such as anorexia, progressive IPCS
weight loss and excess 1994,1999
production of saliva, Muscle pain and weakness ATSDR 1998
have also been reported, enlarged liver, and
elevated concentrations of liver enzymes and dark
urine.

Route-Ingestion Gastrointestinal irritation, cardiovascular, CNS and IPCS

respiratory effects and decreased 1994,1999
body weight ATSDR 1998

Dermal exposure Onychronosis (yellowing of the skin), skin irritation IPCS

skin eruption, as well as dermal inflammation and 1994,1999
necrosis ,ATSDR 1998
DEFRA 2003

Effects on animals Acute effects are generally attributed to the IPCS 1999
Route –Inhalation depression of the CNS, neuromuscular
hyperexcitability (twitching and convulsions),
increased heart rate followed by slow
and irregular heart rate), hypertension followed by
hypotension, salivation, dyspnoea and
hypothermia.

Route-Ingestion Cardiovascular effects, respiratory distress, IPCS 1999,

metabolic acidosis, renal failure, ATSDR
neurological effects, shock, coma and death. 1998

Dermal exposure Erythema, inflammation, oedema, skin irritation, IPCS 1999,

discolouration, eczema and necrosis, congenital NTIS
malformations
2005
Effects on fishes Phenol at 5-25 mg/L are toxic to fishes causing Saha et al 1999,
Route- general genotoxic, carcinogenic, pytotoxic, Gonzalez et al
immunotoxic, haematological, physiological effects, 1990,
antibiosis, ovipositional Rodriguez
deterrence and reduced growth rate 1988,
Girolami et al
1981,
Capsso et al
1992,
Nahed and
Amal 2008

6
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

Uses of phenol
The most important chemical made from phenol is bisphenol A, which is used to make the
polycarbonates. Phenol is also catalytically reduced to cyclohexanol, which is used in the
manufacture of polyamides 6 and 6,6.

Uses of phenol

others
13%

bisphenol A
phenolic resin 46%
28%

cylcohexanol
13%

bisphenol A cylcohexanol phenolic resin others

Figure 1-3:Uses of Phenol[4]

Phenol is also used to make a range of thermosetting polymers (resins). It reacts with methanal in
the presence of a catalyst to form phenol-methanal resins.
Among the other uses of phenol is the production of phenylamine (aniline) needed, for example,
for the manufacture of dyes. Antiseptics such as 2,4-and 2,6-dichlorophenols are also made from
phenol. [3]The annual production is shown on table (1.3)[4]:
Table 1-3:Annual Production of Phenol[4]

World 8.9 million tonnes

Europe 8.9 million tonnes
Asia 2.7 million tonnes
US 2.3 million tonnes
Sudan doesn’t produce phenol but it consumes it in several industrial purposes .
Production of phenol
1.2.6.1 Cumene Peroxidation Process for Phenol Production
Reactions Involved in Cumene Peroxidation Process:

C6H5CH (CH3) + O2 → C6H5C (CH3)2OOH (1.5)

C6H5C (CH3)2OOH + H2SO4 ↔ C6H5OH + CH3COCH3 (1.6)

(Cumeneperoxide) (Phenol) (Acetone)

7
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

Material Requirements :

Cumene, Air, Sulfuric acid and Sodium hydroxide.

Final product: Phenol

Co-product: Acetone

The cumene peroxidation process for the manufacture of phenol involves the liquid phase air
oxidation of cumene to cumene peroxide, which in turn is decomposed to phenol and acetone by
the action of an acid.

The cumene (isopropylbenzene) may be manufactured by either liquid or vapor phase

alkylation of benzene with propylene. In the liquid phase the alkylation catalyst is usually sulfuric
acid; in the vapor phase, it is phosphoric acid absorbed on a carrier. Purified cumene is mixed with
purified recycle cumene and fed to the oxidation vessel along with a dilute soda ash solution, in
order to maintain the pH between 6.0 and8.0, the mixture is contacted with air and held at 110 and
115°C until 20 to 25% of the cumene is converted to the cumene peroxide. Yields of cumene
peroxide may be improved by operating at lower temperature (100 to 110°C) and accepting lower
conversions. In one modified process sequence of three to four reactors is operated at successively
lower temperature.

The crude mixture from the oxidizer is concentrated to about 80% cumene peroxide and fed to
a reactor in which the cumene peroxide is cleaved to phenol and acetone. The reaction is usually
carried out under conditions of mild temperature (70 to 80°C) and pressure, and in the presence of
a small amount of sulfuric acid. Numerous non oxidizing inorganic acids, e.g. sulfuric dioxide are
used. The cleavage mechanism is an example of a 1, 2 shift from carbon to oxygen.

It is highly undesirable that such 1, 2 cleavages occur during the oxidation stage because phenols
are potent inhibitors of free radical oxidation. Therefore, it is essential that no acidic materials
interfere with the oxidation process.

The resulting product mixture consists of the compositions shown in table (1.4)[1]:

Table 1-4:Compositions of Products[1]

Compound(wt%) %composition
Phenol 14
Cumene 76
Acetophenone 0.4
Acetone 8
ά methyl styrene 1.6

The products are separated by distillation. Acetone is removed overhead in the first column and
further purified by distillation. The bottoms from this column are then vacuum distilled to send
unreacted cumene and by-product a methyl styrene overhead. If this impure cumene were recycled

8
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

as such, the methyl styrene must be purified. This can be done by catalytic hydrogenation of the ά
methyl styrene to cumene, to by careful fractionation. In the latter case, a methyl styrene is
available as a by-product. The bottoms from the vacuum still are further distilled to separate
acetophenone and cumene from phenol .phenol is the overhead product obtained with a yield of
90 to 92%.

1.2.6.2 Cholorobenzene and Caustic Process for Phenol Production

Process Description of Chlorobenzene and Caustic process for phenol production

For 1 ton of phenol production approximately the following raw materials are required as per the
process described:

Benzene = 0.90 tons

Chlorine = 0.82 tons

NaOH = 0.67 tons

HCl = 0.51 tons

The main reactions which take place for this process are:

1. Chlorination

C6H6 + Cl 2 85℃ C6H5CL (Chlorobenzene) (1.7)

𝐹𝑒 −

2. Causticization

C6H5Cl +NaOH (aq) → C6H5ONa (1.8)

3. Hydrolysis

C6H5NaO + HCl(aq) →C6H5OH + NaCl(aq) (1.9)

Benzene which is in dry state, reacted with chlorine at the presence of the catalyst iron or
anhydrous ferric chloride at about 85 deg centigrade temperature to form Chlorobenzene in a
chlorination tower, unconverted benzene is recycled and monochlorobenzene is withdrawn all
excess chlorine is used in neutralizer and about 10% solution of dilute caustic soda is mixed with
Chlorobenzene which is reacted with caustic solution where chlorine present at the benzene ring
is reacted with hydrogen and produce water vapors which are removed a tail gas. The resulting
product diphenly oxide is pumped to the preheater and then passed to multi-tube reactor where
causticization reaction occurs at the parameters 425 deg centigrade and 350 atm pressure, then the
reacted mixture is passed to the neutralizer through the effluent heat exchangers.Phenol is obtained
from hydrolysis occurs at the neutralizer where reaction with concentrated hydrochloric acid take
place to form phenol and sodium chloride.Sodium chloride is formed as a side product, this salt is
separated and send to electrolysis.Upstream from the separator is sent to vacuum distillation

9
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

column where phenol is stripped out. About 95% yield is obtained and diphenyl oxide is removed
from the bottom of the column to recycle.
Major engineering problems in this process are:

HCl corrosion in Chlorobenzene plant section

High-pressure vessel design for causticization reactor.

1.2.6.3 Phenol Production by Benzene Sulfonation Process

Benzene can be converted to phenol with the help of inorganic acids and salts and this process
is oldest of all the process where phenol is produced by reactants such as cumene and toluene. This
process involves four major chemical reactions which are:
Sulfonation: Benzene is reacted with sulphuric acid to form benzene sulphonic acid at 150 to 170
deg centigrade.
Neutralization: Benzene sulphonic acid is reacted with sodium sulfite to form sodium benzene
sulphonate.
Fusion: Sodium benzene sulphonate is fused with sodium hydroxide to form sodium phenoxide.
Acidification: sulphuric acid and sodium phenoxide are reacted to produce crude phenol and
sodium sulphite.
The above reaction step explains the requirement of the unit operation equipment in the process as
Filtration: Pressure filter and centrifuge used in the separation of sodium sulphate and sodium
sulphite.
Distillation: Separation of phenol from crude phenol.
Crystallization: Separation and recovery of sodium sulphite.
This process is large-scale batch cycle operation due to slow reaction step at fusionator. Sodium
benzene sulphonate is fed to cast iron make fusion pots which already contains molten caustic soda
at a temperature of 300 deg centigrade, due to slow reaction with take about 5-6 hours of residence
time the pot is fed at regular intervals where continuous loading and unloading of the pot occurs
for continuity of the process, thus sodium phenoxide fraction which is obtained is fed to acidifier
to produce crude phenol by reacting with sulphuric acid and sulphur dioxide. Vacuum distillation
column is used to get phenol from crude phenol and remain salts are stripped in a steam stripper
to remove phenol from them and aqueous salts. Crystallizers are used to increase the purity of the
sodium sulphite; these crystals are separated from mother slurry by a continuous centrifugal
separator, which is recycled to neutralizer.

1.2.6.4 Toluene two-stage oxidation process

Toluene in the liquid phase is oxidized with air in a reactor under 40-70 p.s.i in presence of a
soluble cobalt catalyst maintained at 150°c. benzoic acid and water are thus formed. The reaction
is exothermic and the temperature is maintained by external cooling. The crude molten benzoic
acid at about 150-200°c is transferred from the reactor to distillation column, where separation of
benzoic acid from unreacted toluene and produced water take place. The toluene is separated and
recycled to the first oxidizing reactor. The pure benzoic acid is fed to a second reactor, where it is
oxidized to phenol by air and steam under 20-25 psi at 230°c in presence of cupric benzoate catalyst
promoted with manganese. The reaction mass is periodically withdrawn from the second reactor
into an extractor, where it is washed with water to remove unwanted tars and benzoic acid and
steam are returned to the second reactor. The phenol, water and unreacted benzoic acid are

10
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

conducted overhead to two distillation columns in series. In the first column, crude phenol is
separated from overhead and unreacted benzoic acid is recycled to the second oxidizing reactor.
Pure form phenol is obtained at the second distillation column as overhead product and supply's
aromatics compounds and benzoic acid as a feed for crude phenol rectification column. The yield
of phenol on benzoic acid is about 75- 80%.

1.2.6.5 Raschig process

This process was developed in Germany in 1940. Benzene is first converted into Chlorobenzene
by passing a mixture of benzene vapour, hydrochloric acid vapour and air under normal pressure
at about 23°c in presence of a copper iron catalyst, supported on alumina.

The reaction is exothermic in nature and so the temperature is maintained constant by external
cooling. The conversion .the per pass is 10%. The Chlorobenzene after separation from unchanged
reactants is hydrolyzed into phenol by heating with steam at about 400500°c in presence of silica
catalyst. The conversion is again about 10% per pass in this second step. Hydrogen chloride set
free in the reaction is recovered and recycled. Crude phenol (97%) obtained according to the above
reaction is purified by distillation under vacuum. The yield is about 75-85% of benzene. A small
amount of HCl is sufficient to convert large amounts of benzene into phenol.[1]

Table 1-5:Summery to all the Above Methods[1]

S.No Existing Methods Raw Materials/Catalyst Yield Products Comments

1 Cumene peroxidation Cumene,Air, Zelolite 92% Phenol Produces
catylyst and valuable
Acetone coproduct
acetone
2 Toluene two-stage Toluene,Air,Cobalt 80% Phennol Low-cost
oxidation napthalate,Cupric and CO2 operation by
benzoate catalyst direct toluene

3 Rasching phenol process Benzene,Air,HCl 75% Phenol Feasible

and HCl under large
as units
recycling
4 Chlorobenzene caustic Benzene,Chlorine,HCl 95% Phenol Economically
hydrolysis NaOH and NaCl not feasible
5 Benzene sulfonate Benzene, H2SO4,NaOH 87% Phenol Operates on
process ,Na2SO3, large batch
Na2SO4 cycles

11
CHAPTER ONE: INTRODUCTION AND LITERATURE REVIEW ||PHENOL

References

[1] Types Of Phenol Manufacturing Process [Internet]. Enggyd.blogspot.com. [cited 28

November 2018]. Available from: http://enggyd.blogspot.com/2010/07/phenolmanufacturing-
process.html?m=1
[2] Phenol - Chemical Economics Handbook (CEH) | IHS Markit [Internet]. Ihsmarkit.com.
2018 [cited 7 December 2018]. Available from:
https://ihsmarkit.com/products/phenolchemical-economics-handbook.html
[3] Phenol [Internet]. Pubchem.ncbi.nlm.nih.gov. [cited 7 December 2018]. Available from:
https://pubchem.ncbi.nlm.nih.gov/compound/phenol

[4] Lazonby J. Phenol [Internet]. Essentialchemicalindustry.org. [cited 3 December 2018].

Available from: http://www.essentialchemicalindustry.org/chemicals/phenol.html

[5] Literature review [Internet]. shodhgange.com. 2018 [cited 3 December 2018]. Available
from:
https://www.google.com/urls?sa=t&source=web&rct=j&url=http://shodhganga.inflibne.ac.in/
bitstream/10603/34345/7/07_chapter%25202.pdf&ved=2ahUKEwjR1LqF7orfAhWQZFAK
HSQQCUQFjABegQICRAB&usg=AOvVaw02g5YT53alKNjqGf5XNGFe&cshid=1544083
992539
[6] Kutlu A, Martin D, Ross D, Greco C. Direct route to phenol from benzene. 2012.

[7] Rappoport Z. The Chemistry of Phenols. Chichester: John Wiley & Sons; 2004.

12
CHAPTER TWO: PROCESS DESCRIPTION ||PHENOL

Chapter 2: Process Description

Brief Description

Presently the cumene-to-phenol process is the predominant route for the production of phenol.
In 2008, more than 97% of the phenol worldwide was produced by this process.[2] The process was
first reported by Hock and Lang. Cumene is oxidized with oxygen (from air) to form cumene
hydroperoxide (CHP), followed by acid-catalyzed decomposition (cleavage) of CHP to phenol and
acetone. Phenol, acetone, unconverted cumene, and by-products are then distilled in a series of
distillation towers to recover high purity phenol and acetone products and to recover cumene to be
recycled to reaction. [1]

Figure 2-1: Production of phenol from cumene block diagram

13
CHAPTER TWO: PROCESS DESCRIPTION ||PHENOL

Detailed Description
Liquid Phase Cumene Oxidation
Fresh and recycle cumene are fed to an oxidizer where the cumene contacts air and is
converted to CHP, along with a dilute soda ash to maintain a pH(6-8).
Main reaction

C6H5CH(CH3)2 (L) + O2 (g) C6H5COOH(CH3)2(L) 2.1

Cumene + Oxygen Cumene peroxide
Side reactions

1) 2C6H5CH(CH3)2 (L) + O2 (g) 2C6H5COH(CH3)2(L) 2.2

2Cumene + Oxygen a,a-dimethylbenzyl alcohol (DMBA)
2) C6H5COOH(CH3)2 (L) C6H5COCH3 (L) + CH3OH (L) 2.3
Cumene Peroxide Acetonephenone + Methanol
Air is added at the bottom of the reactor. Oxygen transfers from the air bubbles into the cumene.
The reaction in the liquid phase proceeds by a complex radical mechanism. The reaction is auto-
catalyzed by CHP. The liquid phase in such large reactors is intensively mixed by the rising gas
bubbles. This mixing characteristic plays a critical role in conversion rates and yields. Several by-
products are formed in the oxidation step. The overall process selectivity is mainly dependent on
the formation of dimethylbenzyl alcohol (DMBA), acetophenone (ACP) and methanol. Other by-
products are formic and acetic acid. Small amounts of methyl hydroperoxide (MHP) are formed
and removed with the off-gas. Phenol is a strong inhibitor for the oxidation reaction. Any recycle
cumene must be treated to remove even small traces of phenol.[1]

Acid-Cleavage
The cleavage unit is a CSTR reactor were CHP is decomposed to produce Phenol and Acetone
comprising: introducing a process stream containing CHP into the CSTR contacting catalyst
stream containing material selected from group consisting of FAU,MWW,UZM-4,UZM-5,UZM-
8,ZSM-18,MOR,MTW,SPA and Cs hetropoly acid. CHP decomposes contacting the catalyst
stream. DMBA is partially dehydrated to α- methylstyrene (AMS), which reacts in consecutive
reactions with phenol to high-boiling cumylphenols, see below. DMBA reacts with CHP to
dicumyl peroxide (DCP) and water.

All these by-products require special conditions in the distillation unit to separate them from
phenol and acetone.[1]

Main reaction

C6H5COOH(CH3)2 (L) C6H5OH (g) + (CH3)2CO (g) 2.4

Cumene Peroxide Phenol + Acetone
Side reaction

C6H5COH(CH3)2 (L) C6H5C(CH2)CH3 (g) + H2O (L) 2.5

DMBA ∝ −𝑚𝑟𝑡ℎ𝑦𝑙𝑡𝑦𝑟𝑒𝑛𝑒 + water

14
CHAPTER TWO: PROCESS DESCRIPTION ||PHENOL

In the reactor, DCP reverts to CHP and DMBA. CHP is cleaved spontaneously to
phenol and acetone, while DMBA is completely dehydrated to AMS and water.[1]
Separation
The product from cleavage unit is sent to the first distillation column which is Acetone
atmospheric fractionation to separate Acetone as top product. The bottom product (CHP, Phenol,
AMS, ACP and light/ heavier by-products) are send to the second distillation which mainly
separates Cumene which will be recycled back to the oxidizer. The bottom is an inlet stream to a
third distillation column where the main separate is AMS. The distilled AMS is sent to a recovery
system where the AMS is hydrogenated to Cumene using fresh hydrogen in a CSTR reactor. The
bottom mixture is sent to Phenol column which mainly separates Phenol and its bottom products
which contains heavy by-products, ACP and some phenol can be used as fuel.

Hydrogenation of AMS
The alpha methyl styrene is converted to cumene by feeding the reactor with hydrogen gas and
the aid of Nickel catalyst. This step converts the unsaturated hydrocarbon to saturated
hydrocarbon. The unsaturated compound might yield to other than cumene peroxide, this is the
reason for this pre – purification method as to eliminate the availability of the unsaturated in the
feed stock. The product from this reactor is mix to the fresh cumene feed by a recycle stream.
Hydrogen gas is fed with 4:1 ratio with α – methylstyrene fed to the reactor.

Figure 2-2: Production of phenol from cumene flow sheet

15
CHAPTER TWO: PROCESS DESCRIPTION ||PHENOL

References

[1] Weber M, Weber M. Phenolic Resins: A Century of Progress. Berlin: Springer; 2010.
[2] eni versalis. versalis proprietary process technologies available for licensing. Italy; p. 5.

16
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Chapter 3: Materials balance

Introduction
Material balances are important first step when designing a new process or analyzing an existing
one. They are almost always prerequisite to all other calculations in the solution of process
engineering problems. Material balances are nothing more than the application of the law of
conservation of mass, which states that mass can neither be created nor destroyed. Thus, you
cannot, for example, specify an input to a reactor of one ton of naphtha and an output of two tons
of gasoline or gases or anything else. One ton of total material input will only give one ton of total
output, i.e. total mass of input = total mass of output. A material balance is an accounting for
material. Thus, material balances are often compared to the balancing of current accounts. They
are used in industry to calculate mass flow rates of different streams entering or leaving chemical
or physical processes.

General balance equation

Input + Generation − Output − Consumption = Accumulation

Input (enters through system boundaries), Generation (produced within system boundaries),
Output (leaves through system boundaries), Consumption (consumed within system),
Accumulation (buildup within system). This general balance equation may be written for any
material that enters or leaves any process system; it can be applied to the total mass of this material
or to any molecular or atomic species involved in the process. The general balance equation may
be simplified according to the process at hand. For example, by definition, the accumulation term
for steady-state continuous process is zero. Thus the above equation becomes:

Input + Generation = Output + Consumption

For physical process, since there is no chemical reaction, the generation and consumption terms
will become zero, and the balance equation for steady-state physical process will be simply
reduced to:

Input = Output

Basis: 420 tons/day of phenol

17
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Reactor (1) – Oxidation Reactor

Chemical Reactions
Sodium hydroxide, NaOH acts as the emulsification agent for the emulsification of cumene in the
reactor and not directly involved in the reaction of the reactants to produce the products. Thus, is
not considered for the material balance.

3.2.1.1 Main Reaction

1) C6H5CH(CH3)2(ℓ)+O2(g)→C6H5COOH(CH3)2(ℓ) ___________________________(1)

Cumene + Oxygen → Cumene Peroxide

3.2.1.2 Side Reactions

1) 2C6H5CH(CH3)2(ℓ)+O2(g)→2C6H5COH(CH3)2(ℓ) ____________________________(2)
2 Cumene + Oxygen → a,a – dimethylbenzyl alcohol (DMBA)
2) C6H5COOH(CH3)2(ℓ)→C6H5COCH3(ℓ)+CH3OH(ℓ) ___________________________(3)
Cumene Peroxide → Acetonephenone + Methanol

Assumptions
1) Ratio of feed; Cumene: Oxygen Gas = 1 : 4.

2) Conversion of Cumene to Cumene Peroxide is 80%.

3) Conversion of Cumene to DMBA is 6%.

4) Conversion of Cumene Peroxide to Acetonephenone and Methanol is 2.5%.

18
 CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance
Table 3-1:Component’s molar flow and Composition of R-(101).

Input Output
Flow Flow Flow Flow
Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmole/hr) (kg/hr) (kmole/hr)

Gas Phase Gas Phase

Oxygen 31534.8608 985.4644 Methanol
0.21 157.6743 4.927322 0.17
(O2) (CH3OH)
Nitrogen 103802.25 3707.22 Oxygen
0.79 24991.38 780.98 0.83
(N2) (O2)
Nitrogen
103802.30 3707.22 0.00
(N2)
135337.11 4692.69
Total 1.00 Total 128951.30 4493.13 1.00

Liquid Phase Liquid Phase

Cumene Cumene
29563.93 246.37 0.99 4138.95 34.49 0.14
(C9H12) (C9H12)
Cumene
Peroxide 29209.16 192.17 0.77
(C9H12O2)
DMBA
2010.35 14.78 0.06
(C9H12O)
Acetonephenone
591.28 4.93 0.02
(C8H8O)
Phenol 182.46 1.94 0.01 Phenol 182.46 1.94 0.01
AMS ( α–
17.62 0.15 0.00 AMS 17.62 0.15 0.00
methylstyrene)
H2O 2.69 0.15 0.00 H2O 2.69 0.15 0.00

Total 29766.70 248.61 1.00 Total 36152.51 248.61 1.00

Total of Input Flow Rate (Kg\hr) 165103.80 Total of Output Flow Rate (Kg\hr) 165103.80

19
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Reactor (2) - Cleavage Unit

Chemical Reactions
The catalyst particles are not directly involved in the reaction of the reactants to produce products.
Thus, is not considered for the material balance. However, the aqueous acid solution is required to
enable the hydrolysis of cumene peroxide.

3.3.1.1 Main Reaction

1)C6H5COOH(CH3)2(ℓ)→C6H5OH(g)+(CH3)2CO (g) _____________________________(4)

Cumene Peroxide → Phenol + Acetone

3.3.1.2 Side Reaction

3) C6H5COH(CH3)2(ℓ)→C6H5C(CH2)CH3(g)+H2O(ℓ)____________________________(5)

DMBA → α – methylstyrene + Water

Assumptions
1) Overall conversion of DMBA and Cumene Peroxide are 100%.

2) Main reaction: Selectivity of Phenol over Acetone is 65%.

3) Side reaction: Selectivity of α – methylstyrene over water is 87%.

4) Ratio of ZSM-5 catalyst. Cumene feed: catalyst = 100: 0.7.

20
 CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance
Table 3-2:Component’s molar flow and Composition of R-(102).

Input Output
Flow Flow Flow Flow
Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmole/hr) (kg/hr) (kmole/hr)

Cumene
4138.95 34.49 0.14 Cumene (C9H12) 4138.95 34.49 0.076
(C9H12)
Cumene
Acetonephenone
Peroxide 29209.17 192.17 0.78 591.28 4.93 0.01
(C8H8O)
(C9H12O2)
DMBA Phenol
2010.35 14.78 0.06 18246.02 194.11 0.43
(C9H12O) (C6H5OH)
Acetonephenone Acetone
591.28 4.93 0.02 11145.60 192.17 0.42
(C8H8O) (C3H6O)

α–methylstyrene
Phenol 182.46 1.94 0.01 1761.89 14.93 0.03
(C9H10)

α–methylstyrene 17.62 0.15 0.00 Water (H2O) 268.76 14.93 0.03

H2O 2.69 0.15 0.00

Total 36152.51 248.61 1.00 Total 36152.51 455.55 1.00

21
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Distillation Unit 1: Acetone separation

The first distillation unit separates mainly acetone from the other components.

Assumptions
Distillate composition: 100% of acetone from crude phenol, 99% of water from crude phenol and
8% of cumene from crude phenol.

22
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance

Table 3-3:Component’s molar flow and Composition of T-(101)

Input Output

Flow Flow Flow Flow

Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmole/hr) (kg/hr) (kmole/hr)

Cumene 4138.95 34.49 0.075 Distillate

ACP 591.28 4.93 0.01 Cumene 331.12 2.76 0.01

Phenol 18246.02 194.10 0.43 Acetone 11145.60 192.17 0.92

Acetone 11145.60 192.17 0.42 H2O 266.08 14.79 0.07

AMS 1761.89 14.93 0.03 Total 11742.79 209.71 1.00

H2O 268.76 14.93 0.03 Bottom

Cumene 3807.83 31.73 0.13

ACP 591.28 4.93 0.02

Phenol 18246.02 194.11 0.79

AMS 1761.89 14.93 0.06

H2O 2.69 0.15 0.00

Total 24409.71 245.85 1.00

Total Flow Rate (kg/hr) of Distillate

Total 36152.51 455.55 1.00 & Bottom
36152.51

23
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Distillation Unit 2: cumene separation

The second distillation unit separates mainly large amount of cumene to recycle it to the feed.

Assumptions
Distillate composition: 99% of cumene and 1% of AMS goes to the top of the column.

24
 CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance

Table 3-4:Component’s molar flow and Composition of T-(102).

Input Output

Flow Flow Flow Flow

Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)

Cumene 3807.83 31.7320 0.13 Distillate

ACP 591.28 4.9273 0.02 Cumene 3769.76 31.41 0.99

Phenol 18246.02 194.1066 0.79 AMS 17.62 0.15 0.01

AMS 1761.89 14.9313 0.06 H2O 2.69 0.15 0.00

H2O 2.69 0.1493 0.00 Total 3790.06 31.71 1.00

Bottom
Cumene
38.08 0.32 0.00
ACP
591.28 4.93 0.02

Phenol 18246.02 194.11 0.91

AMS 1744.27 14.78 0.07

Total 20619.65 214.13 1.00

Total Flow Rate (kg/hr) of Distillate

Total 24409.71 245.85 1.00 24409.71
& Bottom

25
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Distillation Unit 3: AMS separation

The third distillation unit separates mainly AMS.

Assumptions
Distillate composition: 99% of AMS and 1% of phenol goes to the top of the column.

26
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance

Table 3-5:Component’s molar flow and Composition of T-(103).

Input Output

Flow Flow Flow Flow

Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)

Cumene 38.08 0.32 0.00 Distillate

ACP 591.29 4.93 0.02 Cumene 38.08 0.32 0.02

Phenol 18246.02 194.11 0.91 Phenol 182.46 1.94 0.15

AMS 1744.27 14.78 0.07 AMS 1726.83 14.63 0.87

Total 1947.37 16.89 1.00

Bottom

ACP 591.28 4.93 0.03

Phenol 18063.56 192.17 0.97

AMS 17.44 0.18 0.00

Total 18672.28 197.24 1.00

Total Flow Rate (kg/hr) of

Total 20619.65 214.13 1.00 20619.65
Distillate & Bottom

27
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Distillation Unit 4: phenol separation

The fourth distillation unit separates mainly phenol.

Assumptions
Distillate composition: 96% of phenol and 5% of ACP goes to the top of the column.

28
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance

Table 3-6:Component’s molar flow and Composition of T-(104).

Input Output

Flow Flow Flow Flow

Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)

ACP 591.28 4.93 0.03 Distillate

Phenol 18063.56 192.17 0.97 ACP 29.56 0.25 0.01

AMS 17.44 0.15 0.00 Phenol 17341.02 184.48 0.99

AMS 17.44 0.15 0.00

Total 17388.03 184.87 1.0000

Bottom

ACP 561.71 4.68 0.38

Phenol 722.54 7.69 0.62

Total 1284.26 12.37 1.00

Total Flow Rate (kg/hr) of

Total 18672.28 197.24 1.00 18672.28
Distillate & Bottom

29
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Reactor 3 – Pre - Purification Reactor

The alpha methyl styrene is converted to cumene by feeding the reactor with hydrogen gas and
the aid of Nickel catalyst. This step converts unsaturated hydrocarbon to saturated hydrocarbon.
The unsaturated compound might yield to other than cumene peroxide, this is the reason for this
pre – purification method as to eliminate the availability of the unsaturated in the feed stock. The
product from this reactor is mix to the fresh cumene feed by a recycle stream. Hydrogen gas is fed
with 4:1 ratio with AMS fed to the reactor.

Chemical Reaction Involved In Pre – Purification Reactor

1) C6H5C(CH2)CH3 (ℓ) + H2(g) → C6H5CH(CH2)CH3 (ℓ) _______________________(6)

α – methylstyrene + Hydrogen gas → Cumene

30
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Material Balance
Table 3-7:Component’s molar flow and Composition of R-(103).

Input Output

Flow Flow Flow Flow

Component Rate Rate Composition Component Rate Rate
Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)

Liquid Phase Liquid Phase

Cumene 38.08 0.33 0.02 Cumene 1794.18 14.95 0.89

Phenol 182.46 1.94 0.11 Phenol 182.46 1.94 0.11

AMS 1726.83 14.64 0.87

Total 1947.37 16.89 1.00 Total 1976.64 16.89 1.00

Gas Phase Gas Phase

H2 117.07 58.54 1.00 H2 87.80 43.90 1.00

Total 117.07 58.54 1.00 Total 87.80 43.90 1.00

Total of Output Flow Rate

Total of Input Flow Rate (Kg\hr) 2064.44 2064.44
(Kg\hr)

31
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Mixer 1

Material Balance
Table 3-8:Component’s molar flow and Composition of M-(101).

Input Output
Flow Flow Flow Flow
Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)
n 27 n 28

Cumene 24000.00 200.00 1.00 Cumene 25794.18 214.95 0.99

Total 24000.00 200.00 1.00 Phenol 182.46 1.9411 0.01

n 26

Recycle
1794.18 14.95 0.89
Cumene

Phenol 182.46 1.94 0.11

Total 1976.64 16.89 1.00

Total of Input Flow Rate (Kg\hr) 25976.64 Total 25976.64 216.89 1.00

32
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Mixer 2

Material Balance
Table 3-9:Component’s molar flow and Composition of M-(102).

Input Output
Flow Flow Flow Flow
Component Rate Rate Composition Component Rate Rate Composition
(kg/hr) (kmol/hr) (kg/hr) (kmol/hr)
n 28 n1

Cumene 25794.18 214.95 0.99 Cumene 29563.93 246.37 0.99

Phenol 182.46 1.94 0.001 Phenol 182.46 1.94 0.01

Total 25976.64 216.89 1.00 AMS 17.62 0.15 0.00

n 21 H2O 2.69 0.15 0.00

Recycle
3769.76 31.41 0.99
Cumene
AMS 17.62 0.15 0.01

H2O 2.69 0.15 0.00

Total 3790.06 31.71 1.0000

Total of Input Flow Rate

29766.69 Total 29766.69 248.60 1.00
(Kg\hr)

33
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

Overall Material Balance

Material Balance

𝑰𝒏𝒑𝒖𝒕 −𝑶𝒖𝒕𝒑𝒖𝒕
Error% = * 100
𝑰𝒏𝒑𝒖𝒕

Input = 159454.1841 kg/hr

Output = 159454.1841 kg/hr

Error = 0%

34
CHAPTER THREE: MATERIAL BALANCE ||PHENOL

References

[1] R. K. Sinnott, Coulson & Richardson's Chemical Engineering. Vol. 6,

Chemical Engineering Design, Butterworth-Heinemann, 3rd Ed., 1999.
[2] David M. Himmelblau, James B. Riggs, Basic Principles and Calculation in
Chemical Engineering, seventh edition.
[3] Perry’s chemical engineer’s handbook, McGraw-Hill, seventh edition, 199

35
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Chapter 4: Energy Balance

Introduction
Energy is transferred either as heat or work. A system does not contain 'heat', but the
transfer of heat or work to a system change its internal energy.
In process design, energy balances are made to determine the energy requirements of the
process: the heating, cooling and power required. In plant operation, an energy balance on the
plant will show the pattern of energy usage, and suggest areas for conservation and savings.
In this chapter, the fundamentals of energy balances are reviewed briefly and calculations
of energy requirement in the process is provided.

Energy balance fundamentals

The most common important energy form is heat energy and the conservation of this can
be illustrated by considering operations such as heating and drying. In these, enthalpy (total heat)
is conserved and as with the mass balances so enthalpy balances can be written around the
various items of equipment or process stages, or around the whole plant, and it is assumed that
no appreciable heat is converted to other forms of energy such as work.
Heat transferred from the system to its surroundings is taken as negative, and transfer of
heat from surrounding to system is taken as positive:
𝑄 − 𝑊 = ∆𝐻𝑟 + (−∆𝐻𝑖𝑛 ) + (∆𝐻𝑜𝑢𝑡 ) + (∆𝐾𝐸) + (∆𝑃𝐸) (4.1)

∆𝐾𝐸 ≡ The change in the kinetic energy.

∆𝑃𝐸 ≡ The change in the potential energy.

𝑄 ≡ Heat duty.

Enthalpy can be calculated from specific and latent heat data. If the kinetic and potential
energy terms are neglected, the general equation can be simplified to:

∆𝐻 = 𝑄 − 𝑊 (4.2)

This equation is usually sufficient for estimating the heating and cooling requirements of
the various units involved in a chemical process.
For many processes, the work term will be zero, or negligible:

𝐻2 − 𝐻1 = 𝑄 (4.3)

𝐻2 ≡ Enthalpy of the outlet stream.

𝐻1 ≡ Enthalpy of the inlet stream.

Calculation of specific enthalpy (H)

Tabulated values of enthalpy are available for the most common materials. In the absence of
published data, the following expressions can be used to estimate the specific enthalpy.

For pure materials with no phase change:

36
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

𝑇𝑜𝑢𝑡
𝐻 = ∫𝑇𝑖𝑛 𝐶𝑝 (4.4)

Where H = specific enthalpy from Tin to Tout.

Cp = specific heat capacity of the material at constant pressure.

If a phase transition takes place between Tin and Tout, the latent heat of the phase transition is
added to the sensible–heat change calculated by the equation. The sensible–heat calculation is
then split into two parts:
𝑇𝑏 𝑇𝑜𝑢𝑡
𝐻 = ∫𝑇𝑖𝑛 𝐶𝑝1 + λ 𝑇𝑏 + ∫𝑇𝑏 𝐶𝑝2 (4.5)
Where 𝑇𝑏 = Phase transition temperature K°.
𝐶𝑝1 = specific heat capacity of the first phase, below Tb.
𝐶𝑝2 = specific heat capacity of the second phase, above Tb.
λ 𝑇𝑏 = latent heat at 𝑇𝑏 kJ/kmol.
The specific heat at constant pressure will vary with temperature:
𝐶𝑝 = 𝑎 + 𝑏𝑇 + 𝑐𝑇 2 + 𝑑𝑇 3 + 𝑒𝑇 4 (4.6)
In appendix A, the heat capacity constants for liquids and gases are collected.
Cp in (kJ/kmol.°K).

37
 CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Equipment energy balance

Mixer M-(101):

1
2
17

Figure 4-1:Mixer M-(101)

Table 4-1:Component’s molar flow, enthalpy and temperature of M-(101).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component 𝐓𝐢𝐧
Tin Of
S1 S17 S2 Of 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S1 S17 S2
S1
S17
298.00 338.00 300.97 298.00
Cumene 200.00 14.95 214.95 0.00 7813.60 580.06

O2 0.00 0.00 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00 0.00 0.00

ACP 0.00 0.00 0.00 0.00 0.00 0.00

Phenol 0.00 1.94 1.94 0.00 8108.80 4059.60

Acetone 0.00 0.00 0.00 0.00 0.00 0.00

AMS 0.00 0.00 0.00 0.00 0.00 0.00

H2 O 0.00 0.00 0.00 0.00 0.00 0.00

H2 0.00 0.00 0.00 0.00 0.00 0.00

Q (kJ/hr) 0.00

38
 CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Mixer M-(102):

2
3
10

Figure 4-2:Mixer M-(102)

Table 4-2:Component’s molar flow, enthalpy and temperature of M-(102).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component 𝐓𝐢𝐧
Tin Of
S2 S10 S3 Of 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S2 S10 S3
S2
S10
Cumene 214.95 31.41 246.37 300.79 380.00 329.03 298.00 580.06 16017.88 6063.06

O2 0.00 0.00 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00 0.00 0.00

ACP 0.00 0.00 0.00 0.00 0.00 0.00

Phenol 1.94 0.00 1.94 4059.60 0.00 6247.95

Acetone 0.00 0.00 0.00 0.00 0.00 0.00

AMS 0.00 0.15 0.15 0.00 15270.04 5779.99

H2O 0.00 0.15 0.15 0.00 6182.80 4.01E+04

H2 0.00 0.00 0.00 0.00 0.00 0.00

Q (kJ/hr) 0.00

39
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Heater E-(101):

Figure 4-3:Heater E-(101)

Table 4-3: Component’s molar flow, enthalpy and temperature of E-(101).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
S5 S5o 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S5 S5o

Cumene 34.49 34.49 2344.08 5860.20

310.00 328.00 298.00
O2 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00

CHP 192.17 192.17 3547.15 8867.88

DMBA 14.78 14.78 2460.12 6150.30

ACP 4.93 4.93 2898.36 7245.90
Phenol 1.94 1.94 2379.28 6033.96

Acetone 0.00 0.00 0.00 0.00

AMS 0.15 0.15 2234.64 5586.60
H2 O 0.15 0.15 904.80 2262.00

H2 0.00 0.00 0.00 0.00

Q (kJ/hr) 1227503.00

40
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Reactor R-(101):

Figure 4-4: Reactor R-(101)

𝑄 = ∑ 𝑟 ∗ ∆𝐻𝑟𝑜 + ∑ 𝐻𝑜𝑢𝑡 − ∑ 𝐻𝑜𝑢𝑡 (4.7)

C6H5CH(CH3)2 (ℓ) + O2 (g) → C6H5COOH(CH3)2 (ℓ) (4.8)

2C6H5CH(CH3)2 (ℓ) + O2 (g) → 2C6H5COH(CH3)2 (ℓ) (4.9)

C6H5COOH(CH3)2 (ℓ) → C6H5COCH3 (ℓ) + CH3OH (ℓ) (4.10)

At T = 25 ℃

𝑟1 ∗ ∆𝐻𝑟1 = -396511.3382 KJ/kmol

𝑟2 ∗ ∆𝐻𝑟2 = -4135.40992 KJ/kmol

𝑟3 ∗ ∆𝐻𝑟3 = -16504.36083 KJ/kmol

Assuming 𝑇𝑟𝑒𝑓 in each reaction is equal to 25 ℃.

41
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-4:Component’s molar flow, enthalpy and temperature of R-(101).

Flowrate o (kmol/hr) T °𝑲 H (kJ/kmol)

Component Tin 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐨𝐮𝐭
S3 S4 S5 S6 Of Of Of Of 𝐓𝐫𝐞𝐟 S3 S4 S5 S6
S3 S4 S5 S6
Cumene 246 0 35 0 329 310 310 310 298 6063 0 2344 0

O2 0 985 0 781 0 385 0 385

N2 0 3708 0 3707 0 361 0 361

Methanol 0 0 0 5 0 0 0 795

CHP 0 0 193 0 0 0 3547 0

DMBA 0 0 15 0 0 0 2460 0

ACP 0 0 5 0 0 0 2898 0

Phenol 2 0 2 0 6247 0 2379 0

Acetone 0 0 0 0 0 0 0 0

AMS 0 0 0 0 5780 0 2234 0

H2 O 0 0 0 0 2E+03 0 9E+02 0

H2 0 0 0 0 0 0 0 0

Q (kJ/hr) -24,644,352.90

42
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Cooler E-(102):

Figure 4-5:Cooler E-(102)

Table 4-5:Component’s molar flow, enthalpy and temperature of E-(102).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
S4 S4o 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S4 S4o

Cumene 0.00 0.00 335.00 310.00 298.00 0.00 0.00

O2 985.46 985.46 0.00 -811.52

N2 3707.22 3707.22 0.00 -761.26

Methanol 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00

ACP 0.00 0.00 0.00 0.00

Phenol 0.00 0.00 0.00 0.00

Acetone 0.00 0.00 0.00 0.00

AMS 0.00 0.00 0.00 0.00

H2 O 0.00 0.00 0.00 0.00

H2 0.00 0.00 0.00 0.00

Q (kJ/hr) -3621884.70

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CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Reactor R-(102):

Figure 4-6:Reactor R-(102)

C6H5COOH(CH3)2 (ℓ) → C6H5OH (g) + (CH3)2CO (g) (4.11)

C6H5COH(CH3)2 (ℓ) → C6H5C(CH2)CH3 (g) + H2O (ℓ) (4.12)

At T = 25 ℃

𝑟4 ∗ ∆𝐻𝑟4 = -832673.8101 KJ/kmol

𝑟5 ∗ ∆𝐻𝑟5 = 8753.750311 KJ/kmol

Assuming 𝑇𝑟𝑒𝑓 in both reactions is equal to 25 ℃.

44
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-6: Component’s molar flow, enthalpy and temperature of R-(102).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
S5 S7 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S5 S7

Cumene 34.49 34.49 328.00 328.00 298.00 5860.20 5860.20

O2 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00

CHP 192.17 0.00 8867.88 0.00

DMBA 14.78 0.00 6150.30 0.00

ACP 4.93 4.93 7245.90 7245.90

Phenol 1.94 194.11 6033.96 6033.96

Acetone 0 192.17 0.00 5436.54

AMS 0.15 14.93 5586.60 5586.60

H2 O 0.15 14.93 2.26E+03 2.26E+03

H2 0.00 0.00 0.00 0.00

Q (kJ/hr) -47391391.97

45
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Heater E-(103):

Figure 4-7: Heater E-(103)

Table 4-7: Component’s molar flow, enthalpy and temperature of E-(103).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
S7 S7o 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐫𝐞𝐟 S7 S7o

Cumene 34.49 34.49 5860.20 18557.30

328.00 393.00 298.00
O2 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00

ACP 4.93 4.93 7245.90 22945.35

Phenol 194.11 194.11 6033.96 20088.15

Acetone 192.17 192.17 5436.54 3.78E+03

AMS 14.93 14.93 5586.60 17690.90

H2 O 14.93 14.93 2.26E+03 4.70E+04

H2 0.00 0.00 0.00 0.00

Q (kJ/hr) 3774920.23

46
 CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Distillation column T-(101):

Figure 4-8:Distillation column T-(101)

Table 4-8:Component’s molar flow, enthalpy and temperature of T-(101).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
SF SD SB 𝐓𝐅 𝐓𝐃 𝐓𝐁 𝐓𝐫𝐞𝐟 𝐇𝐅 𝐇𝐃 𝐇𝐁

Cumene 34.49 2.76 31.73 373.00 343.54 449.22 373.00 0.00 -5753.63 -27522.52
O2 0.00 0.00 0.00 0.00 0.00 0.00
N2 0.00 0.00 0.00 0.00 0.00 0.00
Methanol 0.00 0.00 0.00 0.00 0.00 0.00
CHP 0.00 0.00 0.00 0.00 0.00 0.00
DMBA 0.00 0.00 0.00 0.00 0.00 0.00
ACP 591.28 0.00 4.93 0.00 0.00 18408.39
Phenol 194.11 0.00 194.11 0.00 0.00 17704.31
Acetone 192.17 192.17 0.00 0.00 -3804.35 -43229.24
AMS 14.93 0.00 14.93 0.00 0.00 62956.15
H2 O 14.93 14.78 0.15 0.00 38429.14 2844.79
H2 0.00 0.00 0.00 0.00 0.00 0.00

For Condenser: For Reboiler:

R= 1.15 HF+QR=HD+HB+QC
QC= (1+R) Dλ

47
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-9:Q of T-(101).

Q (kJ/hr)

QF QD QB QC QR

0.00 -178882.51 3594325.07 -14502231.87 17917674.44

Distillation column T-(102):

Figure 4-9:Distillation column T-(102)

48
 CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-10:Component’s molar flow, enthalpy and temperature of T-(102).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component

SF SD SB 𝐓𝐅 𝐓𝐃 𝐓𝐁 𝐓𝐫𝐞𝐟 𝐇𝐅 𝐇𝐃 𝐇𝐁

Cumene 31.73 31.41 0.32 449.22 380.00 453.00 449.22 0.00 45100.00 1179.95

O2 0.00 0.00 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00 0.00 0.00

ACP 4.93 0.00 4.93 0.00 0.00 44396.54

Phenol 194.11 0.00 194.11 0.00 0.00 985.60

Acetone 0.00 0.00 0.00 0.00 0.00 0.00

AMS 14.93 0.15 14.78 0.00 35951.97 765.17

H2 O 0.15 0.15 0.00 0.00 -2586.23 0.00

H2 0.00 0.00 0.00 0.00 0.00 0.00

For Condenser: For Reboiler:

R= 15.09 HF+QR=HD+HB+QC
QC= (1+R) Dλ

49
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-11:Q of T-(102).

Q (kJ/hr)

QF QD QB QC QR

0.00 1421781.93 421753.67 -23004805.21 2.48E+07

Distillation column T-(103):

Figure 4-10:Distillation column T-(103)

50
 CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-12:Component’s molar flow, enthalpy and temperature of T-(103).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
SF SD SB 𝐓𝐅 𝐓𝐃 𝐓𝐁 𝐓𝐫𝐞𝐟 𝐇𝐅 𝐇𝐃 𝐇𝐁

Cumene 0.32 0.32 0.00 453.00 441.00 454.00 453.00 0.00 -3729.2 312.41

O2 0.00 0.00 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00 0.00 0.00

ACP 4.93 0.00 4.93 0.00 0.00 44638.07

Phenol 194.11 1.94 192.17 0.00 -3125.4 245.76

Acetone 0.00 0.00 0.00 0.00 0.00 0.00

AMS 14.78 14.63 0.15 0.00 -2426.4 202.20

H2 O 0.00 0.00 0.00 0.00 0.00 0.00

H2 0.00 0.00 0.00 0.00 0.00 0.00

For Condenser: For Reboiler:

R= 42.55 HF+QR=HD+HB+QC
QC= (1+R) Dλ

51
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-13:Q of T-(103).

Q (kJ/hr)

QF QD QB QC QR

0.00 -42758.23 267201.89 -34243052.26 3.45E+07

Distillation column T-(104):

Figure 4-11:Distillation column T-(104)

52
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-14:Component’s molar flow, enthalpy and temperature of T-(104).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component
SF SD SB 𝐓𝐅 𝐓𝐃 𝐓𝐁 𝐓𝐫𝐞𝐟 𝐇𝐅 𝐇𝐃 𝐇𝐁

Cumene 0.00 0.00 0.00 454.00 454.00 464.00 454.00 0.00 0.00 0.00

O2 0.00 0.00 0.00 0.00 0.00 0.00

N2 0.00 0.00 0.00 0.00 0.00 0.00

Methanol 0.00 0.00 0.00 0.00 0.00 0.00

CHP 0.00 0.00 0.00 0.00 0.00 0.00

DMBA 0.00 0.00 0.00 0.00 0.00 0.00

ACP 4.93 0.25 4.68 0.00 0.00 47053.37

Phenol 192.17 184.48 7.69 0.00 0.00 2604.50

Acetone 0.00 0.00 0.00 0.00 0.00 0.00

AMS 0.15 0.15 0.00 0.00 0.00 0.00

H2 O 0.00 0.00 0.00 0.00 0.00 0.00

H2 0.00 0.00 0.00 0.00 0.00 0.00

For Condenser: For Reboiler:

R= 404.52 HF+QR=HD+HB+QC
QC= (1+R) Dλ

53
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-15:Q of T-(104).

Q (kJ/hr)

QF QD QB QC QR

0.00 0.00 240274.55 -4.40E+09 4.41E+09

Reactor R-(103):

Figure 4-12:Reactor R-(103)

C6H5C(CH2)CH3 (ℓ) + H2(g) → C6H5CH(CH2)CH3 (ℓ) (4.13)

At T = 25 ℃

𝑟6 ∆𝐻𝑟6 = -3.96E+04 KJ/kmol.

Assuming 𝑇𝑟𝑒𝑓 in reaction is equal to 25 ℃.

54
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

Table 4-16:Component’s molar flow, enthalpy and temperature of R-(103).

Flowrate (kmol/hr) T °𝑲 H (kJ/kmol)

Component Tin 𝐓𝐢𝐧 𝐓𝐨𝐮𝐭 𝐓𝐨𝐮𝐭

S12 S16 S17 S18 Of Of Of Of 𝐓𝐫𝐞𝐟 S12 S16 S17 S18
S12 S16 S17 S18

Cumene 0 0 15 0 338 338 338 338 298 7814 0 7814 0

O2 0 0 0 0 0 0 0 0

N2 0 0 0 0 0 0 0 0

Methanol 0 0 0 0 0 0 0 0

CHP 0 0 0 0 0 0 0 0

DMBA 0 0 0 0 0 0 0 0

ACP 0 0 0 0 0 0 0 0

Phenol 2 0 0 0 8109 0 8108 0

Acetone 0 0 0 0 0 0 0 0

AMS 15 0 0 0 7449 0 0 0

H2 O 0 0 0 0 0 0 0 0

H2 0 59 0 44 0 1290 0 1290

Q (kJ/hr) -1.74E+06

55
CHAPTER FOUR: ENERGY BALANCE ||PHENOL

References

[1] R. K. Sinnott, Coulson & Richardson's Chemical Engineering. Vol. 6, Chemical Engineering
Design, Butterworth-Heinemann, 3rd Ed., 1999.
[2] David M. Himmelblau, James B. Riggs, Basic Principles and Calculation in Chemical
Engineering, seventh edition,
[3] Perry’s chemical engineer’s handbook, McGraw-Hill, seventh edition,1997.
[4] R Harry Silla, Chemical process engineering Design and Economics, Stevens Institute of
Technology, 2003.
[5] Aspen technology Inc. HYSYS v3.2.
[6] Mahmoud M. El-Halwagi, sustainable design through process integration, Elsevier Inc.
,2012.

56
CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Chapter 5: Heat Integration

Introduction
Heating and cooling are the most common operations in the processes. Significant quantities of
external heating and cooling utilities are used to drive reaction, induce separation, and render units
and streams in desirable states of operation. To satisfy the need for heating and cooling, industrial
operations require the extensive use of different forms of energy. The excessive usage of external
heating utilities incurs a substantial economic burden in the form of operating costs, depletes
unsustainable energy resources, and generates large quantities of greenhouse gas emissions.
Consequently, considerable attention has been given to the problem of conserving energy through
heat integration and the synthesis of heat-exchange networks (HENs).

The basic idea for heat integration is that there are process streams and units that need to be
heated and other process streams and units that need to be cooled. Before using external utilities
to provide the necessary heating and cooling, heat integration seeks to transfer the heat from the
process hot streams and units to the process cold streams and units. The remaining heating and
cooling tasks are then fulfilled using the external heating and cooling utilities.

Figure 5-1: Synthesis of HENs

For heat-exchange to be practically feasible, a minimum heat-exchange driving force (referred
to as∆𝑇 𝑚𝑖𝑛 ) should be employed. This minimum driving force can be used to establish a one-to-
one correspondence between the temperatures of the hot and the cold streams for which heat
transfer is feasible, that is:
𝑇 = 𝑡 + ∆𝑇 𝑚𝑖𝑛 ………………………………………………………………….. (5.1)

Where:

T ≡ The temperature of the hot stream.

t ≡ The temperature of the cold stream.

∆𝑇 𝑚𝑖𝑛 ≡ Minimum heat-exchange driving force.

57
CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Minimum utility target can be determined by:

1. The thermal pinch diagram (graphical).

2. The algebraic cascade diagram.
The algebraic cascade diagram is used since it provides the exact value of the minimum
utility targets.

Minimum utility targets using the algebraic cascade diagram

This method is developed by Linnhoff and Flower (1978). The first step is the construction of
a temperature-interval diagram (TID). Two corresponding temperature scales are generated: hot
and cold. Next a table of exchangeable heat loads (TEHL) is constructed to determine the heat-
exchange loads of the process streams in each temperature interval. The exchangeable load of the
uth hot stream (losing sensible heat) that passes through the zth interval is defined as:

𝐻𝐻𝑢,𝑧 = 𝐹𝑢 𝐶𝑝,𝑢 (𝑇𝑧−1 − 𝑇𝑧 )

……………………………………………………………………….. (5.2)
Where:

𝐹𝑢 ≡ Flowrate of the hot stream.

𝐶𝑝,𝑢 ≡ Heat capacity of the hot stream.

𝑇𝑧−1 and 𝑇𝑧 are the hot-scale temperatures defining the zth interval.
The exchangeable capacity of the vth cold stream (gaining sensible heat) that passes through
th
the z interval is computed through:

𝐻𝐶𝑣,𝑧 = 𝑓𝑣 𝑐𝑝,𝑣 (𝑡𝑧−1 − 𝑡𝑧 )

…………………………………………………………………………… (5.3)
Where:

𝑓𝑣 ≡ Flowrate of the cold stream.

𝐶𝑝,𝑣 ≡ Heat capacity of the cold stream.

𝑡𝑧−1 and 𝑡𝑧 arethe cold-scale temperature defining the zth interval.

After determining the loads and capacity for each interval, the collective load and capacity can
be obtained by summing up the individual loads of the hot streams or capacity of the cold streams
that pass through specific interval, that is:

𝐻𝐻𝑧𝑡𝑜𝑡𝑎𝑙 = ∑𝑢 𝑝𝑎𝑠𝑠𝑠 𝑡ℎ𝑟𝑜𝑢𝑔ℎ 𝑖𝑛𝑡𝑒𝑟𝑣𝑎𝑙 𝑧 𝐻𝐻𝑢,𝑧 ……………………………………… (5.4)

𝑤ℎ𝑒𝑟𝑒 𝑢=1,2,…,𝑁𝐻

Similarly, the collective cooling capacity of the cold process streams within the z th interval is
calculated as follows:

𝐻𝐶𝑧𝑡𝑜𝑡𝑎𝑙 = ∑𝑣 𝑝𝑎𝑠𝑠𝑒𝑠 𝑡ℎ𝑟𝑜𝑢𝑔ℎ 𝑖𝑛𝑡𝑒𝑟𝑣𝑎𝑙 𝑧 𝐻𝐶𝑣,𝑧 ………………………….. (5.5)

𝑤ℎ𝑒𝑟𝑒 𝑣=1,2,…,𝑁𝐶

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Within each temperature interval, it is thermodynamically as well as technically feasible to

transfer heat from a hot process stream to a cold process stream. Moreover, it is feasible to pass
heat from a hot process stream in an interval to any cold stream in a lower interval. Hence, for the
zth temperature interval, heat-balance equation can be written as follow:

𝑟𝑧 = 𝐻𝐻𝑧𝑡𝑜𝑡𝑎𝑙 − 𝐻𝐶𝑧𝑡𝑜𝑡𝑎𝑙 + 𝑟𝑧−1 ………………………………………… (5.6)

Where: 𝑟𝑧 and 𝑟𝑧−1 are the residual heats entering and leaving the zth interval. (1)
Table 5-1:Heat integration calculations

Stream Cp(kj/kgk) load(kj/h.k) Ts Tt Q(kj/hr)

s14-AMS H1 280.90 4745.11 369.00 338.00 -147098.48
s5-oxidizer H2 329.98 82035.25 373.00 328.00 -3691586.30
s4-Air C1 29.09 136524.52 335.00 393.00 7891117.03
s7-cleavage C2 166.70 75940.74 328.00 393.00 4936147.95

Table 5-2: Temperature -interval diagram.

Th Tc

403 393
` 1 369 359
2 H1 338 328
C2
3 335 325 Pinch point
4 320 310 C1
H2
5 310 300

59
CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Table 5-3:TEHL for hot streams.

Interval H1 H2 Htotal

1 0.00 0.00 0

2 147098.48 0.00 147098.48

3 0.00 0.00 0.00

Pinch

4 0.00 2047867.74 2047867.74

5 0.00 1365245.16 1365245.16

Table 5-4:TEHL for cold streams.

Interval C2 C1 Ctotal

1 2581985.08 0.00 2581985.083

2 2354162.87 0.00 2354162.87

3 0.00 246105.75 246105.75

Pinch

4 0.00 1230528.77 1230528.77

5 0.00 0.00 0.00

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Cascade diagram:

0 1 2581985
-2581985

147098,5 2 2354163
-4789049

0 3 246105,8
-5035155
Hu
2047868 4 1230529
-4217816

1365245 5 0
-2852571

Figure 5-2: Cascade diagram of the phenol process.

All negative residual heats can be made nonnegative by adding a hot load equals to the most
𝑚𝑖𝑛
negative𝑟𝑧 . This load is referred to as the minimum heating utility requirement, 𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 . Once
this hot load is added, the cascade is revised.
The load leaving the last temperature interval is the minimum cooling utility
𝑚𝑖𝑛
requirement,𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 .

The most negative hot load = -5035155.226 kJ/h.

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Revised cascade diagram:

5035155

0 1 2581985
2453170

147098,5 2 2354163
246106

0 3 246106
0
Pinch point
2047868 4 1230529
817339

1365245 5 0

2182584 Cu

Figure 5-3: Revised cascade diagram of the phenol process.

The load leaving the last temperature interval is the minimum cooling utility
𝑚𝑖𝑛
requirement,𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 .

A zero-residual heat designates the thermal pinch location.

Stream matching and synthesis of heat-exchange networks

For matching streams two rules should be satisfied:
Stream population rules
Above the pinch:

𝑁ℎ𝑎 ≤ 𝑁𝑐𝑎 ……………………………………………………………………….. (5.7)

Where:

𝑁ℎ𝑎 ≡ Number of hot streams.

𝑁𝑐𝑎 ≡ Number of cold streams

Below the pinch:

𝑁𝑐𝑎 ≤ 𝑁ℎ𝑎 ………………………………………………………………………. (5.8)

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Flowrate × heat capacity rules:

Above the pinch

𝐹𝑢 𝐶𝑝,𝑢 ≤ 𝑓𝑣 𝑐𝑝,𝑣 ………………………………………………………………….. (5.9)

Below the pinch

𝑓𝑣 𝑐𝑝,𝑣 ≤ 𝐹𝑢 𝐶𝑝,𝑢 ………………………………………………………………… (5.10)

Hu
393 C2
369 4789049 4789049
H1 329,937
328
147098,4804 147098,5
C1
338 246105,8 246105,8
328

Pinch

Figure 5-4 : Stream matching above the pinch.

335 325
Pinch
H2 C1

1230529 1230529
325,986756
2182584 2182584
Cu 310
310

Figure 5-5 : Stream matching below the pinch.

𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 (before heat integration) = -3587516.3 kJ/hr

𝑚𝑖𝑛
𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 (after heat integration) = -5035155.226 kJ/hr
𝑚𝑖𝑛
(𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 − 𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 )
Saving in cooling utility requirement = × 100% ………… (5.11)
𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔

∴ Saving =40.35%

𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 (before heat integration) = 6412782.47 kJ/hr

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

𝑚𝑖𝑛
𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 (after heat integration) = 2182584 kJ/hr
𝑚𝑖𝑛
(𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 − 𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 )
Saving in heating utility requirement = × 100% ………… (5.12)
𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔

∴ Saving =65.97%

Total Q before heat integration = 𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 + 𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 ……………………….. (5.13)

∴ Total Q before heat integration = 10000298.76 kJ/hr

𝑚𝑖𝑛 𝑚𝑖𝑛
Total Q after heat integration = 𝑄𝑐𝑜𝑜𝑙𝑖𝑛𝑔 + 𝑄ℎ𝑒𝑎𝑡𝑖𝑛𝑔 ………………………… (5.14)

∴ Total Q after heat integration =7217739 kJ/hr

Total saving in energy =27.82%

∆𝑇 𝑚𝑖𝑛 in these calculations is equal to 10 ℃.

LINGO Code
5.3.2.1 Targeting code
min=((6/1000000*Qhmin)+(8/1000000*Qcmin))*8000*3600;
!Qhmin is the minimum heating utility required;
!Qcmin is the minimum cooling utility required;
!r is the heat residual;
r1-Qhmin=-2581985.1;
r2-r1=-2207064.4;
r3-r2=-246105.75;
r4-r3=817338.973;
-r4+Qcmin=1365245.16;
r1>=0;
r2>=0;
r3>=0;
r4>=0;
Qhmin>=0;
Qcmin>=0;

5.3.2.1.1 Solution obtained by LINGO:

Global optimal solution found.
Objective value: 0.1372942E+10
Infeasibilities: 0.000000
Total solver iterations: 0
Elapsed runtime seconds: 0.37
Model Class: LP
Total variables: 6

64
CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Nonlinear variables: 0
Integer variables: 0
Total constraints: 12
Nonlinear constraints: 0
Total nonzeros: 18
Nonlinear nonzeros: 0
Variable Value Reduced Cost
QHMIN 5035155. 0.000000
QCMIN 2182584. 0.000000
R1 2453170. 0.000000
R2 246105.8 0.000000
R3 0.000000 403.2000
R4 817339.0 0.000000

Row Slack or Surplus Dual Price

1 0.1372942E+10 -1.000000
2 0.000000 172.8000
3 0.000000 172.8000
4 0.000000 172.8000
5 0.000000 -230.4000
6 0.000000 -230.4000
7 0.000000 2453170
8 0.000000 246105.8
9 0.000000 0.000000
10 0.000000 817339.0
11 0.000000 5035155
12 0.000000 2182584

65
CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

5.3.2.2 Matching of streams code

min=E212+E311+E321+E111+E121+E232;
!Balance of H1;
r13-r12+Q113=0;
r14-r13+Q114=0;
-r14+Q135=0;
!Balance of H2;
r24+Q214=2047868;
!Balance of H3;
r31+Q321=5035155;
r32-r31+Q322=0;
r33-r32+Q313=0;
r34-r33+Q314=0;
-r34=0;
!Balance of C1;
Q313=246105.7533;
Q214=1230528.767;
!Balance of C2;
Q321=2581985.08;
Q122=2354162.87;
!Balance of C3;
Q235=2182584;
!Matching of loads;
Q113+Q112<=147098.5*E111;
Q313<=246105.7533*E311;
Q321+Q322<=4936147.95*E321;
Q214<=1230528.767*E212;
Q234+Q235<=2182584*E232;
!BINARY CONTRAINS;
@BIN(E111);
@BIN(E311);
@BIN(E321);
@BIN(E212);
@BIN(E232);
!Non negativity constrains;
r12>=0;
r13>=0;
r14>=0;
r24>=0;
r31>=0;
r32>=0;
r33>=0;
r34>=0;
Q112>=0;
Q113>=0;
Q114>=0;
Q122>=0;
Q135>=0;
Q214>=0;
Q235>=0;;
Q321>=0;
Q322>=0;
Q313>=0;
Q314>=0;

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Solution obtained by LINGO:

Global optimal solution found.

Objective value: 4.000000

Objective bound: 4.000000

Infeasibilities: 0.000000

Extended solver steps: 0

Total solver iterations: 0

Elapsed runtime seconds: 0.16

Model Class: MILP

Total variables: 18

Nonlinear variables: 0

Integer variables: 5

Total constraints: 31

Nonlinear constraints: 0

Total nonzeros: 40

Nonlinear nonzeros: 0

Variable Value Reduced Cost

E212 1.000000 1.000000

E311 1.000000 1.000000

E321 1.000000 1.000000

E111 0.000000 1.000000

E121 0.000000 1.000000

E232 1.000000 1.000000

R13 0.000000 0.000000

R12 0.000000 0.000000

Q113 0.000000 0.000000

R14 0.000000 0.000000

Q114 0.000000 0.000000

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

Q135 0.000000 0.000000

R24 817339.2 0.000000

Q214 1230529. 0.000000

R31 2453170. 0.000000

Q321 2581985. 0.000000

R32 2453170. 0.000000

Q322 0.000000 0.000000

R33 2207064. 0.000000

Q313 246105.8 0.000000

R34 0.000000 0.000000

Q314 2207064. 0.000000

Q122 2354163. 0.000000

Q235 2182584. 0.000000

Q112 0.000000 0.000000

Q234 0.000000 0.000000

Matlab code
5.3.3.1 Targeting code
Aeq=[1 0 0 0 -1 0
-1 1 0 0 0 0
0 -1 1 0 0 0
0 0 -1 1 0 0
0 0 0 -1 0 1];
beq=[-6373957.61 -521720.01 -3016437.4 75877.3795 820352.5];
LB = zeros(5,1); UB = [Inf;Inf;Inf;Inf;Inf;Inf];
f=[0 0 0 0 172.8 230.4];
[X,FVAL] = linprog(f,[],[],Aeq,beq,LB,UB)

5.3.3.1.1 Solution obtained by Matlab

=X
* e+061.0
3.5382
3.0164
0.0000

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

0.0759
9.9121
0.8962
= FVAL
1.9193e+09

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CHAPTER FIVE: HEAT INTEGRATION ||PHENOL

References

[1] El-Halwagi, M. (2006). Process Integration. Burlington: Elsevier.

[2] M. Wagialla, P., 2017. Introduction To MATLAB Applications In Chemical Engineering. 1st
ed.

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Chapter Six: Equipment Design

Bubble Column Reactor
Introduction
Every industrial chemical process is designed to produce economically a desired product from
a variety of starting materials (raw material) through a succession of treatment steps. The raw
materials undergo a number of physical treatment steps to put them in the form in which they can
be reacted chemically. [1] The chemical treatment is the heart of the process and that makes or
break the process economically.
Design of the reactor is no routine matter, and many alternatives can be proposed for a process.
In searching for the optimum it is not just the cost of the reactor that must be minimized. One
design may have low reactor cost, but the materials leaving the unit may be such that their
treatment requires a much higher cost than alternative designs. Hence, the economics of the overall
process must be considered. [1]
Reactor design uses information, knowledge, and experience from a variety of areas
thermodynamics, chemical kinetics, fluid mechanics, heat transfer, mass transfer, and economics.
To find what a reactor is able to do we need to know the kinetics, the contacting pattern and the
performance equation. [1]

Figure 6-1: Information needed to predict what a reactor can do.[1]

In reactor design we want to know what size and type of reactor and method of operation are
best for a given job. Because this may require that the conditions in the reactor vary with position
as well as time, this question can only be answered by a proper integration of the rate equation for
the operation. (1) Types of reactors is shown in Fig 6.2.

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Figure 6-2:Broad classification of reactor types. (a) The batch reactor. (b) The steady-state flow
reactor. (c), (d), and (e) Various forms of the semibatch reactor. [1]

The starting point for any design is the material balance, illustrated in Fig 6.3.

Figure 6-3: Material balance for an element of volume of the reactor. [1]

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

In nonisothermal operations energy balances must be used with material balances, illustrated in
Fig 6.4.

Figure 6-4: Energy balance for an element of volume of the reactor. [1]

Fluid-Fluid Reactors
We must first choose the right kind of contactor, then find the size needed. There are two kinds
of contactor-towers and tanks, and Fig. 6.5 shows some examples. As may be expected, these
contactors have widely different GIL volume ratios, interfacial areas, kg and kl, and concentration
driving forces. The particular properties of the system you are dealing with, the solubility of
gaseous reactant, the concentration of reactants, etc.-in effect the location of the main resistance
in the rate equation-will suggest that you use one class of contactor and not the other. Reactions in
such reactors are made to take place for one of three reasons. For the product of reaction may be a desired
material. (1)

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Figure 6-5: Tower and tank contactors for G/L reactions.[1]

Bubble Column Reactor

Bubble columns are intensively used as multiphase contactors and reactors in chemical,
biochemical and petrochemical industries. They provide several advantages during operation and
maintenance such as high heat and mass transfer rates, compactness and low operating and
maintenance costs. Three-phase bubble column reactors are widely employed in reaction
engineering, i.e. in the presence of a catalyst and in biochemical applications where
microorganisms are utilized as solid suspensions in order to manufacture industrially valuable
bioproducts.
Investigation of design parameters characterizing the operation and transport phenomena of
bubble columns have led to better understanding of the hydrodynamic properties, heat and mass
transfer mechanisms and flow regime characteristics ongoing during the operation.[2]

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Figure 6-6: Scheme of a bubble column (5)

A successful design and scale-up of bubble columns require an advanced understanding of

multiphase fluid dynamics. The design and scale-up of bubble column reactors generally depend
on three main phenomena: (i) heat and mass transfer characteristics; (ii) mixing characteristics;
(iii) system. The main interest of published studies is concentrated on influence of a length-to-
diameter ratio of the column, fluid dynamics and regime analysis and characteristic parameters,
especially gas holdup, bubble characteristics, and mass and heat transfer coefficients. (5)
Gas Holdup
Gas holdup is a dimensionless key parameter for design purposes that characterizes the
transport phenomena of bubble column systems which is basically defined as the volume fraction
of gas phase occupied by the gas bubbles. Most studies conclude that the temperature and column
size effects on gas holdup are not significant. Gas holdup in bubble columns depend mainly on
superficial gas velocity which is defined as the average velocity of the gas that is sparged into the
column. In calculations, superficial gas velocity is simply expressed as the volumetric flow rate
divided by the cross-sectional area of the column.(5)One of various correlations predicting gas
holdup in bubble columns as a function of superficial gas velocity is the following:

……………………………………… (6.1)

Where superficial gas velocity =0.4m/s [2]

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Bubble Characteristics
Bubble size has a significant impact on heat and mass transfer coefficients in a bubble size
column. Various studies proposed methodologies to follow the estimation of bubble properties.
One of the key parameters affecting bubble size is a gas sparger type. Small orifice diameter plates
enable the formation of smaller sized bubbles. (5)A simple correlation for size of bubbles produced
at an orifice was proposed by Moo-Young M:

…………………………… (6.2)

Table 6-1 : properties of reactor inlet

g= 10 m/s2
ρl = 862 Kg/m3
ρg = 1.429 Kg/m3
d0= 0.005 m
σ= 0.02769 Kg/s2

Mass Coefficient
In gas-liquid reactors, mass transfer from the gas to liquid phase is the most important goal
of the process. Therefore, it is important to estimate the mass transfer coefficients for design and
scale up of the reactor. Published studies propose superficial gas velocity as the main parameter
affecting the mass transfer coefficient. (3)The simplest correlation used:

…………………………………………………………… (6.3)

………………………………………………………(6.4)

Heat Coefficients
Thermal control is of importance since chemical reactions are typically accompanied by heat
supply or removal operation. Therefore, turbulent heat transfer from the reactor wall and inserted
coils to the liquid is a major topic of literature research. Bubble columns are known for their
excellent heat transfer characteristics. [3]

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Correlations used:

…………………………………………………… (6.5)

…………………………………………………… (6.6)

…………………………………………………… (6.7)

…………………………………………………… (6.8)

…………………………………………………… (6.9)

Reaction and Rate Calculations

The main reaction is the oxidation of cumene to cumene hydroperoxide in the following
reaction:

…………………… (6.10)

Rate equation:

−𝑟𝐴′′′′ = −𝑟𝐵′′′′ = 𝑘𝑙 𝑎(𝐶𝐴𝐼 − 𝐶𝐴 ) , kmol/cm-sec …………………………….. (6.11)

A= Oxygen

B= Cumene

𝐶𝐴𝐼 = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑂2 𝑖𝑛 𝑡ℎ𝑒 𝑏𝑢𝑏𝑏𝑙𝑒 , kmol/m3

𝐶𝐴 = 𝐵𝑢𝑙𝑘 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑂2 𝑖𝑛 𝑡ℎ𝑒 𝐶𝑢𝑚𝑒𝑛𝑒 , kmol/m3

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Volume of the Reactor

𝑉 𝐶𝐴2 𝑑𝐶𝐴
= ∫𝐶𝐴1 (−𝑟 ′′′′) ……………………………………………………… (6.12)
𝐶𝑇 𝐴

𝐶𝑇 = 𝑇𝑜𝑡𝑎𝑙 𝑐𝑢𝑚𝑒𝑛𝑒 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 , kmol/m3

V= Reactor’s volume, m3

Residence Time Calculation

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑣𝑒𝑠𝑠𝑒𝑙
𝛤= , hr …………………………………………….. (6.13)
𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒

Pressure Drop
∆𝑃 = (𝜌𝑔 𝜀𝑔 + 𝜌𝐿 𝜀𝐿 )𝑔 ∗ ∆𝐻 , Kpa …………………………………………. (6.14)

𝜌𝑔 = 𝑂𝑥𝑦𝑔𝑒𝑛 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 , kg/m3

𝜌𝐿 = 𝐶𝑢𝑚𝑒𝑛𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 , kg/m3

𝜀𝐿 = 0.9 (1)

∆𝐻 = 𝐻𝑒𝑖𝑔ℎ𝑡, 𝑚

Mechanical Design
By using Sparger selection

Porous plate distributor is selected because:

• Low price

• Easy manufacturing

• Variety of specifications [4]

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Figure 6-7 : Porous plate sparger. (4)

Thickness
Rule of thumb optimal length/diameter ratio is in range of 2.5-5, usually taken as 3.

L=3*D ……………………………………………………………………………. (6.15)

D =1.678m

L= 5.035m

Vessel thickness
Assumptions:

1. Design pressure of the vessel is 10% above the operating pressure.

2. The Material of construction is carbon steel.
3. The welding efficiency is 85%.
4. A corrosion allowance of 3 mm.

Thickness depends on the operating pressure and temperature beside material of construction.

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Figure 6-8 : Design stress chart (3)

……………………………………………………………............... (6.16)

t ≡ Thickness.

Design stress for carbon steel at 120 °C, 121 N/mm

Internal pressure=0.000152N/mm2

Corrosion allowance=3 mm

By taking design pressure 10% above operating pressure:

Therefore, wall thickness =3mm

Outside diameter = 1.68m

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Specification Sheet
Table 6-2: specification sheet

Type Bubble column Reactor

Volume 11.137 m3

Residence time 0.405906922 h

Height 5.035 m

Diameter 1.678 m

Temperature 37C

Working pressure 151.988 kpa

Wall thickness 3 mm

Sparger type Porous plate

Pressure drop 39 kpa

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Cleavage reactor design

Introduction
In any manufacturing process where there is a chemical change taking place, the reactor will be
the heart of the process. Its main purpose is to give specific products from a given reactants. Design
of the reactor is no routine matter, and many alternatives can be proposed for a process. In
searching for the optimum, it is not just the cost of the reactor that must be minimized.

Reactor design uses information, knowledge, and experience from a variety of areas;
thermodynamics, chemical kinetics, fluid mechanics, heat transfer, mass transfer, and economics.
A chemical reaction is a process that results in the conversion of chemical substances. The
substance or substances initially involved in a chemical reaction are called reactants. These
reactants are characterized by a chemical change and they yield one or more products. These
products are generally different from the original reactants. Chemical reactions may be of different
nature depending on the type of reactants, type of product desired, conditions and time of the
reaction, for example: synthesis, decomposition, displacement, precipitation, isomerization, acid-
base, redox or organic reactions.

Reactors are designed based on features like mode of operation or types of phases present or
the geometry of reactors. They are thus called:

1. Batch or continuous depending on the mode of operation.

2. Homogeneous or heterogeneous depending upon the phases present.

They may also be classified as:

1. Stirred Tank Reactor.

2. Tubular Reactor.
3. Packed Bed Reactor.
4. Fluidized Bed Reactor.

Stirred tank reactors

Stirred tank (agitated) reactors consist of a tank fitted with a mechanical agitator and a cooling
jacket or coils. They are operated as batch reactors or continuously. Several reactors may be used
in series. The stirred tank reactor can be considered the basic chemical reactor, modeling on a large
scale the conventional laboratory flask. Tank sizes range from a few liters to several thousand
liters. They are used for homogeneous and heterogeneous liquid-liquid and liquid-gas reactions,
and for reactions that involve finely suspended solids, which are held in suspension by the
agitation.

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

An agitator is introduced to disperse the reactants thoroughly into the reaction mixture
immediately they enter the reactor. The product is continuously drawn out and that is why it is
known for perfect mixing. Compositions at outlet and inside reactor are the same.

CSTRs are best suitable for liquid phase reactions.

Figure 6-9 : CSTR

6.2.2.1 Comparison between batch and continuous stirred reactors:

Batch
Advantages:

1. Suitable for small scale production.

2. Suitable for processes where a range of different products or grades is to be produced in
the same equipment.
3. Suitable for reactions requiring long reaction times.
4. Suitable for reactions with superior selectivity.

Limitations:

1. Not suitable for large batch sizes

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

2. It is a closed system in which once the reactants are added in the reactor, they will come
out as products only after the completion of the reaction

Continuous stirred tank reactor (CSTR)

Advantages:

1. One or more fluid reagents are introduced into a tank reactor equipped with an impeller
while the reactor effluent is recovered. A stepped-up concentration gradient exists
2. Highly flexible device.
3. By products may be removed in between the reaction.
4. It is economically beneficial to operate several CSTRs in series or in parallel.
5. Reaction can be carried out in horizontal as well as vertical reactors.

Limitations:

1. Chemical industry especially involving liquid/gas reactions.

Continuous stirred tank reactor design

Assumptions:

1. CSTR is operating at steady state (accumulation = 0).

2. All calculations performed with continuous reactor assumed perfect mixing.
3. Conversion 100%.
4. First order reaction.

Reaction kinetics:
The following reaction occur in a mixed flow reactor:

C6H5COOH (CH3)2 (ℓ) → C6H5OH (g) + (CH3)2CO (g)

The composition of A is uniform in liquid phase, and the rate equation is:

-𝑟𝐴′′′′ = 𝑘 ′′′′ × 𝐶𝐴 …………………………………………………………………………… (6.17)

A ≡ CHP .

The limiting reactant is CHP.

𝐸𝑎
𝑘 ′′′′ = 𝐴 × 𝑒−(𝑅𝑇) …………………………………………………………………………… (6.18)

𝑘 ′′′′ ≡ Reaction rate constant 𝑠 −1 .

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

𝐿𝑛(𝐴) ≡ Frequency or pre-exponential factor, 9.14638. (6)

𝐸𝑎 ≡ Activation energy of the reaction, 38500 𝐽/𝑘𝑚𝑜𝑙. (6)

𝑅 ≡ Gas constant, 8.314 𝐽/𝑚𝑜𝑙 𝐾.

Since the conversion is 100% then CA=CA0

𝑁
𝐶𝐴𝑜 = 𝑣 ……………………………………………………………………… (6.19)
𝑜

K= 0,006931078 𝑠 −1

Where:

𝑁 ≡ Inlet flowrate of CHP, 0,053379 𝑘𝑚𝑜𝑙/𝑠.

𝑣𝑜 ≡ Volume of solution 28.63644 𝑚3 ⁄ℎ𝑟.

𝐶𝐴 ≡ Concentration of CHP 𝑘𝑚𝑜𝑙/𝑚3 .

𝐶𝐴𝑜 ≡ Initial concentration of CHP 𝑘𝑚𝑜𝑙/𝑚3 .

𝑃 ≡ Operating pressure, 253.312 𝑘𝑃𝑎.

𝑇 ≡ Operating temperature, 55 ℃.

𝐶𝐴𝑜 = 6.710526 𝑘𝑚𝑜𝑙/𝑚3 .

∴ −𝑟′′′′𝐴 = 0.046511183 𝑘𝑚𝑜𝑙 ⁄𝑚3 . 𝑠

−𝑟′′′′𝐴
(𝐶𝐴𝑜 ) = 𝑉𝑟 …………………………………………………………………… (6.20)
𝐹𝐴𝐶𝑇 𝐹𝑙

Where:

𝑉𝑟 ≡ Volume of reactor 𝑚3 .

𝐹𝑙 ≡ Inlet flowrate of CHP kmol/hr.

𝐶𝑇 ≡ Total concentration of liquid 𝑘𝑚𝑜𝑙/𝑚3 .

∴ 𝑉𝑟 =1.74 𝑚3 .

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Mechanical design
Rule of thumb optimal length/diameter ratio is in range of 2.5-5, usually taken as 3.

𝐿 = 3 × 𝐷 ……………………………………………………………………… (6.21)

D = 0.9 𝑚

L= 2.7 𝑚

6.2.3.1.1 Vessel thickness

Assumptions:

1. Design pressure of the vessel is 10% above the operating pressure.

2. The Material of construction is carbon steel.
3. The welding efficiency is 85%.
4. A corrosion allowance of 3 mm.

Thickness depends on the operating pressure and temperature beside material of construction.

Table 6-3 : Typical design stresses for plate thickness..

𝑃𝑖 ×𝐷𝑖
𝑡= + 𝐶 ……………………………………………………………………………………… (6.22)
2×𝑓−𝑃𝑖

T≡ Thickness.

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𝑓 ≡ Design stress for carbon steel at 190 °C, 107.01 𝑁⁄𝑚𝑚2.

𝑃𝑖 ≡ Internal pressure, kPa.

𝐶 ≡ Corrosion allowance, 3 mm.

By taking design pressure 10% above operating pressure:

Therefore, wall thickness = 3 𝑚𝑚

∴ Outside diameter = 𝐷𝑖 + 𝑡 = 0.9 𝑚

Reactor head
The ends of a cylindrical vessel are closed by heads of various shapes. The principal types used
are:

1. Flat plates and formed flat heads.

2. Hemispherical heads.
3. Ellipsoidal heads.
4. Tropospherical heads.

Ellipsoidal head is used for pressure greater than 150 atm and for less than that pressure we use
tropospherical head.

Vessel supports
The method used to support a vessel will depend on the size, shape, and weight of the vessel,
the design temperature and pressure, the vessel location and arrangement, and the internal and
external fittings and attachments.

Brackets, or lugs, are used for all types of vessel. The supports must be designed to carry the
weight of the vessel and contents, and any superimposed loads, such as wind loads.

Supports will impose localized loads on the vessel wall, and the design must be checked to
ensure that the resulting stress concentrations are below the maximum allowable design stress.
They should be designed to allow easy access to the vessel and fittings for inspection and
maintenance.

Impeller sizing and speed calculation

Selection criteria of impeller:
The impeller selected is pinched blade turbine, because:

1. Efficient turbulence flow impeller for blending immiscible liquids.

2. Combine axial and radial flows are achieved.

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3. Especially effective for heat exchange with vessel walls and internal coils.
4. It can operate at reasonable speed.
5. Low cost.
6. Wide application range.

Agitator dimensions
𝐷𝑎 = 𝐷𝑖 ⁄3 ……………………………………………………………………………………… (6.23)

𝐸𝑗 = 𝐷𝑎 ………………………………………………………………………………………… (6.24)

𝐿 = 𝐷𝑎 /4 ………………………………………………………………………………………… (6.25)

𝑊 = 𝐷𝑎 /5 ……………………………………………………………………………………… (6.26)

𝐽 = 𝐷𝑖 /10 ……………………………………………………………………………………… (6.27)

Where:

𝐷𝑎 ≡ Impeller diameter, 0.3 m.

𝐸𝑗 ≡ Impeller height above vessel floor, 0.3 m.

𝐿 ≡ Length of impeller blade, 0.08 m.

𝑊 ≡ Width of impeller blade, 0.06 m.

𝐽 ≡ Width of baffle, 0.09 m.

𝑁 = (𝑉𝑡 × 60)⁄(𝜋 × 𝐷𝑎 ) ………………………………………………………………. (6.28)

Where:

𝑁 ≡ Speed of the impeller, rpm (round per minute).

𝑉𝑡 ≡ Tip velocity, m/s.

Tip velocity is in the range of 3-6 m/s, now taken as 4.8 m/s.

N = 304 rpm

𝐴𝑐𝑡𝑢𝑎𝑙 𝑝𝑜𝑤𝑒𝑟 = (𝑁𝑝 × 𝜌 × 𝑁 3 × 𝐷𝑎5 )⁄𝐼𝑚𝑝𝑒𝑙𝑙𝑒𝑟 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 ………………… (6.29)

By assuming an impeller efficiency of 85% and number of power of 0.25:

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∴ Actual power = 97 kW = 130 hp.

Shaft design
Material of construction is carbon steel.

𝑓𝑠 ≡ Shear stress = 105 𝑁 ⁄𝑚𝑚2 .

𝑇𝑐 = (𝐴𝑐𝑡𝑢𝑎𝑙 𝑝𝑜𝑤𝑒𝑟 × 75 × 60)/(2 × 𝑃𝑖 × 𝑁) ………………………………………………. (6.30)

𝑇𝑚 = 1.5 × 𝑇𝑐 ………………………………………………………………………… ……………… (6.31)

𝑍𝑝 = 𝑇𝑚 ⁄𝑓𝑠………………………………………………………………………… ………………… (6.32)

Where:

𝑇𝑐 ≡ Continuous average rated torque on the agitator shaft, 28414 kg.m.

𝑇𝑚 ≡ Main average rated torque on the agitator shaft, 42621 kg.m.

𝑍𝑝 ≡ Molar modulus of the shaft, 405 𝑐𝑚3 .

3 Zp ×16
Dshaft = √ π
………………………………………………………… ……………………… (6.33)

Where:

𝐷𝑠ℎ𝑎𝑓𝑡 ≡ Shaft diameter, 12 cm.

Table 6-4 : Design summary for R-(102).

Type Jacketed, stirred tank reactor

Volume 1.7 𝑚3

Height 2.7 m

Diameter 0.9 m

Temperature 55 ℃

Working pressure 2026.5 kPa

Type of head Tropospherical head

Wall thickness 3 mm

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Number of baffles 4

Reactor material of construction Carbon steel

Type of agitator Pinched bladed turbine

Number of blades 6

Impeller diameter 0.3 m

Length of blade 0.08 m

Width of blade 0.06 m

Impeller above vessel floor 0.09 m

Speed of impeller 304 rpm

Power required 97 kW

Shaft diameter 12 cm

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Hydrogenation Reactor
Assumptions
1. The catalyst activity was assumed to be constant (sulfer content was assumed to be
constant).
2. H2 was assumed to undergo dissociative adsorption on the catalyst surface.
3. Same sites for both H2 and reactant adsorption.
4. Other terms are incorporated into the hydrogenation rate constant (kHYD)

Reaction kinetics:
The following reaction occur in a mixed flow reactor:

C6H5C(CH2)CH3 (ℓ) + H2(g) → C6H5CH(CH2)CH3 (ℓ)

Rate equation:

𝑟𝐻𝑌𝐷 = 𝑘𝐻𝑌𝐷 𝐶𝑅 …………………………………………………………… (6.34)

𝑘𝐻𝑌𝐷 ≡hydrogenation rate constant, cm3∙min-1∙g-1

𝐶𝑅 ≡hydrogenation rate expression, mol∙min-1∙g-1

𝑘𝐻𝑌𝐷 =8,814 cm3∙min-1∙g-1 (7)

Weight of the catalyst

𝐹 𝑋𝑅
𝑊 = 𝐴𝑀𝑆 ……………………………………………………………………………………………. (6.35)
𝑟 𝐻𝑌𝐷
W≡ weight of the catalyst (Ni-Mo-S), g.
𝐹𝐴𝑀𝑆 ≡ AMS flow rate, mole/min
𝑋𝑅 ≡ Conversion of the AMS, 100%.

W=3628 g Ni-Mo-S (7)

Reactor’s volume
𝑊∗𝑟𝐻𝑌𝐷 ∗𝜏
𝑉𝑟 = ……………………………………………………………… (6.36)
𝐶𝑅
𝜏≡ Residence time, 133 min. (7)

𝑉𝑟 =4253116 cm3 =4.2 m3

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Acetone distillation column

Introduction
Distillation has long been used as the separation process in the chemical and petroleum
industries because of its reliability, simplicity, and low-capital cost.
Today, with 40,000 distillation towers in operation, distillation makes about 95% of all current
industrial separation processes. It is a process that separates two or more components into an
overhead distillate and bottoms. The separation is based on the relative volatility of the
components. Additional vapour phase is generated by the thermal means.
Only a brief review of the essential principles that determine the design procedure will be
mentioned. The design of a distillation column can be divided into the following steps:
1. Specify the degree of separation required: set product specifications.
2. Select the operating conditions: batch or continuous; operating pressure.
3. Select the type of contacting device: plates or packing.
4. Determine the stage and reflux requirements: the number of equilibrium stages.
5. Size the column: diameter, number of real stages.
6. Design the column internals: plates, distributors, packing supports.
7. Mechanical design: vessel and internal fittings.
The principal step will be to determine the stage and reflux requirements. This is a relatively
simple procedure when the feed is a binary mixture, but a complex and difficult task when the feed
contains more than two components (multicomponent).

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Step 1: Product specifications

The product specification demanded by the market is as follow:
Table 6-5: Product specifications.

Component 𝑥𝐷 𝑥𝐵

Cumene 0.01 0.13

ACP 0.00 0.02

Phenol 0.00 0.79

Acetone 0.92 0.00

AMS 0.00 0.06

H2O 0.07 0.00

Step 2: Selection of operating conditions

Types of the operation
The separation of liquid mixtures by distillation depends on differences in volatility between
the components. The greater the relative volatilities, the easier the separation. This operation is
classified into two types; batch and continuous operation. Batch operation should be considered
when the quantity to be distilled is small, when it is produced at irregular intervals, when a range
of products has to be produced or when the feed composition is likely to vary considerably.
The production of acrylic acid is not subjected to these factors. In addition, the distillation is
considered as multi-component system, which limits the choice to the continuous distillation.
Brief description of continuous distillation
In continuous distillation, the vapour flows up the column and liquid counter-currently down
the column. The vapour and liquid are brought into contact on plates, or packing. Part of the
condensate from the condenser is returned to the top of the column to provide liquid flow above
the feed point (reflux), and part of the liquid from the base of the column is vaporised in the re-
boiler and returned to provide the vapour flow.
In the section below the feed, the more volatile components are stripped from the liquid and
this is known as the stripping section. Above the feed, the concentration of the more volatile
components is increased and this is called the enrichment, or more commonly, the rectifying

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section. Figure (6.10) shows a column producing two product streams, referred to as tops and
bottoms, from a single feed.

Figure 6-10 : Distillation column.

Reflux considerations
The reflux ratio, R, is normally defined as:
Flow returned as reflux
𝑅= ……………………………………… (6.37)
Flow of top product taken off

The number of stages required for a given separation will be dependent on the reflux ratio used.
In an operating column, the effective reflux ratio will be increased by vapour condensed within
the column due to heat leakage through the walls. With a well-lagged column, the heat loss will
be small and no allowance is normally made for this increased flow in design calculations. If a
column is poorly insulated, changes in the internal reflux due to sudden changes in the external
conditions, such as a sudden rain storm, can have a noticeable effect on the column operation and
control.
Total reflux
Total reflux is the condition when all the condensate is returned to the column as reflux: no
product is taken off and there is no feed. At total reflux, the number of stages required for a given
separation is the minimum at which it is theoretically possible to achieve the separation. Though

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not a practical operating condition, it is a useful guide to the likely number of stages that will be
needed.
Columns are often started up with no product take-off and operated at total reflux till steady
conditions are attained. The testing of columns is also conveniently carried out at total reflux.
Minimum reflux
As the reflux ratio is reduced a pinch point will occur at which the separation can only be
achieved with an infinite number of stages. This sets the minimum possible reflux ratio for the
specified separation
Optimum reflux ratio
Practical reflux ratios will lie somewhere between the minimum for the specified separation
and total reflux. The designer must select a value at which the specified separation is achieved at
minimum cost. Increasing the reflux reduces the number of stages required, and hence the capital
cost, but increases the service requirements (steam and water) and the operating costs. The
optimum reflux ratio will be that which gives the lowest annual operating cost. No hard and fast
rules can be given for the selection of the design reflux ratio, but for many systems the optimum
will lie between 1.2 to 3 times the minimum reflux ratios.
At low reflux ratios, the calculated number of stages will be very dependent on the accuracy of
the vapour-liquid equilibrium data available. If the data are suspect a higher than normal ratio
should be selected to give more confidence in the design.
Feed-point location
The precise location of the feed point will affect the number of stages required for a specified
separation and the subsequent operation of the column. As a general rule, the feed should enter the
column at the point that gives the best match between the feed composition (vapour and liquid if
two phases) and the vapour and liquid streams in the column. In practice, it is wise to provide two
or three feed-point nozzles located round the predicted feed point to allow for uncertainties in the
design calculations and data, and possible changes in the feed composition after start-up
Selection of column pressure
Except when distilling heat-sensitive materials, the main consideration when selecting the
column operating-pressure will be to ensure that the dew point of the distillate is above that which
can be easily obtained with the plant cooling water.

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Vacuum operation is used to reduce the column temperatures for the distillation of heat-
sensitive materials -as acetone – and where very high temperatures would otherwise be needed to
distil relatively non-volatile materials. When calculating the stage and reflux requirements it is
usual to take the operating pressure as constant throughout the column. In vacuum columns, the
column pressure drop will be a significant fraction of the total pressure and the change in pressure
up the column should be allowed for when calculating the stage temperatures. This may require a
trial and error calculation, as clearly the pressure drop cannot be estimated before an estimate of
the number of stages is made.
Step 3: Selection of the contacting device
The choice between a plate and packed column for a particular application can only be made
with complete assurance by costing each design. However, this will not always be worthwhile, or
necessary, and the choice can usually be made, on the basis of experience by considering main
advantages and disadvantages of each type; which are listed below:
1. Plate columns can be designed to handle a wider range of liquid and gas flow-rates than
packed columns.
2. Packed columns are not suitable for very low liquid rates.
3. The efficiency of a plate can be predicted with more certainty than the equivalent term for
packing (HETP or HTU).
4. Plate columns can be designed with more assurance than packed columns. There is always
some doubt that good liquid distribution can be maintained throughout a packed column
under all operating conditions, particularly in large columns.
5. It is easier to make provision for cooling in a plate column; coils can be installed on the
plates.
6. It is easier to make provision for the withdrawal of side-streams from plate columns.
7. If the liquid causes fouling, or contains solids, it is easier to make provision for cleaning in
a plate column; man-ways can be installed on the plates. With small diameter columns, it
may be cheaper to use packing and replace the packing when it becomes fouled.
8. For corrosive liquids, a packed column will usually be cheaper than the equivalent plate
column.

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9. The liquid hold-up is appreciably lower in a packed column than a plate column. This can
be important when the inventory of toxic or flammable liquids needs to be kept as small as
possible for safety reasons.
10. Packed columns are more suitable for handling foaming systems.
11. The pressure drop per equilibrium stage (HETP) can be lower for packing than plates; and
packing should be considered for vacuum columns.
12. Packing should always be considered for small diameter columns, say less than 0.6 m,
where plates would be difficult to install, and expensive.
From the previous discussion it is clear that the use of plate in this design is more appropriate.
Step 4: Determination of the stage and reflux requirements
Most of the short-cut methods which can be used to estimate stage and reflux requirements
without the aid of computers were developed for the design of separation columns for hydrocarbon
systems in the petroleum and petrochemical systems industries, and caution must be exercised
when applying them to other systems. One of the more useful short-cut procedures is the empirical
correlations.
Minimum number of stages (Fenske equation)
The Fenske equation can be used to estimate the minimum stages required at total reflux and
can be written as:
𝑥 𝑥
[𝑥 𝑖 ] = 𝛼𝑖 𝑁𝑚𝑖𝑛 [𝑥 𝑖 ] ………………. …………………………………… (6.38)
𝑟 𝐷 𝑟 𝐵

Where:
𝑥
[ 𝑖⁄𝑥𝑟 ] ≡ The ratio of the concentration of any component i to the concentration of a
reference component r, and the suffixes D and B denote the distillate (top) and the bottom.
𝑁𝑚 ≡ Minimum number of stages at total reflux, including the re-boiler.
𝛼𝑖 ≡ Average relative volatility of component i with respect to the reference component.
Normally the separation required will be specified in terms of the key components, and
equation (6.39) can be rearranged to give an estimate of the number of stages.
𝑥 𝑥
𝐿𝑜𝑔([ 𝐿𝐾 ] 𝑥[ 𝐿𝐾 ] )
𝑥𝐻𝐾 𝐷 𝑥𝐻𝐾 𝑊
𝑁𝑚𝑖𝑛 = …………………………………………… (6.39)
𝐿𝑜𝑔(𝛼𝑎𝑣𝑔 )

Where:
𝑥𝐿𝐾 and 𝑥𝐻𝐾 ≡ Are the light and heavy key concentrations, respectively.

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𝛼𝑎𝑣𝑔 ≡ Is the average relative volatility of the light key with respect to the heavy key. The
relative volatility is taken as the geometric mean of the values at the column top and bottom
temperatures.
𝛼𝑎𝑣𝑔 = √𝛼𝑡𝑜𝑝 𝑥 𝛼𝑏𝑜𝑡𝑡𝑜𝑚 …………………………………………… (6.40)
𝐾𝑖
𝛼𝑖 = …………………………………………………………… (6.41)
𝐾𝐻𝐾

To calculate these temperatures initial estimates of the compositions must be made, so the
calculation of the minimum number of stages by the Fenske equation is a trial-and- error
procedure:
Overall material balance:
𝐹 = 𝐷 + 𝑊 ………………………………………………………………….. (6.42)
Component material balance on acetone:
𝑥𝐹 𝐹 = 𝑥𝐷 𝐷 + 𝑥𝐵 𝐵 ……………………………………………………………. (6.43)
By solving equations (6.42) and (6.43) we get:
𝐷 = 209.7068 kmol/hr
𝐵 = 245.8465 kmol/hr
The complete material balance is as follows:

Table 6-6 : Initial compositions and molar flow rates of the product streams.

Component 𝐹𝑖 𝑥𝐹𝑖 𝐷𝑖 𝑥𝐷𝑖 𝐵𝑖 𝑥𝐵𝑖

Cumene 34.49 0.08 2.76 0.01 31.73 0.13

ACP 4.927 0.01 0.00 0.00 4.93 0.02

Phenol 194.10 0.43 0.00 0.00 194.11 0.79

Acetone 192.17 0.42 192.17 0.92 0.00 0.00

AMS 14.93 0.03 0.00 0.00 14.93 0.06

H2O 14.93 0.03 14.78 0.07 0.15 0.00

∑ 1.00 1.00 1.00

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Dew points and bubble points

To estimate the stage, and the condenser and re-boiler temperatures, procedures are required
for calculating dew and bubble points. By definition, a saturated liquid is at its bubble point (any
rise in temperature will cause a bubble of vapour to form), and a saturated vapour is at its dew
point (any drop in temperature will cause a drop of liquid to form).
Dew points and bubble points can be calculated from knowledge of the vapour-liquid
equilibrium for the system. In terms of equilibrium constants, the bubble point is defined by the
equation:
Bubble point: ∑ 𝑦𝑖 = ∑ 𝐾𝑖 𝑥𝑖 = 1 ……………………. (6.44)
𝑦
Dew Point: ∑ 𝑥𝑖 = ∑ 𝑖 = 1 ………………………. (6.45)
𝐾 𝑖

For multi-component mixtures the temperature that satisfies these equations, at a given
system pressure, must be found by trial and error (Excel spread sheet was used):
Table 6-7: Dew point (top temperature).

𝑃𝑡 𝑃𝑠
Component 𝐾𝑖 𝑥𝐷 Y=𝑥𝐷 /𝐾𝑖 𝑇℃
mmHg mmHg

Cumene 49.424 0.07 0.01 0.20

ACP 6.71 0.01 0.00 0.00

Phenol 9.91 0.01 0.00 0.00

Acetone 760 1213.22 1.60 0.92 0.57 70.54

AMS 31.34 0.041 0.00 0.00

H2O 239.28 0.31 0.07 0.22

∑ 1.00 1.00

α top = 4.8413

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Table 6-8: Bubble point (bottom temperature).

𝑃𝑡 𝑃𝑠
Component 𝐾𝑖 𝑥𝐵 Y=𝑥𝐵 𝐾𝑖 𝑇℃
mmHg mmHg

Cumene 1361.86 1.79 0.13 0.23

ACP 385.30 0.51 0.02 0.01

Phenol 648.70 0.86 0.79 0.67

Acetone 760 14347.22 18.88 0.00 0.00 176.22

AMS 989.74 1.30 0.06 0.08

H2O 6915.32 9.10 0.00 0.01

∑ 1.00 1.00

α bottom= 5.0778
Tmean =124‫ﹾ‬c
At Tmean, the K-values and relative volatilities with respect to the heavy key were calculated
as follow:
Table 6-9: Relative volatilities.

Component 𝑃𝑠 αi/hk

mmHg

Cumene HK 3.35E+02 1.00E+00

ACP 6.95E+01 2.08E-01

Phenol 1.12E+02 3.36E-01

Acetone 4.99E+03 1.49E+01

AMS 2.30E+02 6.86E-01

H2O LK 1.66E+03 4.95E+00

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Then the minimum number of stages:

𝑁𝑚 = 4 stages
Minimum and practical reflux ratio
Colburn (1941) and Underwood (1948) have derived equations for estimating the minimum
reflux ratio for multi-component distillations. These equations are discussed in Volume 2, Chapter
11. As the Underwood equation is more widely used it is used here. The equation can be stated in
the form:
𝛼𝑖/ℎ𝑘 ∗ 𝑥𝑖𝐷
1 + 𝑅𝑚𝑖𝑛 = ∑ 𝛼𝑖/ℎ𝑘 −𝜃
………………………………………… (6.46)

Where:
𝛼𝑖 ≡ The relative volatility of component i with respect to the heavy key.
𝑅𝑚𝑖𝑛 ≡ The minimum reflux ratio.
𝑥𝑖𝐷 ≡ The mole fraction of component i in the tops at minimum reflux.
And θ is the root of the equation:
𝑉 𝛼𝑖/ℎ𝑘 ∗ 𝑥𝑖𝐹
1−𝑞 =𝐹 = ∑ 𝛼𝑖/ℎ𝑘 −𝜃
……………………………………….. (6.47)

Where the mole fraction of component i in the feed and q depend on the condition of the
feed and can be defined as:
𝐿𝐹
𝑞= …………………………………………………………………… (6.48)
𝐹

This parameter must be found first using flash calculations as will be shown in the next
section.
Equilibrium flash calculations
In equilibrium flash process, a feed stream is separated into liquid and vapour streams at
equilibrium. The composition of the streams will depend on the quantity of the feed vaporised
(flashed). Flash calculations are often needed to determine the condition of the feed to a distillation
column and, occasionally, to determine the flow of vapour from the re-boiler, or condenser if a
partial condenser is used.
A trail-and-error procedure followed to find the fraction of feed vaporized (𝑉𝐹 ) by setting
∑ 𝑥𝑖 = 1 or ∑ 𝑦𝑖 = 1 using the following equations:
𝐹∗𝑥𝑖𝐹
𝑙𝑖𝑋𝑖 = 𝑉 …………………………………………….. (6.49)
1+ 𝐹 ∗𝐾𝑖
𝐿

𝑦𝑖 = 𝐾𝑖 ∗ 𝑋𝑖 ………………………………………………………..........…. (6.50)

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𝑃
𝐾𝑖 = 𝑃𝑠 ……………………………………………………………………. (6.51)
𝑡

Several equations have been developed to express vapor pressure as a function of

temperature. One of the most commonly used is the Antoine equation.
𝑏
𝐿𝑜𝑔𝑃(𝑚𝑚𝐻𝑔) = 𝑎 − 𝑇+𝑐 …………………………………………………. (6.52)

𝑇 ≡ Temperature, c.
Antoine constants are illustrated in Appendix A.
Table 6-10: Feed compositions.

Component 𝐹𝑖 (kmol/hr) 𝑥𝑖𝐹

Cumene 34.49 0.08

ACP 4.93 0.01

Phenol 194.10 0.43

Acetone 192.17 0.42

AMS 14.93 0.03

H2O 14.93 0.03

Table 6-11:Flash calculation results

comp. Ps K Xf Lxi Xi Yi
713.44 0.94 0.08 9.01 0.08 0.07
Cumene
175.17 0.23 0.01 2.91 0.03 0.01
ACP
290.05 0.38 0.43 90.32 0.79 0.30
Phenol
8805.73 11.59 0.42 5.35 0.05 0.55
Acetone
504.93 0.66 0.03 4.98 0.04 0.03
AMS
3577.31 4.71 0.03 0.98 0.01 0.04
H2O
113.55 1.00 1.00
Total

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Using Excel Spread Sheet the fraction was found as:

𝑉𝐹
= 3.01106
𝐿
Accordingly, 𝑉𝐹 = 341.999 kmol/hr
∴ 𝐿𝐹 = 113.555 kmol/hr
Next, the value of the second parameter of equation (6-43), (θ), must lie between the values
of the relative volatility of the light and heavy keys; (1 < 𝜃 < 4.95) and were found by trial and
error:
𝜃 = 4.24075 ≫ 𝑅𝑚𝑖𝑛 =0.768
Taking the reflux ratio as 1.5 the minimum reflux:
𝑅 = 1.5 × 𝑅𝑚𝑖𝑛 =1.15
Actual number of ideal stages
To estimate the actual number of ideal stages an equation developed by Molokonov relates
the actual number of ideal stages to the minimum number of ideal stages and the minimum and
actual reflux ratio-was used:
1+54.4𝑋 𝑋−1
(( )×( 0.5 ))
𝑌 =1− 𝑒 11+117.2𝑋 𝑋 ……………………………………………. (6.53)
Where:
𝑅−𝑅𝑚𝑖𝑛
𝑋= …………………………………………………………….. (6.54)
𝑅+1
𝑁−𝑁𝑚𝑖𝑛
𝑌= ……………………………………………………………… (6.55)
𝑁+1

Using these equations, the actual number of ideal stages:

𝑁 = 9.37 ≅ 9 stages
Feed plate location
A limitation of the empirical methods is that they do not give the feed-point location. An
estimate can be made by using the Fenske equation to calculate the number of stages in the
rectifying and stripping sections separately, but this requires an estimate of the feed-point
temperature. An alternative approach is to use the empirical equation given by Kirkbride (1944):
𝑁 𝑥 𝐵 𝑥 2
𝐿𝑜𝑔 𝑁𝑒 = 0.206 log (( 𝑥𝐻𝐾 ) × 𝐷 × (𝑥 𝐿𝐾 𝑎𝑡 𝐵 ) ) ……………………… (6.56)
𝑠 𝐿𝐾 𝐹 𝐻𝐾 𝑎𝑡 𝐷

Where:
𝑁𝑒 ≡ Number of stages above the feed, including any partial condenser.

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𝑁𝑠 ≡ Number of stages below the feed, including the re-boiler.

𝐵 ≡ Molar flowrate of the bottom product.
𝐷 ≡ Molar flowrate of the top product.
(𝑥𝐻𝐾 𝑎𝑛𝑑 𝑥𝐿𝐾 ) 𝐹 ≡ Concentration of the heavy key and the light key in the feed
respectively.
𝑥𝐻𝐾 at top ≡ Concentration of the heavy key in the top product.
𝑥𝐿𝐾 at bottom ≡ Concentration of the light key if in the bottom product.
And it is known that the total number of ideal stages is the sum of that above and below the
feed:
𝑁 = 𝑁𝑒 + 𝑁𝑠 ………………………………………………………….. (6.57)
Using these equations, it is found:
𝑁𝑒 = 6.65767
The feed enters at the 7 stage.
Column gas and liquid flow rates
Assuming constant over flow, the flow rates of the vapor and liquid in the top section:
𝐿
𝑅=𝐷 …………………………………………………………………. (6.58)

𝐿𝑛 = 𝑅 × 𝐷 = 113.5548 kmol/hr 𝑉𝑛+1 = 𝐷 + 𝐿 = 341.998 kmol/hr

Flow rates of the vapor and liquid in the bottom section:
𝐿𝑚 = 𝐿𝑛 + 𝐿𝐹 ………………………………………………………… (6.59)
𝐿𝑚 = 227.10969 kmol/hr
𝑉𝑚+1 = 𝑉𝑛+1 − 𝑉𝐹 ………………………………………………………. (6.60)
𝑉𝑚+1 = 683.997 kmol/hr

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Table 6-12 : Summary on conceptual design calculations.

Symbol Value

Minimum reflux ratio 𝑅𝑚𝑖𝑛 0.77

Actual reflux ratio 𝑅 1.15

Minimum number of ideal stages 𝑁𝑚𝑖𝑛 4.00

Actual number of ideal stages 𝑁 9.00

Vapor flow rate of enriching section 𝑉𝑛+1 342.00

Liquid flow rate of enriching section 𝐿𝑛 113.55

Vapor flow rate of stripping section 𝑉𝑚+1 684.00

Liquid flow rate of stripping section 𝐿𝑚 227.11

Step 5: Column sizing

An approximate estimate of the overall column size can be made once the number of real stages
required for the separation is known. This is often needed to make a rough estimate of the capital
cost for project evaluation.
Overall column efficiency
An estimate of the overall column efficiency will be needed when the design method used
gives an estimate of the number of ideal stages required for the separation. This is sometimes
confusingly referred to as the overall plate efficiency.
𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑖𝑑𝑒𝑎𝑙 𝑠𝑡𝑎𝑔𝑒𝑠
𝐸𝑜 = 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑟𝑒𝑎𝑙 𝑠𝑡𝑎𝑔𝑒𝑠
……………………………………………… (6.61)

A quick estimate of the overall column efficiency can be obtained from the correlation given
by O’Connell (1946). Eduljee (1958) has expressed the O’Connell correlation in the form of an
equation:
𝐸𝑜 = 51 − 32.5𝐿𝑜𝑔(𝜇𝑎 𝛼𝑎 ) ……………………………………………. (6.62)
Where:
𝜇𝑎 ≡ The molar average liquid viscosity, 𝑚𝑁𝑠/𝑚2.
𝛼𝑎 ≡ Average relative volatility of the light key.
From appendix A: 𝜇𝑎 = 0.1936 𝑚𝑁𝑠/𝑚2

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𝛼𝑎 = 4.958
Then:
𝐸𝑜 = 51.6%
𝑁−1
The actual number of real trays = ………..………………………… (6.63)
𝐸𝑜

Number of real trays =15.5 ≅ 16 trays.

Plate contactors
Cross-flow plates are the most common type of plate contactor used in distillation and
absorption columns. In a cross-flow plate the liquid flows across the plate and the vapor up through
the plate. The flowing liquid is transferred from plate to plate through vertical channels called
“down comers”. A pool of liquid is retained on the plate by an outlet weir.
Other types of plate are used which have no down comers (non-cross-flow plates), the liquid
showering down the column through large openings in the plates (sometimes called shower plates).
These, and, other proprietary non-cross flow plates, are used for special purposes, particularly
when a low-pressure drop is required.
Three principal types of cross-flow tray are used, classified according to the method used to
contact the vapor and liquid.
Sieve plates (perforated plates) Figure (6.11a)
This is the simplest type of cross-flow plate. The vapor passes up through perforations in the
plate; and the liquid is retained on the plate by the vapor flow. There is no positive vapor liquid
seal, and at low flow-rates liquid will “weep” through the holes, reducing the plate efficiency. The
perforations are usually small holes, but larger holes and slots are used.
Bubble-cap plates Figure (6.11b)
In which the vapor passes up through short pipes, called risers, covered by a cap with a
serrated edge, or slots. The bubble-cap plate is the traditional, oldest, type of cross-flow plate, and
many different designs have been developed. Standard cap designs would now be specified for
most applications.
The most significant feature of the bubble-cap plate is that the use of risers ensures that a
level of liquid is maintained on the tray at all vapor flow-rates.
Valve plates (floating cap plates) (Figure 6.11c)
Valve plates are proprietary designs. They are essentially sieve plates with large-diameter
holes covered by movable flaps, which lift as the vapor flow increases.

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As the area for vapor flow varies with the flow-rate, valve plates can operate efficiently at lower
flow-rates than sieve plates: the valves closing at low vapor rates.
Some very elaborate valve designs have been developed, but the simple type shown in Figure
(6-11)c is satisfactory for most applications.

Figure 6-11: Plate contractors.

(a) Sieve plate. (b) Bubble cap. (c) Simple valve.
Selection of plate type
The principal factors to consider when comparing the performance of bubble-cap, sieve and
valve plates are: cost, capacity, operating range, efficiency and pressure drop.
Cost: Bubble-cap plates are appreciably more expensive than sieve or valve plates. The relative
cost will depend on the material of construction used; for mild steel the ratios, bubble-cap: valve:
sieve, are approximately 3.0: 1.5: 1.0.
Capacity: There is little difference in the capacity rating of the three types (the diameter of the
column required for a given flow-rate); the ranking is sieve, valve, and bubble-cap.
Operating range: This is the most significant factor. By operating range is meant the range of
vapor and liquid rates over which the plate will operate satisfactorily (the stable operating range).
Some flexibility will always be required in an operating plant to allow for changes in production
rate, and to cover start-up and shut-down conditions. The ratio of the highest to the lowest flow
rates is often referred to as the “turn-down” ratio.

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Bubble-cap plates have a positive liquid seal and can therefore operate efficiently at very low
vapor rates.
Sieve plates rely on the flow of vapor through the holes to hold the liquid on the plate, and
cannot operate at very low vapor rates. But, with good design, sieve plates can be designed to give
a satisfactory operating range; typically, from 50 per cent to 120 per cent of design capacity.
Valve plates are intended to give greater flexibility than sieve plates at a lower cost than bubble-
caps.
Efficiency: The Murphree efficiency of the three types of plate will be virtually the same when
operating over their design flow range, and no real distinction can be made between them.
Pressure drop: The pressure drop over the plates can be an important design consideration,
particularly for vacuum columns. The plate pressure drop will depend on the detailed design of the
plate but, in general, sieve plates give the lowest pressure drop, followed by valves, with bubble-
caps giving the highest.
Summary, Sieve plates are the cheapest and are satisfactory for most applications.
Valve plates should be considered if the specified turn-down ratio cannot be met with sieve
plates. Bubble-caps should only be used where very low vapor (gas) rates have to be handled and
a positive liquid seal is essential at all flow-rates.
Plate areas
The following areas terms are used in the plate design procedure:
𝐴𝑐 ≡ Total column cross-sectional area.
𝐴𝑑 ≡ Cross-sectional area of downcomer.
𝐴𝑛 ≡ Net area available for vapor-liquid disengagement, normally equal to
(𝐴𝑐 − 𝐴𝑑 ) for a single pass plate.
𝐴𝑎 ≡ Active of bubbling area equal to (𝐴𝑐 − 2𝐴𝑑 ) for single pass plates.
𝐴ℎ ≡ Hole area, the total area of all active holes.
𝐴𝑝 ≡ perforated area (including blanked areas).
𝐴𝑎𝑝 ≡ The clearance area under the downcomer apron.

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Step 6: Detailed column sizing and internals design

Column diameter
The principal factor that determines the column diameter is the vapor flow rate. The vapor
velocity must be below that which would cause excessive liquid entrainment or a high-pressure
drop.
The flooding condition fixes the upper limit of vapor velocity. A high vapor velocity is needed
for high plate efficiencies, and the velocity will normally be between 70 to 90 per cent of that
which would cause flooding. For design, a value of 80 to 85 per cent of the flooding velocity
should be used.
The flooding velocity can be estimated from the correlation given by Fair (1961):
𝜌𝐿 −𝜌𝑣
𝑢𝑓 = 𝐾1 √ …………………………………………………………. (6.64)
𝜌𝑣

Where:
𝑢𝑓 ≡ Flooding vapor velocity, m/s, based on the net column area.
𝐾1 ≡ A constant obtained from Figure (6.12):

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Figure 6-12: Flooding velocity, sieve plates.

The liquid-vapor flow factor 𝐹𝐿𝑉 in Figure (6.12) is given by:

𝐿𝑤 𝜌𝐿
𝐹𝐿𝑉 = √𝜌 …………………………………………………………. (6.65)
𝑉𝑤 𝑉

Where:
𝐿𝑤 ≡ Liquid mass flow rate, kg/s
𝑉𝑤 ≡ Vapor mass flow rate, kg/s.

Where the vapor and liquid flow rates, or physical properties, vary significantly throughout the
column a plate design should be made for several points up the column.
For distillation, it will usually be sufficient to design for the conditions above and below the
feed points, changes in the vapor flow rate will normally be accommodated by adjusting the hole
area; often by blanking off some rows of holes. Different column diameters would only be used
where there is a considerable change in flow-rate. Changes in liquid rate can be allowed for by
adjusting the liquid down comer areas.
From Appendix A the top and bottom densities are as follow:
Top section:
𝜌𝑣 = 2.084258 kg/m3 , 𝜌𝐿 = 894.047 kg/m3
Bottom section:
kg
𝜌𝑣 = 2.75343 m3, 𝜌𝐿 = 1018.97 kg/m3

Substituting these vales in equation (5.49) we get:

𝐹𝐿𝑉𝑡𝑜𝑝 = 0.026.
𝐹𝐿𝑉𝑏𝑜𝑡𝑡𝑜𝑚 = 0.017.
Another parameter is required to use this figure.
Plate spacing
The overall height of the column will depend on the plate spacing. Plate spacing from 0.15 m
(6 in.) to 1 m (36 in.) are normally used. The spacing chosen will depend on the column diameter
and operating conditions. Close spacing is used with small-diameter columns, and where head
room is restricted; as it will be when a column is installed in a building. For columns above 1 m
diameter, plate spacing of 0.3 to 0.6 m will normally be used, and 0.5 m (18 in.) can be taken as
an initial estimate. Here it will be taken as 0.4 m.

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The following restrictions apply to the use of Figure (6.12):

1. Hole size less than 6.5 mm. Entrainment may be greater with larger hole sizes.
2. Weir height less than 15 per cent of the plate spacing.
3. Non-foaming systems.
4. Hole: active area ratio greater than 0.10; for other ratios apply the following corrections:

Table 6-13: other ratios of active area corrections

Hole: active area Multiply 𝐾1 by
0.1 1
0.08 0.9
0.06 0.8

Liquid surface tension 24.506 N/m, for other surface tensions 𝜎 multiply the value of 𝐾1 by
𝜎 0.2
[0.02] .

From Figure (5-3) and for tray spacing = 0.4 m

(𝐾1 )𝑡𝑜𝑝 = 0.08.
Because the surface tension in the top section is greater than (from appendix A, 𝜎𝑚 =0.017029
N/m); this value need to be corrected.
𝜎 0.2
𝑚
(𝐾1 )𝑡𝑜𝑝,𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 = 𝐾1 × (0.02) =0.077468.

(𝐾1 )𝑏𝑜𝑡𝑡𝑜𝑚 = , needs to be corrected (from appendix A, 𝜎𝑚 = 0.018634 N/m).

𝜎 0.2
𝑚
(𝐾1 )𝑏𝑜𝑡𝑡𝑜𝑚,𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 = 𝐾1 × (0.02) = 0.083806.

Then the flooding velocity:

𝑢𝑓𝑡𝑜𝑝 = 1.602577 m/s and 𝑢𝑓 = 1.6100115 m/s
𝑏𝑜𝑡𝑡𝑜𝑚

Design for 85 % at maximum flow rate: 𝑢̂𝑣 = 0.85 × 𝑢𝑓

𝑢̂𝑣𝑡𝑜𝑝 = 1.36219 m/s and 𝑢̂𝑣𝑏𝑜𝑡𝑡𝑜𝑚 = 1.36851 m/s
To calculate the column diameter an estimate of the net area 𝐴𝑛 is required. As a first trial take
the down comer area as 12 per cent of the total, and assume that the hole-active area is 10 per cent.
𝑉𝑛+1
Maximum volumetric flow rate (vapor) (𝑣) =
𝜌𝑣

𝑣𝑛 = 2.55228 m3 /s and 𝑣𝑛 = 6.851342 m3 /s

𝑣
Net area required 𝐴𝑛 = ̂𝑣
𝑢

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𝐴𝑛𝑡𝑜𝑝 = 1.87366 m2 and 𝐴𝑛𝑏𝑜𝑡𝑡𝑜𝑚 = 5.006425 m2

According to the previous assumption the down comer area (𝐴𝑑 ) = 0.12 × 𝐴𝑐
𝑛 𝐴
Then the column cross sectioned area (𝐴𝑐 ) = 0.88

𝐴𝑐𝑡𝑜𝑝 = 2.12916 m2 and 𝐴𝑐𝑏𝑜𝑡𝑡𝑜𝑚 = 5.68912 m2

4×𝐴𝑐
Then the column diameter (𝐷𝑐 ) = √ 𝜋

𝐷𝑐𝑡𝑜𝑝 = 1.64649 m and 𝐷𝑐𝑏𝑜𝑡𝑡𝑜𝑚 = 2.691396 m

Both of the two diameters are out of standard range. The largest one will be taken as the
uniform column diameter.
Liquid flow pattern
Cross-flow trays are also classified according to the number of liquid passes on the plate.
The design shown in Figure (6.13a) is a single-pass plate. For low liquid flow rates, reverse flow
plates are used; Figure (6.13b). In this type, the plate is divided by a low central partition, and inlet
and outlet down-comers are on the same side of the plate. Multiple pass plates, in which the liquid
stream is sub-divided by using several down-comers, are used for high liquid flow-rates and large
diameter columns. A double-pass plate is shown in Figure (6.13c).

Figure 6-13: Liquid flow pattern on cross-flow tray.

(a) single pass (b) reverse flow (c) double pass

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Figure 6-14: Selection of liquid-flow arrangement.

Maximum liquid volumetric flow rate = 0.006147 m3 /s

From Figure (6.14) and for Dc = 2.69 m the liquid-flow arrangement is: cross flow (single
pass).
Weir dimensions
Weir height
The height of the weir determines the volume of liquid on the plate and is an important factor
in determining the plate efficiency. A high weir will increase the plate efficiency but at the expense
of a higher plate pressure drop. For columns operating above atmospheric pressure the weir heights
will normally be between 40 mm to 90 mm (1.5 to 3.5 in.); 40 to 50 mm is recommended. For
vacuum operation, lower weir heights are used to reduce the pressure drop; 6 to 15 mm (0.6 to
0.25 in.) is recommended.
Weir length
With segmental down corners, the length of the weir fixes the area of the downcomer. The
chord length will normally be between 0.6 to 0.85 of the column diameter . A good initial value to

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use is 0.761, equivalent to a downcomer area of 12 percent. The relationship between weir length
and downcomer area is given in Figure (6.15).
𝐴𝑑 𝑙
For = 12% , 𝐷𝑤 = 0.761 ≫ 𝑙𝑤 = 2.04815 m
𝐴𝑐 𝑐

Figure 6-15:The relation between downcomer area and weir length.

Weir liquid crest

The height of the liquid crest over the weir can be estimated using the Francis weir formula.
For a segmental downcomer this can be written as:
Lw 2/3
how = 750 [ρ ] ………………………………………………………. (6.66)
L lw

Where:
lw ≡ Weir length, m.
how ≡ Weir crest, mm liquid.
Lw ≡ Liquid flowrate, kg/s.
Maximum liquid flowrate = Lw × Mwavg 6.2637 kg/s
≫ how = 15.6055 mm liquid
Minimum liquid flowrate = 4.3846 kg/s
≫ how = 12.3027 mm liquid

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Hole size
The hole sizes used vary from 2.5 to 12 mm; 5 mm is the preferred size. Larger holes are
occasionally used for fouling systems. The holes are drilled or punched. Punching is cheaper, but
the minimum size of hole that can be punched will depend on the plate thickness, for carbon steel,
hole sizes approximately equal to the plate thickness can be punched, but for stainless steel the
minimum hole size that can be punched is about twice the plate thickness. Typical plate thicknesses
used are: 6 mm (3/16 in.) for carbon steel, which will be the material of plates. When punched
plates are used they should be installed with the direction of punching upward. Punching forms, a
slight nozzle, and reversing the plate will increase the pressure drop.
Provisional plate design
Column diameter 𝐷𝑐 = 2.691396 m

Column area 𝐴𝑐 = 5.68912 m2

Downcomer area 𝐴𝑑 = 0.68269m2

Net area 𝐴𝑛 = 5.006425 m2

Active area 𝐴𝑎 = 4.323731 m2

Hole area 𝐴ℎ = 10% × 𝐴𝑎 = 0.43237 m2

Take weir height 15 mm

Plate thickness for carbon steel 6 mm

Hole diameter 5 mm

Weep point
The lower limit of the operating range occurs when liquid leakage through the plate holes
becomes excessive. This is known as the weep point. The vapor velocity at the weep point is the
minimum value for stable operation. The hole area must be chosen so that at the lowest operating
rate the vapor flow velocity is still well above the weep point.
Several correlations have been proposed for predicting the vapor velocity at the weep point.
That given by Eduljee (1959) is one of the simplest to use, and has been shown to be reliable.

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The minimum design vapor velocity is given by:

[𝐾2 − 0.90(25.4−𝑑ℎ )]
𝑢̂ℎ = (𝜌𝑣 )1/2
………………………………………………… (6.61)

Where:
𝑢̂ℎ ≡ Minimum vapor velocity through the holes (based on the hole area), m/s.
𝑑ℎ ≡ Hole diameter, mm.
𝐾2 ≡ Constant, dependent on the depth of clear liquid on the plate, obtained from Figure (6-
7).
The clear liquid depth is equal to the height of the weir hw plus the depth of the crest of
liquid over the weir how .
At minimum liquid flow rate:
hw + how = 12.3027 mm
From Figure (6.18) K 2 = 29.5
Then the minimum vapor velocity based on the minimum density (top density) will be:
ûh = 8.339704 m/s
Take the down-turn ratio as 70 %
The minimum vapour volumetric flow rate = 0.7 × Maximum vapor rate
Minimum vapour rate
Actual minimum vapour velocity = = 11.0921 m/s
Ah
The minimum operating rate will be well above weep point.

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Figure 6-16:Weep-point correlation.

Plate pressure drop

The pressure drop over the plates is an important design consideration. There are two main
sources of pressure loss: that due to vapor flow through the holes (an orifice loss), and that due to
the static head of liquid on the plate.
A simple additive model is normally used to predict the total pressure drop. The total is taken
as the sum of the pressure drop calculated for the flow of vapor through the dry plate (the dry plate
drop hd ); the head of clear liquid on the plate (hw + how ) and a term to account for other, minor,

sources of pressure loss, the so-called residual loss hr . The residual loss is the difference between
the observed experimental pressure drop and the simple sum of the dry-plate drop and the clear-
liquid height. It accounts for the two effects: the energy to form the vapor bubbles and the fact that
on an operating plate the liquid head will not be clear liquid but a head of “aerated” liquid froth,
and the froth density and height will be different from that of the clear liquid.
Dry plate drop
The pressure drop through the dry plate can be estimated using expressions derived for flow
through orifices.

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uh 2 ρv
Hd = 51 [ ] …………………………………………………..…… (6.67)
C0 ρL

Where the orifice coefficient C0 is a function of the plate thickness, hole diameter, and the hole
to perforated area ratio. C0 can be obtained from Figure (6.17); which has been adapted from a
similar figure by Liebson et al. (1957). Uh is the velocity through the holes, m/s.
To calculate the perforated area first we need to determine the hole pitch.
Hole pitch
The hole pitch (distance between the hole centers) lp should not be less than 2 × hole diameters,
and the normal range will be 2.5 to 4.0 diameters. Within this range the pitch can be selected to
give the number of active holes required for the total hole area specified. Square and equilateral
triangular patterns are used; triangular is preferred. It will be taken as 2.5 diameters.
Lp = 1.5 mm
The total hole area as a fraction of the perforated area Ap is given by the following expression,
for an equilateral triangular pitch:
2
Ah dh
= 0.9 [ ] …..…………………………………………………………. (6.68)
Ap lp

Using this equation and substituting the previous values of hole diameter:
Ah
% = 14.4.
Ap

Also, the ratio of plate thickness to hole diameter = 0.83. Accordingly, from Figure (6.17):
𝐶0 = 0.95
ℎ𝑑 = 38.34178 mm liquid

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Figure 6-17:Discharge coefficient, sieve plates.

Residual head
Methods have been proposed for estimating the residual head as a function of liquid surface
tension, froth density and froth height. However, as this correction term is small the use of an
elaborate method for its estimation is not justified, and the simple equation proposed by Hunt et
al. (1955) can be used, which is equivalent to taking the residual drop as a fixed value of 12.5 mm
of water (~ in.):
12.5 × 103
ℎ𝑟 = = 12.267 mm liquid
𝜌𝐿

Total drop
The total plate drop is given by:
ℎ𝑡 = ℎ𝑑 + (ℎ𝑤 + ℎ𝑜𝑤 ) + ℎ𝑟 = 81.2143 mm liquid/plate
In pressure units (∆P) = 9.81 × 10−6 ℎ𝑡 𝜌𝐿 = 0.811822 kPa/plate

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Figure 6-18: Downcomer backup.

Downcomer design [back-up]

The downcomer area and plate spacing must be such that the level of the liquid and froth in the
downcomer is well below the top of the outlet weir on the plate above. If the level rises above the
outlet weir the column will flood.
The back-up of liquid in the downcomer is caused by the pressure drop over the plate (the
downcomer in effect forms one leg of a U-tube) and the resistance to flow in the downcomer itself;
see Figure (6.18).
In terms of clear liquid, the downcomer back-up is given by:
ℎ𝑏 = (ℎ𝑤 + ℎ𝑜𝑤 ) + ℎ𝑡 + ℎ𝑑𝑐 ………………………………………….. (6.69)
Where:
ℎ𝑏 ≡ Downcomer back-up, measured from plate surface, mm.
ℎ𝑑𝑐 ≡ Head loss in the downcomer, mm.
The main resistance to flow will be caused by the constriction at the downcomer outlet, and
the head loss in the downcomer can be estimated using the equation given below:
𝐿 2
ℎ𝑑𝑐 = 166 [𝜌 𝑤𝑑 ] …………………………………………………….. (6.70)
𝐴 𝐿 𝑚

Where:
𝐿𝑤𝑑 ≡ Liquid flow rate in downcomer, kg/s; (maximum liquid flow rate).

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𝐴𝑚 ≡ Either the downcomer area Ad or the clearance area under the downcomer Aap ;

whichever is the smaller, m2 .

The clearance area under the downcomer is given by:
𝐴𝑎𝑝 = ℎ𝑎𝑝 × 𝑙𝑤 …………………………………………………………. (6.71)
Where:
ℎ𝑎𝑝 is height of the bottom edge of the apron above the plate. This height is normally set at
5 to 10 mm (0.5 to 0.25 in.) below the outlet weir height, here it will be taken as 5 mm. For weir
height of 15 mm and length of 1.760 m:
ℎ𝑎𝑝 = ℎ𝑤 − 5 =10
𝐴𝑎𝑝 = 0.020482 m2 which is less than the area of downcomer ( m2).
ℎ𝑑𝑐 = 19.4234 mm
ℎ𝑏 = 131.243 mm
Froth height
To predict the height of “aerated” liquid on the plate, and the height of froth in the
downcomer, some means of estimating the froth density is required. The density of the “aerated”
liquid will normally be between 0.4 to 0.7 times that of the clear liquid. A number of correlations
have been proposed for estimating froth density as a function of the vapor flow-rate and the liquid
physical properties; however, none is particularly reliable, and for design purposes it is usually
satisfactory to assume an average value of 0.5 of the liquid density.
This value is also taken as the mean density of the fluid in the downcomer; which means that
for safe design the clear liquid back-up, calculated from equation (5.61), should not exceed half
the plate spacing 𝑙𝑡 , to avoid flooding.
Allowing for the weir height:
1
ℎ𝑏 ≯ 2 (ℎ𝑤 + 𝑙𝑡 )…………………………………………………………. (6.72)
ℎ𝑤 +𝑙𝑡
This constrain have been met as the value of = m which is well above the downcomer
2

back-up.

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Downcomer residence time

Sufficient residence time must be allowed in the downcomer for the entrained vapor to
disengage from the liquid stream; to prevent heavily “aerated” liquid being carried under the
downcomer.
A time of at least 3 seconds is recommended.
This time is given by:
𝐴𝑑 ℎ𝑏𝑐 𝜌𝐿
𝑡𝑟 = ………………………………………………………….. (6.73)
𝐿𝑤𝑑

Where:
𝑡𝑟 ≡ Residence time, s.
ℎ𝑏𝑐 ≡ Clear liquid back-up, m.
This gives a residence time = 14.6 seconds.
Entrainment
Entrainment can be estimated from the correlation given by Fair (1961), Figure (5.21), which
gives the fractional entrainment ψ (kg/kg gross liquid flow) as a function of the liquid-vapor factor
𝐹𝐿𝑉 with the percentage approach to flooding as a parameter.
𝑢𝑛 actual velocity based on net area
The percentage flooding = …………………….. (6.74)
𝑢𝑓 (from equation 5.27)

The effect of entrainment on plate efficiency can be estimated using equation (6.66). As a
rough guide, the upper limit of ψ can be taken as 0.1; below this figure the effect on efficiency will
be small. The optimum design value may be above this figure, see Fair (1963).
𝐸𝑚𝑉
𝐸𝑎 = ψ ……………………………………………………… (6.75)
1+𝐸𝑚𝑉 [ ]
1−ψ

As a check of the entrainment to be within the limit:

Maximum volumetric vapor flowrate
𝑢𝑣 = = 1.3685 m/s
𝐴𝑛
For a flooding velocity uf of 4.285 m/s and liquid-vapor factor flv of 0.01, The
percentage flooding = 85 % and from Figure (6.19) ψ = 0.08 .

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Figure 6-19:Entrainment correlation for sieve plates.

Plate construction
The mechanical design features of sieve plates are described in this section.
Two basically different types of plate construction are used. Large-diameter plates are normally
constructed in sections, supported on beams. Small plates are installed in the column as a stack of
pre-assembled plates.

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Stacked plates (cartridge plates)

The stacked type of construction is used where the column diameter is too small for a man
to enter to assemble the plates, say less than 1.2 m (4 ft). It will not be discussed further because
this column diameter is more than 1.2 m, it has been described in details in volume 6 (section
11.12.2).
Sectional construction
A typical plate is shown in Figure (6.20). The plate sections are supported on a ring welded
round the vessel wall, and on beams. The beams and ring are about 50 mm wide, with the beams
set at around 0.6 m spacing. The beams are usually angle or channel sections, constructed from
folded sheet. Special fasteners are used so the sections can be assembled from one side only. One
section is designed to be removable to act as a manway. This reduces the number of manways
needed on the vessel, which reduces the vessel cost.

Figure 6-20:Typical sectional plate construction.

Downcomers
The segmental, or chord downcomer, which will be used here, shown in Figure (6.21a) is the
simplest and cheapest form of construction and is satisfactory for most purposes. The downcomer
channel is formed by a flat plate, called an apron, which extends down from the outlet weir. The

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apron is usually vertical, but may be sloped Figure (6.21b) to increase the plate area available for
perforation. If a more positive seal is required at the downcomer at the outlet, an inlet weir can be
fitted Figure (6.21c) or a recessed seal pan used Figure (6.21d).
Circular downcomers (pipes) are sometimes used for small liquid flowrates.

Figure 6-21:Segment (chord) downcomer designs.

(b) Vertical apron (b) Inclined apron (c) Inlet weir (d) Recessed well
Trail layout
Allow 50 mm unperforated area strip round plate edge (ring wide), 50 mm wide calming zones.
Perforated area
From Figure (5-13) at 𝑙𝑤 /𝐷𝑐 = 0.761
𝜃𝑐 = 99 °
Angle subtended at plate edge by unperforated strip = 81 °
Mean length, unperforated edge strips = 3.734 m
Area of unperforated edge strips = 0.1867𝑚2
Mean length of calming zone = 1.83 𝑚
Area of calming zone = 0.183 𝑚2
Total area for perforations, 𝐴𝑝 = 3.954𝑚2

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𝐴ℎ
= 0.10935
𝐴𝑝

𝑙𝑝
From Figure (6.22) = 2.869 , which is within 2.5 to 4 .
𝑑ℎ

Number of holes:
Area of one hole = 2.82743𝐸 − 05 m
total area of holes
Number of holes = = 15292.07 ≅ 15292 hole
area of one hole

Figure 6-22:Relation between hole area and pitch.

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Table 6-14:Plate specifications.

Plate No. 1 Turn-down per cent max rate

Plate I.D. 2.13 M Plate material Carbon steel

Hole size 15.00 Mm Downcomer material Carbon steel

Hole pitch 6.00 Mm Plate spacing 0.40 M

Total no. holes - Plate thickness 5.00 Mm

Active holes 15292.00 Plate pressure drop 81.20 mm liquid=0.812 kPa

Step 7: Mechanical design of Acetone distillation column

General design considerations: pressure vessels
Design pressure
A vessel must be designed to withstand the maximum pressure to which it is likely to be
subjected in operation.
Vessels subject to external pressure should be designed to resist the maximum differential
pressure that is likely to occur in service. Vessels likely to be subjected to vacuum should be
designed for a full negative pressure of 1 bar, unless fitted with an effective, and reliable, vacuum
breaker.
Design temperature
The strength of metals decreases with increasing temperature so the maximum allowable design
stress will depend on the material temperature. The design temperature at which the design stress
is evaluated should be taken as the maximum working temperature of the material, with due
allowance for any uncertainty involved in predicting vessel wall temperatures.
Materials
Pressure vessels are constructed from plain carbon steels, low and high alloy steels, other alloys,
clad plate, and reinforced plastics.
Selection of a suitable material must take into account the suitability of the material for
fabrication (particularly welding) as well as the compatibility of the material with the process
environment.

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The pressure vessel design codes and standards include lists of acceptable materials; in
accordance with the appropriate material standards.
Corrosion allowance
The “corrosion allowance” is the additional thickness of metal added to allow for material lost
by corrosion and erosion, or scaling. The allowance to be used should be agreed between the
customer and manufacturer. Corrosion is a complex phenomenon, and it is not possible to give
specific rules for the estimation of the corrosion allowance required for all circumstances. The
allowance should be based on experience with the material of construction under similar service
conditions to those for the proposed design.
For carbon and low-alloy steels, where severe corrosion is not expected, a minimum allowance
of 2.0 mm should be used; where more severe conditions are anticipated this should be increased
to 4.0 mm. Most design codes and standards specify a minimum allowance of 1.0 mm.
Design stress (nominal design strength)
For design purposes, it is necessary to decide a value for the maximum allowable stress
(nominal design strength) that can be accepted in the material of construction.
This is determined by applying a suitable “design stress factor” (factor of safety) to the
maximum stress that the material could be expected to withstand without failure under standard
test conditions. The design stress factor allows for any uncertainty in the design methods, the
loading, the quality of the materials, and the workmanship.
For materials not subjected to high temperatures, the design stress is based on the yield stress
(or proof stress), or the tensile strength (ultimate tensile stress) of the material at the design
temperature.
For materials subject to conditions at which the creep is likely to be a consideration, the design
stress is based on the creep characteristics of the material: the average stress to produce rupture
after 105 hours, or the average stress to produce a 1 per cent strain after 105 hours, at the design
temperature. Typical design stress factors for pressure components are shown in table 6-10.

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Table 6-15:Design stress factors.

Material

Carbon
Austenitic
Property
Carbon- No-ferrous
manganese, Stainless metals
steel
low alloy steels

Minimum yield stress or 0.2 per cent proof

stress, at the design temperature
1.50 1.50 1.50

Minimum tensile

strength, at room temperature 2.35 2.50 2.40

Mean stress to produce rupture

at 105 h at the design temperature 1.50 1.50 1.00

In the British Standard, BS 5500, the nominal design strengths (allowable design stresses), for
use with the design methods given, are listed in the standard, for the range of materials covered by
the standard the standard should be consulted for the principles and design stress factors used in
determining the nominal design strengths.
Typical design stress values for some common materials are shown in Table 13.2 (Chemical
Engineering Volume 6), These may be used for preliminary designs. The standards and codes
should be consulted for the values to be used for detailed vessel design.
DESIGN OF VESSELS SUBJECTED TO EXTERNAL PRESSURE
Cylindrical shells
Two types of process vessel are likely to be subjected to external pressure: those operated under
vacuum, where the maximum pressure will be 1 bar (atm); and jacketed vessels, where the inner
vessel will be under the jacket pressure. Thin-walled vessels subject to external pressure are liable
to failure through elastic instability (buckling) and it is this mode of failure that determines the
wall thickness required.
For an open-ended cylinder, the critical pressure to cause buckling Pc is given by the following
expression; see Windenburg and Trilling (1934):

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2𝐸
1 2 2𝑛2 −1−𝑣 2𝐸 𝑡 3 𝐷0
𝑃𝑐 = 3 [𝑛 − 1 + 2 ] (1−𝑣2 ) (𝐷 ) + 2 …………………… (6.77)
𝑛2 (
2𝐿
) −1 0 2𝐿 2
𝜋𝐷0 (𝑛2 −1)[𝑛2 ( ) +1]
𝜋𝐷0

Where:
L ≡ The unsupported length of the vessel, the effective length.
𝐷0 ≡ External diameter.
T ≡ Wall thickness.
E ≡ Young’s modulus.
V ≡ Poisson’s ratio.
N ≡ The number of lobes formed at buckling.
For long tubes and cylindrical vessels this expression can be simplified by neglecting terms
with the group 2𝐿/𝜋𝐷0 in the denominator. The minimum value of the critical pressure will occur
when the number of lobes is 2, and for most pressure-vessel materials Poisson’s ratio can be taken
as 0.3; substituting these in equation (6.40) gives:
𝑡 3
𝑃𝑐 = 2.2𝐸 (𝐷 ) ……………………………………………………………………. (6.78)
0

For short closed vessels, and long vessels with stiffening rings, the critical buckling pressure
will be higher than that predicted by equation (6.47). The effect of stiffening can be taken into
account by introducing a “collapse coefficient”,𝐾𝑐 , into equation (6.48).
𝑡 3
𝑃𝑐 = 𝐾𝑐 𝐸 (𝐷 ) ……………………………………………………………………… (6.79)
0

Where 𝐾𝑐 is a function of the diameter and thickness of the vessel, and the effective length
L’ between the ends or stiffening rings.
The minimum practical wall thickness of vessels of diameter from 2.5 to 3 m is 10 mm including
a corrosion allowance of 2 mm (volume 6, section (13.4.8)). In the proceeding paragraphs this
thickness will be checked with the previous specification of the column to ensure that the column
is sufficiently rigid to its own weight and any identical loads.
Checking the plate spacing: In vacuum distillation columns, the plate-support rings will act as
stiffening rings and strengthen the vessel, thus the critical distance beyond which stiffening will
not be effective can be taken as the plate spacing (0.4 m).
It can be shown (see Southwell, 1913) that the critical distance between stiffeners, Lc, is given
by:

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𝐷 1/2
𝐿𝑐 = 1.11 𝐷0 ( 𝑡0 ) ………………………………………………………….. (6.80)

Where:
𝑡 ≡ Shell thickness = 0.01m.
𝐷0 ≡ Outside diameter of the shell = 2.6964 m.
Then the critical distance 𝐿𝑐 is found to be 69.5046 m, which is well above the chosen plate
spacing.
Checking the buckling pressure:
By taking the modulus of elasticity is 2.1 × 1011 𝑁/𝑚2 at room temperature, and from
𝐷0 𝐿′
Figure (6.23) for = 539.27 and = 0.148 .
𝑡 𝐷0

The collapse coefficient (𝐾𝑐 ) =130.

Substituting in equation (6.73): 𝑃𝑐 = 174069.09 N/m2 which is well above the maximum design
pressure of 111457.5 N/m2.

Figure 6-23: Collapse coefficient for cylindrical shells.

Checking the ring dimensions: The usual procedure is to design stiffening rings to carry the
pressure load for a distance of ½ Ls on each side of the ring, where Ls is the spacing between the
rings. So, the load per unit length on a ring 𝐹𝑟 will be given by:
Fr = Pe Ls …………………………………………………………………… (6.81)
Where Pe is the external pressure.

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This gives 40000 N/m.

The critical load to cause buckling in a ring under a uniform radial load Fc is given by the
following expression:
24EIr
Fc = ………………………………………………………………… (6.82)
Dr 3

Where
Ir ≡ Second moment of area of the ring cross-section.
Dr ≡ Diameter of the ring (approximately equal to the shell outside diameter).
Combining equations (6.75) and (6.76) will give an equation from which the required
dimensions of the ring can be determined:
24EIr
Pe Ls ⊁ ……………………………………………………………. (6.83)
Dr 3

Converting this equation to equality yields a second moment of inertia:

Ir = 1.5559E − 07 m4
In calculating the second moment of area of the ring some allowance is normally made for the
vessel wall; the use of Ir calculated for the ring alone will give an added factor of safety.
For a rectangular section, the second moment of area is given by:
breadth ×depth3
I= …………………………………………………………….. (6.84)
12

So, for the support rings with wide = depth = 10 mm; I = 8.33333E-10 m4, which is quite
minimum than that obtained from the critical load; and the support ring is of an adequate size to
be considered as a stiffening ring.
Vessel heads
For a sphere subject to external pressure the minimum thickness is given by:
𝑃
𝑒 = 4 𝑅𝑠 √( 𝐸𝑒) ……………………………………………………………… (6.85)

Where 𝑅𝑠 is the outside radius of the sphere which can be taken as the column diameter, that
yields a minimum thickness of 3.72137 mm, which is less than the practical thickness of 10 mm.
Design loads
A structure must be designed to resist gross plastic deformation and collapse under all the
conditions of loading. They can be classified as major loads „that must always be considered in
vessel design‟ and subsidiary loads.

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Major loads
1. Design pressure: including any significant static head of liquid.
2. Maximum weight of the vessel and contents, under operating conditions.
3. Maximum weight of the vessel and contents under the hydraulic test conditions.
4. Wind loads.
5. Earthquake (seismic) loads.
6. Loads supported by, or reacting on, the vessel.
Weight of the vessel and the wind loads are the most probable loads to occur in our surrounding
environment, they will be considered in the following calculations.
Shell weight
For preliminary calculations the approximate weight of a cylindrical steel vessel with domed
ends, and uniform wall thickness, can be estimated from the following equation:
𝑊𝑣 = 240 𝐶𝑣 𝐷𝑚 (𝐻𝑣 + 0.8𝐷𝑚) 𝑡 ………………………………………… (6.86)
Where:
𝑊𝑣 ≡ Total weight of the shell, excluding internal fittings, such as plates, N.
𝐶𝑣 ≡ A factor to account for the weight of nozzles, manways, internal supports etc; which
can be taken as:
1.08 for vessels with only a few internal fittings,
1.15 for distillation columns, or similar vessels, with several manways, and with plate support
rings, or equivalent fittings, it will be taken = 1.15.
𝐻𝑣 ≡ Height, or length, between tangent lines (the length of the cylindrical section).
𝐷𝑚 ≡ Mean diameter of vessel = (𝐷𝑖 + 𝑡 × 10−3 ).
In this case these values are as follow:
𝐶𝑣 = 1.15
(𝑁−1)𝐶+0.1𝑁𝐶
𝐻𝑣 = ………………………………………………………… (6.87)
0.8

𝐻𝑣 = 8.3 m
𝑊𝑣 = 38.91 kN
Weight of one plate = 1.2 × plate area = 6.827 kN
Total weight of plates = 109.231 kN
Total weight of the vessel = 148.1423 kN
Wind load

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

The wind load is calculated based on location and the weather of surrounding. The load imposed
on any structure by the action of the wind will depend on the shape of the structure and the wind
velocity. For a smooth cylindrical column or stack the following semi-empirical equation can be
used to estimate the wind pressure:
𝑃𝑤 = 0.5 × 𝑢𝑤 2 …………………………………………………………. (6.88)
Where:
𝑃𝑤 ≡ Wind pressure (load per unit area), 1.28kN/m2 .
𝑢𝑤 ≡ Wind velocity, km/h.
Loading per unit meter = mean diameter × wind pressure = 3.45 kN/m.
Total wind load = loading per unit meter × height = 28.647 kN.
Table 6-16:Provisional plate design specification.

Item Value

Column diameter, Dc 2.69 m5

Total tower height 8.00 m

Number of trays 16.00

Plate spacing 0.40 m

Plate thickness 5.00 mm

Plate material Carbon steel

Downcomer area, Ad 0.68 m2

Column area, Ac 5.69 m2

Net area, An 1.87 m2

Active area, Aa 4.32 m2

Hole area, Ah 2.83E-05 m2

Weir length 1.76 m2

Weir height 15.00 mm

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Table 6-17:Mechanical design of plate column.

Operating pressure 101325.00 N/m2

Design pressure 111457.50 N/m2

Safety factor 0.10

Shell thickness 10.00 mm

Type of head Spherical

Head thickness 10.00 m

Cumene Distillation
Following the same procedure in acetone distillation:
Table 6-18:Design summery for Cumene distillation column.

Step 1: Product specifications:

Component 𝑥𝐷 𝑥𝐵

Cumene 0.99 0.00

ACP 0 0.02

Phenol 0 0.91

Acetone 0 0.00

AMS 0.01 0.07

H2O 0.00 0.00

Step 2: Selection of operating

conditions:

Types of the operation

Selection of column pressure 725.00 mmHg

Step 3: Selection of the contacting

device:

Contacting device Plates

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CHAPTER SIX: EQUIPMENT DESIGN ||PHENOL

Feed specifications:

Component 𝐹𝑖 kmol/hr 𝑥𝐹

Cumene 31.73 0.13

ACP 4.93 0.02

Phenol 194.10 0.79

Acetone 0.00 0.00

AMS 14.93 0.06

H2O 0.15 0.00

Component 𝐷𝑖 𝑥𝐷 𝐵𝑖 𝑥𝐵

Cumene 31.41 0.99 0.32 0.00

ACP 0.00 0.00 4.93 0.02

Phenol 0.00 0.00 194.10 0.91

Acetone 0.00 0.00 0.00 0.00

AMS 0.15 0.00 14.78 0.07

H2O 0.15 0.00 0.00 0.00

D 31.71 𝑘𝑚𝑜𝑙/ℎ𝑟

B 214.13 𝑘𝑚𝑜𝑙/ℎ𝑟

Dew po ints and bubble points:

Top section 𝑇𝑇 = 152.30℃

Bottom section 𝑇𝐵 = 180.90 ℃

Minimal and practical reflux ratio:

𝑁𝑚𝑖𝑛 27.94 𝑠𝑡𝑎𝑔𝑒𝑠

𝜃 1.50

𝑅𝑚𝑖𝑛 10.10

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R = 1.5× 𝑅𝑚𝑖𝑛 15.10

Actual number of ideal stages 45 𝑠𝑡𝑎𝑔𝑒𝑠

Feed plate location 𝑁𝑒 = 42.00

𝐿𝑛 137.78 𝑘𝑚𝑜𝑙/ℎ𝑟

𝑉𝑛+1 108.07 𝑘𝑚𝑜𝑙/ℎ𝑟

𝐿𝑚 275.55 𝑘𝑚𝑜𝑙/ℎ𝑟

𝑉𝑚+1 216.14 𝑘𝑚𝑜𝑙/ℎ𝑟

Step 5: Column sizing:

Overall column efficiency:

𝐸𝑜 46.30%

Actual number of real trays:

𝑁𝑎𝑐𝑡𝑢𝑎𝑙 95 stages

Plate contractor:

Sieve plate
Plate type
(perforated plate)

Step 6: Column diameter and internals design calculations:

Liquid-vapor flow factor:

𝐹𝐿𝑉,𝑡𝑜𝑝 0.04

𝐹𝐿𝑉,𝑏𝑜𝑡𝑡𝑜𝑚 0.07

Plate spacing: 0.40 m

Flooding constants:

𝐾1,𝑡𝑜𝑝 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.11

𝐾1,𝑏𝑜𝑡𝑡𝑜𝑚 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.27

Flooding velocity:

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𝑢𝑓𝑡𝑜𝑝 2.40 𝑚/𝑠

𝑢𝑓𝑏𝑜𝑡𝑡𝑜𝑚 4.99 𝑚/𝑠

Design velocity:

𝑢𝑣𝑡𝑜𝑝 2.04 𝑚/𝑠

𝑢𝑣𝑏𝑜𝑡𝑡𝑜𝑚 4.25 m/s

Maximum velocity flow rate:

𝑣 0.98 𝑚3 ⁄𝑠

𝑣′ 2.19 m^3⁄s

Net area required:

𝐴𝑛,𝑡𝑜𝑝 0.48 𝑚2

𝐴𝑛,𝑏𝑜𝑡𝑡𝑜𝑚 0.52 m^2

Column cross-sectioned area:

𝐴𝑐,𝑡𝑜𝑝 0.55 𝑚2

𝐴𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 0.59 m^2

Column diameter:

𝐷𝑐,𝑡𝑜𝑝 0.83 𝑚

𝐷𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 0.86 m

Downcomer area:

𝐴𝑑 0.07 𝑚2

Active area:

𝐴𝑎 0.45 𝑚2

Hole area:

𝐴ℎ 0.04 𝑚2

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Liquid flow pattern:

Cross flow Single pass

Weir dimensions:

Weir height 15.00 𝑚𝑚

Weir length 1.31 m

Weir liquid crest:

Maximum liquid flow rate 7.37kg/s

Minimum liquid flowrate 5.16 𝑘𝑔/𝑠

Hole size:

Plate thickness 5.00 𝑚𝑚

Hole diameter 6.00 𝑚𝑚

Weeping:

(ℎ𝑜𝑤 + ℎ𝑤 )𝑚𝑖𝑛 45.79 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

𝐾2 29.50

𝑢̌ℎ 6.29 𝑚/𝑠

𝑢̌ℎ𝑎𝑐𝑡𝑢𝑎𝑙 7.44 m/s

Plate pressure drop:

Dry pressure drop:

Hole pitch (𝑙𝑝 ) 15.00 𝑚𝑚

𝐴ℎ
14.40
𝐴𝑝

Plate thickness/hole diameter:

𝐶𝑜 0.85

ℎ𝑑 382.17 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

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Residual head:

ℎ𝑟 13.24 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Total drop:

ℎ𝑡 449.47 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

∆𝑃 395.39 mmHg/plate

Downcomer design [back-up]

ℎ𝑎𝑝 10.00 𝑚𝑚

𝐴𝑎𝑝 0.01 𝑚2

ℎ𝑑𝑐 80.37 𝑚𝑚

ℎ𝑏 583.89 𝑚m

𝑡𝑟 5.26 𝑠

Entrainment:

𝑢𝑛 4.24 𝑚/𝑠

Flooding percent 85%

Ψ 0.08

Trail layout:

Plate construction Sectional construction

Downcomers Vertical apron

Ring wide 50 𝑚𝑚

Calming zones 50 𝑚𝑚

𝜃𝑐 99 degrees

Mean length, unperforated edge strips 0.56 𝑚

Area of unperforated edge strips 0.058 𝑚2

Mean length of calming zone 0.56 𝑚

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𝐴𝑝 0.33 𝑚2

Area of one hole 2.83E-05 𝑚2

Number of holes 1574.25 holes

Tower Height 39.70 m

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AMS Distillation
Table 6-19: Design summery for AMS distillation column.

Step 1: Product specifications:

Component 𝑥𝐷 𝑥𝐵

Cumene 0.02 0.00

ACP 0.00 0.03

Phenol 0.11 0.97

Acetone 0.00 0.00

AMS 0.87 0.00

H2O 0.00 0.00

Step 2: Selection of operating conditions:

Types of the operation

Selection of column pressure 750.00mmHg

Step 3: Selection of the contacting device:

Contacting device Plates

Feed specifications:

Component 𝐹𝑖 (kmol/hr) 𝑥𝐹

Cumene 0.32 0.00

ACP 4.93 0.02

Phenol 194.11 0.91

Acetone 0.00 0.00

AMS 14.78 0.07

H2O 0.00 0.00

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Component 𝐷𝑖 𝑥𝐷 𝐵𝑖 𝑥𝐵

Cumene 38.08 0.02 0.00 0.00

ACP 0.00 0.00 4.93 0.02

Phenol 1.94 0.11 192.17 0.97

Acetone 0.00 0.00 0.00 0.00

AMS 14.63 0.87 0.15 0.00

H2O 0.00 0.00 0.00 0.00

D 54.65 𝑘𝑚𝑜𝑙/ℎ𝑟

B 197.24 𝑘𝑚𝑜𝑙/ℎ𝑟

Dew po ints and bubble points:

Top section 𝑇𝑇 = 167.90 ℃

Bottom section 𝑇𝐵 = 182.18 ℃

Minimal and practical reflux ratio:

𝑁𝑚𝑖𝑛 12 𝑠𝑡𝑎𝑔𝑒𝑠

𝜃 1.49

𝑅𝑚𝑖𝑛 28.40

R = 1.5× 𝑅𝑚𝑖𝑛 42.60

Actual number of ideal stages 20 𝑠𝑡𝑎𝑔𝑒𝑠

Feed plate location 𝑁𝑒 = 16

𝐿𝑛 105.32 𝑘𝑚𝑜𝑙/ℎ𝑟

𝑉𝑛+1 108.07 𝑘𝑚𝑜𝑙/ℎ𝑟

𝐿𝑚 217.62 𝑘𝑚𝑜𝑙/ℎ𝑟

𝑉𝑚+1 210.65 𝑘𝑚𝑜𝑙/ℎ𝑟

Step 5: Column sizing:

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Overall column efficiency:

𝐸𝑜 44.90%

Actual number of real trays:

𝑁𝑎𝑐𝑡𝑢𝑎𝑙 41 stages

Plate contractor:

Sieve plate
Plate type
(perforated plate)

Step 6: Column diameter and internals design calculations:

Liquid-vapor flow factor:

𝐹𝐿𝑉,𝑡𝑜𝑝 0.055

𝐹𝐿𝑉,𝑏𝑜𝑡𝑡𝑜𝑚 0.05

Plate spacing: 0.40 m

Flooding constants:

𝐾1,𝑡𝑜𝑝 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.08

𝐾1,𝑏𝑜𝑡𝑡𝑜𝑚 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.07

Flooding velocity:

𝑢𝑓𝑡𝑜𝑝 1.36 𝑚/𝑠

𝑢𝑓𝑏𝑜𝑡𝑡𝑜𝑚 1.22𝑚/𝑠

Design velocity:

𝑢𝑣𝑡𝑜𝑝 1.15 𝑚/𝑠

𝑢𝑣𝑏𝑜𝑡𝑡𝑜𝑚 1.03 m/s

Maximum velocity flow rate:

𝑣 0.98 𝑚3 ⁄𝑠

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𝑣′ 2.19 m^3⁄s

Net area required:

𝐴𝑛,𝑡𝑜𝑝 0.86 𝑚2

𝐴𝑛,𝑏𝑜𝑡𝑡𝑜𝑚 2.05 m^2

Column cross-sectioned area:

𝐴𝑐,𝑡𝑜𝑝 0.98 𝑚2

𝐴𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 2.33 m^2

Column diameter:

𝐷𝑐,𝑡𝑜𝑝 1.12 𝑚

𝐷𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 1.72 m

Downcomer area:

𝐴𝑑 0.28 𝑚2

Active area:

𝐴𝑎 1.78 𝑚2

Hole area:

𝐴ℎ 0.18 𝑚2

Liquid flow pattern:

Cross flow Single pass

Weir dimensions:

Weir height 15.00 𝑚𝑚

Weir length 1.31 m

Weir liquid crest:

Maximum liquid flow rate 5.72 kg/s

Minimum liquid flowrate 4.00 𝑘𝑔/𝑠

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Hole size:

Plate thickness 5.00 𝑚𝑚

Hole diameter 6.00 𝑚𝑚

Weeping:

(ℎ𝑜𝑤 + ℎ𝑤 )𝑚𝑖𝑛 31.543 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

𝐾2 29.50

𝑢̌ℎ 6.54 𝑚/𝑠

𝑢̌ℎ𝑎𝑐𝑡𝑢𝑎𝑙 8.44 m/s

Plate pressure drop:

Dry pressure drop:

Hole pitch (𝑙𝑝 ) 15.00 𝑚𝑚

𝐴ℎ
14.4
𝐴𝑝

Plate thickness/hole diameter:

𝐶𝑜 0.85

ℎ𝑑 22.78 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Residual head:

ℎ𝑟 13.42 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

Total drop:

ℎ𝑡 72.18 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑

∆𝑃 27.05 mmHg/plate

Downcomer design [back-up]

ℎ𝑎𝑝 10.00 𝑚𝑚

𝐴𝑎𝑝 0.01 𝑚2

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ℎ𝑑𝑐 27.18 𝑚𝑚

ℎ𝑏 0.14 𝑚

𝑡𝑟 6.18 𝑠

Entrainment:

𝑢𝑛 1.04 𝑚/𝑠

Flooding percent 85.00%

Ψ 0.08

Trail layout:

Plate construction Sectional construction

Downcomers Vertical apron

Ring wide 50.00 𝑚𝑚

Calming zones 50.00 𝑚𝑚

𝜃𝑐 99 degrees

Mean length, unperforated edge strips 2.37 𝑚

Area of unperforated edge strips 0.12 𝑚2

Mean length of calming zone 0.12 𝑚

𝐴𝑝 1.54 𝑚2

Area of one hole 2.83E-05𝑚2

Number of holes 6280.00 holes

Tower Height 18.10 m

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Phenol Distillation
Table 6-20 :. Design summery for Phenol distillation column.

Step 1: Product specifications:

Component 𝑥𝐷 𝑥𝐵
Cumene 0.00 0.00
ACP 0.01 0.38
Phenol 0.99 0.62
Acetone 0.00 0.00
AMS 0.00 0.00
H2O 0.00 0.00
Step 2: Selection of operating conditions:
Types of the operation
Selection of column pressure 750.00mmHg
Step 3: Selection of the contacting
device:
Contacting device Plates
Feed specifications:
Component Fi (kmol/hr) 𝑥𝐹
Cumene 0.00 0.00
ACP 4.93 0.03
Phenol 192.17 0.97
Acetone 0.00 0.00
AMS 0.15 0.00
H2O 0.00 0.00
Component 𝐷𝑖 𝑥𝐷 𝐵𝑖 𝑥𝐵
Cumene 0.00 0.00 0.00 0.00
ACP 0.25 0.01 4.68 0.39
Phenol 184.48 0.99 7.69 0.62
Acetone 0.00 0.00 0.00 0.00
AMS 0.15 0.00 0.00 0.00
H2O 0.00 0.00 0.00 0.00

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D 184.87 𝑘𝑚𝑜𝑙/ℎ𝑟
B 12.37 𝑘𝑚𝑜𝑙/ℎ𝑟
Dew po ints and bubble points:
Top section 𝑇𝑇 = 181.84 ℃
Bottom section 𝑇𝐵 = 188.00 ℃
Minimal and practical reflux ratio:
𝑁𝑚𝑖𝑛 14 𝑠𝑡𝑎𝑔𝑒𝑠
𝜃 1.68
𝑅𝑚𝑖𝑛 27.00
R = 1.5× 𝑅𝑚𝑖𝑛 40.00
Actual number of ideal stages 22.00 𝑠𝑡𝑎𝑔𝑒𝑠
Feed plate location 𝑁𝑒 = 3.00
𝐿𝑛 100.44 𝑘𝑚𝑜𝑙/ℎ𝑟
𝑉𝑛+1 96.80 𝑘𝑚𝑜𝑙/ℎ𝑟
𝐿𝑚 200.87 𝑘𝑚𝑜𝑙/ℎ𝑟
𝑉𝑚+1 193.61 𝑘𝑚𝑜𝑙/ℎ𝑟
Step 5: Column sizing:
Overall column efficiency:
𝐸𝑜 43.60%
Actual number of real trays:
𝑁𝑎𝑐𝑡𝑢𝑎𝑙 48.00 stages
Plate contractor:
Sieve plate
Plate type
(perforated plate)
Step 6: Column diameter and internals design calculations:
Liquid-vapor flow factor:
𝐹𝐿𝑉,𝑡𝑜𝑝 0.01
𝐹𝐿𝑉,𝑏𝑜𝑡𝑡𝑜𝑚 0.06
Plate spacing: 0.40 m
Flooding constants:
𝐾1,𝑡𝑜𝑝 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.06

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𝐾1,𝑏𝑜𝑡𝑡𝑜𝑚 𝑐𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 0.07

Flooding velocity:
𝑢𝑓𝑡𝑜𝑝 1.13𝑚/𝑠
𝑢𝑓𝑏𝑜𝑡𝑡𝑜𝑚 1.24 𝑚/𝑠
Design velocity:
𝑢𝑣𝑡𝑜𝑝 0.96 𝑚/𝑠
𝑢𝑣𝑏𝑜𝑡𝑡𝑜𝑚 1.05 m/s
Maximum velocity flow rate:
𝑣 0.95 𝑚3 ⁄𝑠
𝑣′ 1.99 m^3⁄s
Net area required:
𝐴𝑛,𝑡𝑜𝑝 0.98 𝑚2
𝐴𝑛,𝑏𝑜𝑡𝑡𝑜𝑚 1.88 m^2
Column cross-sectioned area:
𝐴𝑐,𝑡𝑜𝑝 1.12 𝑚2
𝐴𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 2.14 m^2
Column diameter:
𝐷𝑐,𝑡𝑜𝑝 1.20 𝑚
𝐷𝑐,𝑏𝑜𝑡𝑡𝑜𝑚 1.67 m
Downcomer area:
𝐴𝑑 0.26 𝑚2
Active area:
𝐴𝑎 1.63 𝑚2
Hole area:
𝐴ℎ 0.16 𝑚2
Liquid flow pattern:
Cross flow Single pass
Weir dimensions:
Weir height 15.00 𝑚𝑚
Weir length 1.31 m
Weir liquid crest:

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Maximum liquid flow rate 5.79 kg/s

Minimum liquid flowrate 4.06 𝑘𝑔/𝑠
Hole size:
Plate thickness 5.00 𝑚𝑚
Hole diameter 6.00 𝑚𝑚
Weeping:
(ℎ𝑜𝑤 + ℎ𝑤 )𝑚𝑖𝑛 31.70 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
𝐾2 29.50
𝑢̌ℎ 7.29 𝑚/𝑠
𝑢̌ℎ𝑎𝑐𝑡𝑢𝑎𝑙 8.54 m/s
Plate pressure drop:
Dry pressure drop:
Hole pitch (𝑙𝑝 ) 15.00 𝑚𝑚
𝐴ℎ
14.40
𝐴𝑝
Plate thickness/hole diameter:
𝐶𝑜 0.85
ℎ𝑑 24.34 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
Residual head:
ℎ𝑟 12.88 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
Total drop:
ℎ𝑡 73.42 𝑚𝑚 𝑙𝑖𝑞𝑢𝑖𝑑
∆𝑃 33.53 mmHg/plate
Downcomer design [back-up]
ℎ𝑎𝑝 10.00 𝑚𝑚
𝐴𝑎𝑝 0.01 𝑚2
ℎ𝑑𝑐 40.83 𝑚𝑚
ℎ𝑏 0.15 𝑚
𝑡𝑟 6.49 𝑠
Entrainment:
𝑢𝑛 1.05 𝑚/𝑠

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Flooding percent 85.00%

Ψ 0.08
Trail layout:
Plate construction Sectional construction
Downcomers Vertical apron
Ring wide 50.00 𝑚𝑚
Calming zones 50.00 𝑚𝑚
𝜃𝑐 99.00 degrees
Mean length, unperforated edge
2.27 𝑚
strips
Area of unperforated edge strips 0.12 𝑚2
Mean length of calming zone 0.11 𝑚
𝐴𝑝 1.41 𝑚2
Area of one hole 2.83E-05 𝑚2
Number of holes 5768.35 holes
Tower Height 20.90 m

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References

[1] Levenspiel, O. (1999). Chemical reaction engineering. 3rd ed. New Delhi: Wiley India.

[2] Kantarcia, N., Borakb, F. and O. Ulgen, K. (2004). Bubble Column Reactor. Turkey: 153lsevier.

[3] Sinnott, R. (2005). Chemical engineering. Amsterdam: Elsevier Butterworth-Heinemann.

[4] Tahir, Z., Waqas, A. and Hameed, U. (2005). Production of Cyclohexane from Benzene. Pakistan:
Lahore University of engineering and technology.

[5] Sui, M. and Sakarinen, E. (2017). Design of a bubble column reactor. Aalto University.

[6] IchemE, 1998. THERMAL DECOMPOSITION KINETICS OF CUMENE HYDROPEROXIDE. Taiwan.

[7] Zhao, X., 2015. A Kinetic Study Of The Hydrogenation And Dimerization Of Styrene And Α-
Methylstyrene On Ni-Mo-S Catalyst. The University of British Columbia.

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Chapter 7: Ancillaries Design

Mixing and storage facilities
Raw materials feed and products are stored in storage tanks of various sizes and types.
Vertical cylindrical tanks, with flat bases and conical roofs, are universally used for the bulk
storage of liquids at atmospheric pressure. Tank sizes vary from a few hundred gallons (tens of
cubic meters) to several thousand gallons (several hundred cubic meters).
Sizing of storage and mixing tanks
The storage tanks can be sizing using the following equation:
𝜋𝐷 2
𝑉𝑁 = (𝐻1 + 𝐻2 + ℎ𝑡 ) + 𝑉1 + 𝑉2 (7.1)
4

Where:
VN ≡ Nominal capacity of the tank.
D ≡ diameter of the tank.
H1 ≡ Tank dead height.
H2 ≡ vapor space height or maximum safe working level.
V1 ≡ Net-working capacity of the tank.
V2 ≡ Liquid volume pumped out of the tank in three minutes.
H1 and H2 can be calculated from the following equations:
H1 = 2.5 d1 +5 inch (7.2)
Where:
d1 is the inlet nozzle, the minimum inlet nozzle = 12 inch.
H1 = 35 inch = 0.889 m
H2 = 1.5 d2
d2 is the outlet nozzle, the minimum inlet nozzle = 12 inch.
H2 = 18 inch = 0.457 m
0.04𝑉1
ℎ𝑡 = (7.3)
𝜋𝐷 2

Where ht is in meters.
Procedure:
1. Assume first larger value of net-working capacity (V1), considering V≥V1.
2. Read diameter related to V from Table (7-1).
3. Calculate the nominal capacity 𝑉𝑁 from equation (7.1).

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4. Compare 𝑉𝑁 with V, if 𝑉𝑁 ≤ V, then select the related diameter and height of V from the
table. If 𝑉𝑁 > V then pick next greater value for V from the table and repeat the steps.
Table 7-1:Nominal capacities of standard vertical cylindrical tanks, m3.

Cumene storage tank

This tank is used to store liquid cumene product.
Mass flowrate = 24000 kg/hr
Volumetric flowrate = 27.90698 m3 ⁄hr
Storage period = 1 day
𝑉1 ≡ Net-working capacity of the tank = 669.767 m3 = 178130.6121 gal
Beyond 10,000 gal, use vertical tanks on concrete foundations.
From Table (7-1), V = 785 m3, D = 10 m, Height = 10 m
ℎ𝑡 = 0.08527 m
𝑉2 = 1.395 m3
From equation (7.1), 𝑉𝑁 = 779.789 < 𝑉1

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Then:
Volume of the tank = 785 m3
The diameter of the tank = 10 m
The height of the tank = 10 m
Acetone storage tank
This tank is used to store liquid acetone product.
Mass flowrate = 11742.79 kg/hr
Volumetric flowrate = 14.666 m3 ⁄hr
Storage period = 1 day
𝑉1 ≡ Net-working capacity of the tank = 351.98 m3 = 93612.9 gal
Beyond 10,000 gal, use vertical tanks on concrete foundations.
From Table (7-1), V = 452 m3, D = 8 m, Height = 9 m
ℎ𝑡 = 0.07 m
𝑉2 = 0.7332 m3
From equation (7.1), 𝑉𝑁 = 421.47 < 𝑉1
Then:
Volume of the tank = 452 m3
The diameter of the tank = 8 m
The height of the tank = 9 m
Phenol storage tank
This tank is used to store liquid phenol product.
Mass flowrate = 17388.027 kg/hr.
Volumetric flowrate = 16.22 m3/hr.
For 1 day storage period.
𝑉1 ≡ Net-working capacity of the tank = 389.2868 m3 = 103534.29 gal
Beyond 10,000 gal, use vertical tanks on concrete foundations.
From Table (7-1), V = 502 m3, D = 8 m, Height = 10 m
ℎ𝑡 = 0.0774 m
𝑉2 = 0.811 m3
From equation (7.1), 𝑉𝑁 = 459.225 < 𝑉1
Then:

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Volume of the tank = 502 m3

The diameter of the tank = 8 m
The height of the tank = 10 m
Cumene mixing tank 1
This tank is used to mix fresh with recycled cumene.
Mass flowrate = 25976.64 kg/hr
Volumetric flowrate = 30.1389 m3 ⁄hr
Mixing period = 5 minutes
𝑉1 ≡ Net-working capacity of the tank = 2.5116 m3
From Table (7-1), V = 14 m3, D = 3 m, Height = 2 m
ℎ𝑡 = 0.00355 m
𝑉2 = 1.51 m3
From equation (7.1), 𝑉𝑁 = 13.218 < 𝑉1
Then:
Volume of the tank = 14 m3
The diameter of the tank = 3 m
The height of the tank = 2 m
Cumene mixing tank 2
This tank is used to mix the mixture of the first mixing tank with another recycled cumene.
Mass flowrate = 29766.699 kg/hr
Volumetric flowrate = 34.53426 m3 ⁄hr
Mixing period = 5 minutes
𝑉1 ≡ Net-working capacity of the tank = 2.878 m3
From Table (7-1), V = 14 m3, D = 3 m, Height = 2 m
ℎ𝑡 = 0.00407 m
𝑉2 = 1.726 m3
From equation (7.1), 𝑉𝑁 = 13.807 < 𝑉1
Then:
Volume of the tank = 14 m3
The diameter of the tank = 3 m
The height of the tank = 2 m

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Heat exchangers
Introduction
The transfer of heat to and from process fluids is an essential part of most chemical
processes. The most commonly used type of heat-transfer equipment is the shell and tube heat
exchanger.
The prime objective in the design of an exchanger is to determine the surface area required for
the specified duty (rate of heat transfer) using the temperature differences available.
The shell and tube exchanger is by far the most commonly used type of heat-transfer equipment
used in the chemical and allied industries. The advantages of this type are:
1. The configuration gives a large surface area in a small volume.

2. Good mechanical layout: a good shape for pressure operation.

3. Uses well-established fabrication techniques.

4. Can be constructed from a wide range of materials.

5. Easily cleaned.

6. Well-established design procedures.

The steps in a typical design procedure are given below:

1. Define the duty: heat-transfer rate, fluid flowrates, and temperatures.

2. Collect together the fluid physical properties required: density, viscosity, thermal
conductivity.

3. Decide on the type of exchanger to be used.

4. Select a trial value for the overall coefficient, U.

5. Calculate the mean temperature difference,∆𝑇𝑚 .

6. Calculate the area required from equation (7.4).

7. Decide the exchanger layout.

8. Calculate the individual coefficients.

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9. Calculate the overall coefficient and compare with the trial value. If the calculated value
differs significantly from the estimated value, substitute the calculated for the estimated
value and return to step 6.

10. Calculate the exchanger pressure drop; if unsatisfactory return to steps 7 or 4 or 3, in that
order of preference.

Basic design procedure and theory:

The general equation for heat transfer across a surface is:
𝑄 = 𝑈𝐴∆𝑇𝑚 (7.4)
Where:
Q ≡ Heat transferred per unit time, W.
U ≡ The overall heat transfer coefficient, W/m2°C.
A ≡ Heat-transfer area, m2.
∆𝑇𝑚 ≡ The mean temperature difference, the temperature driving force, °C.
𝑑
1 1 1 𝑑𝑜 𝑙𝑛( 𝑜 ) 𝑑 1 𝑑 1
𝑑𝑖
= +ℎ + + 𝑑𝑜 × ℎ + 𝑑𝑜 × ℎ (7.5)
𝑈𝑜 ℎ𝑜 𝑜𝑑 2𝑘𝑤 𝑖 𝑖𝑑 𝑖 𝑖

Where:
𝑈𝑜 ≡ The overall coefficient based on the outside area of the tube, W/m2°C.
ℎ𝑜 ≡ Outside fluid film coefficient, W/m2°C.
ℎ𝑖 ≡ Inside fluid film coefficient, W/m2°C.
ℎ𝑜𝑑 ≡ Outside dirt coefficient (fouling factor), W/m2°C.
ℎ𝑖𝑑 ≡ Inside dirt coefficient, W/m2°C.
𝑘𝑤 ≡ Thermal conductivity of the tube wall material, W/m° C.
𝑑𝑖 ≡ Tube inside diameter, m.
𝑑𝑜 ≡ Tube outside diameter, m.
(𝑇1 −𝑡2 )−(𝑇2 −𝑡1 )
∆𝑇𝑙𝑚 = (𝑇 −𝑡2 ) (7.6)
𝑙𝑛 (𝑇1
2 −𝑡1 )

Where:
∆𝑇𝑙𝑚 ≡ log mean temperature difference.
𝑇1 ≡ Inlet shell-side fluid temperature.
𝑇2 ≡ Outlet shell-side fluid temperature.
𝑡1 ≡ Inlet tube-side temperature.

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𝑡2 ≡ Outlet tube-side temperature.

∆𝑇𝑚 = 𝐹𝑡 ∆𝑇𝑙𝑚 (7.7)

Where:
∆𝑇𝑚 ≡ True temperature difference, the mean temperature difference for use in the design
equation (7.4).
𝐹𝑡 ≡ The temperature correction factor.
The correction factor is a function of the shell and tube fluid temperatures, and the number
of tube and shell passes. It is normally correlated as a function of two dimensionless temperature
ratios:
(𝑇 −𝑇 )
𝑅 = (𝑡1−𝑡2) (7.8)
2 1

And
(𝑡 −𝑡 )
𝑆 = (𝑇2 −𝑡1 ) (7.9)
1 1

Figure 7-1:Temperature correction factor: one shell pass; two or more even tube passes.

Tube-side heat transfer coefficient:

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ℎ𝑖 𝑑𝑖
= 𝑗ℎ 𝑅𝑒𝑃𝑟 0.33 (7.10)
𝑘𝑓

Where:
ℎ𝑖 ≡ Heat transfer coefficient for tube side.
𝑑𝑖 ≡ Tube inside diameter.
𝑘𝑓 ≡ Fluid thermal conductivity.
𝑗ℎ ≡ Heat transfer factor, which can be estimated from Figure (7-1).
Re ≡ Reynolds number = 𝜌𝑢𝑡 𝑑𝑒 ⁄𝜇 (7.11)
Pr ≡ Prandtl number = 𝐶𝑝 × 𝜇 ⁄𝑘𝑓 (7.12)
𝜌 ≡ Fluid density at the bulk fluid temperature.
𝑑𝑒 ≡ 4× cross-sectional area for flow / wetted perimeter = 𝑑𝑖 for tubes.
𝑢𝑡 ≡ Fluid velocity, m/s.
𝜇 ≡ Fluid viscosity at the bulk fluid temperature, Ns/m2.
𝐶𝑝 ≡ Fluid specific heat, heat capacity, J/kg℃.

Figure 7-2: Tube-side heat transfer factor.

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Tube-side pressure drop:

There are two major sources of pressure loss on the tube-side of a shell and tube exchanger: the
friction loss in the tubes and the losses due to the sudden contraction and expansion and flow
reversals that the fluid experiences in flow through the tube arrangement.
𝐿 𝜇 −𝑚 𝜌𝑢𝑡2
∆𝑃𝑡 = 𝑁𝑝 [8𝑗𝑓 (𝑑 ) (𝜇 ) + 2.5] (7.13)
𝑖 𝑤 2

Where:
∆𝑃𝑡 ≡ Tube-side pressure drop, N/m2(Pa).
Np ≡ Number of tube-side passes.
𝑢𝑡 ≡ Tube-side velocity, m/s.
L ≡ Length of one tube.
𝑗𝑓 ≡ Dimensionless friction factor, which can be obtained from Figure (7-3)
m = 0.25 for laminar flow, Re < 2100.
= 0.14 for turbulent flow, Re > 2100.
𝜇
is taken as 1.
𝜇𝑤

Figure 7-3:Tube-side friction factors.

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Shell-side heat transfer coefficient:

1⁄
𝑁𝑡 𝑛1
𝐷𝑏 = 𝑑𝑜 (𝐾 ) (7.14)
1

Where:
𝐷𝑏 ≡ Bundle diameter, m.
𝑁𝑡 ≡ Number of tubes.
N1 & K1 ≡ Constants depend on tubes arrangement and number of tube passes. Some values of
these are shown on the following table.
Table 7-2: Constants used in equation (7.13).

Shell diameter:
𝐷𝑠 = 𝐷𝑏 + 𝑐𝑙𝑒𝑎𝑟𝑎𝑛𝑐𝑒 (7.15)
The clearance between shell and tube bundle depends on bundle diameter and type of head. It
can be estimated using Figure (7-4)

Figure 7-4: Shell-bundle clearance.

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𝑙
𝐴𝑠 = ( 𝑝𝑡 – 𝑑𝑜 ) × 𝐷𝑠 × 𝑝𝐵 (7.16)
𝑡

Where:
𝑃𝑡 ≡ Tube pitch, 𝑃𝑡 = 1.25𝑑𝑜 .
do ≡ Tube outside diameter,
Ds ≡ Shell inside diameter, m,
lB ≡ Baffle spacing, lB = 0.2 to 1 shell diameter.

𝐺𝑠 = 𝑊𝑠 ⁄𝐴𝑠 (7.17)
𝑢𝑠 = 𝐺𝑠 / (7.18)
Where:
𝑊𝑠 ≡ Fluid flow-rate on the shell-side, kg/s,
 ≡ Shell-side fluid density, kg/m3.
Equivalent diameter for a square pitch arrangement:
1.27
𝑑𝑒 = (𝑝𝑡 2 − 0.785𝑑𝑜 2 ) (7.19)
𝑑𝑜

Equivalent diameter for an equilateral triangular pitch arrangement:

1.10
𝑑𝑒 = (𝑝𝑡 2 − 0.917𝑑𝑜 2 ) (7.20)
𝑑𝑜

Re = 𝐺𝑠 𝑑𝑒 /= 𝑢𝑠 𝑑𝑒  / (7.21)
ℎ𝑠 𝑑𝑒
𝑁𝑢 = = 𝑗ℎ 𝑅𝑒𝑃𝑟 1⁄3 (7.22)
𝑘𝑓

Where:
ℎ𝑠 ≡ Heat transfer coefficient for shell side,
𝑗ℎ ≡ Heat transfer factor for shell side, can be estimated from Figure (7-5).

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Figure 7-5: Shell-side heat transfer factor.

Shell-side pressure drop:

0.14
𝐷 𝐿 𝑢𝑠2 
𝑃𝑠 = 8𝑗𝑓 (𝑑 𝑠 ) (𝑙 ) 2
( ) (7.23)
𝑒 𝐵 𝑤

Where:
L ≡ Tube length.
𝐼𝐵 ≡ Baffle spacing.
𝑗𝑓 ≡ Shell friction factor, which can be estimated from Figure (7-6).

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Figure 7-6:Shell-side friction factors.

Heat Exchanger 1 (E-101)

Step 1:
135337.1109 Kg/hr of stream 4 at 62 ℃ is cooled to 52.986 ℃, by exchange with 35949.74 kg/hr
of stream 5 which is heated from 37 ℃ to 52 ℃.
Fouling factor for stream 4 is 0.0003(𝑚2 ℃⁄𝑊 ), and 0.0003 (𝑚2 ℃⁄𝑊 ) for stream 5.
𝑄 = 341.8135 𝑘𝑊
𝑄 = 𝑚̇𝐶𝑝∆𝑇 (7.24)

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Step 2:
Physical properties are calculated at the mean temperature.
Table 7-3: Physical properties for liquid mixture in shell-side.

Property Value
𝑇𝑖𝑛 62.00 ℃

𝑇𝑜𝑢𝑡 52.99℃

𝑇𝑚𝑒𝑎𝑛 57.49℃

𝐶𝑝 29.09 kJ/kg.℃

K 2.86E-02 W/m. ℃

𝜌 1.50 kg/m3

𝜇 2.02E-02 Cp

Table 7-4:Physical properties for liquid mixture in tube-side.

Property Value
𝑇𝑖𝑛 37.00 ℃

𝑇𝑜𝑢𝑡 52 .00℃

𝑇𝑚𝑒𝑎𝑛 44.50℃

𝐶𝑝 329.98 kJ/kg.℃

K 8.28E-02 W/m. ℃

𝜌 643.73 kg/m3

𝜇 1.7E-02 Cp

Step 3:
Overall coefficient:
For this type of process, the overall coefficient lies between 100-300 W/m2.K.
U is taken as 300 W/m2.K

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Step 4:
Exchanger type and dimensions:
An even number of tube passes is usually the preferred arrangement, as this positions the inlet
and outlet nozzles at the same end of the exchanger, which simplifies the pipe work.
Start with one shell pass and 3 tube passes.
(62 − 52) − (52.986 − 37)
∆𝑇𝑙𝑚 = = 12.75984℃
62 − 52
𝑙𝑛 ( )
52.986 − 37
(37 − 52)
𝑅= = 1.664
(52.986 − 62)
(52.986 − 62)
𝑆= = 0.3606
(37 − 62 )
From Figure (7-1)𝐹𝑡 = 0.95, which is acceptable.
So ∆𝑇𝑚 = 0.95 × 12.758 = 12.1285 ℃
Step 5:
Heat transfer area:
341.8135 × 103
𝐴𝑜 = = 93.9983 𝑚2
12.1285 × 300
Step 6:
Layout and tube size:
Using a split-ring floating head exchanger for efficiency and ease of cleaning.
Since operating pressure is high, stainless steel can be used for tubes and stainless can be
used for the shell.
Since stream 5 has higher pressure and stream 4 is more viscous; stream 5 is located at the
tube and stream 4 at the shell.
Use 25 mm outside diameter, 21.8 mm inside diameter, 7.32 m long tubes on a triangular 31.25
mm pitch (pitch/dia. = 1.25).
Step 7:
Number of tubes:
Area of one tube (neglecting thickness of tube sheets)
= 𝜋 × 25 × 10−3 × 6.1 = 0.47889𝑚2
Number of tubes = 93.9983⁄0.47889 = 196.297 ≈ 196
So, for 2 passes, tubes per pass = 98

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Check the tube-side velocity at this stage to see if it looks reasonable.

𝜋
Tube cross-sectional area = 4 ( 21.8 × 10−3 )2 = 0.000373 𝑚2

Area per pass = 98 × 0.000373 = 0.036614 𝑚2

135337.1
Volumetric flow = 3600×643.7261 = 0.0584 𝑚3 ⁄𝑠
0.0584
Tube-side velocity = 0.036614 = 1.6 𝑚/𝑠

The velocity is satisfactory, between 1 to 2 m/s.

Step 8:
Bundle and shell diameter:
From Table (7-2), for 2 tube passes, 𝐾1 = 0.249, 𝑛1 = 2.207.
196 1⁄2.207
𝐷𝑏 = 25 × ( ) = 513.38 𝑚𝑚
0.249
For a split-ring floating head exchanger the typical shell clearance from Figure (7-9) is 67 mm,
so the shell inside diameter:
𝐷𝑠 = 513.38 + 67 = 580.3882 𝑚𝑚
Step 9:
Tube-side heat transfer coefficient:
643.7261 × 21.8 × 1.6
𝑅𝑒 = = 13100 (1 × 104 )
1.7 × 10−5
329.9813 × 1000 × 1.7 × 10−3
𝑃𝑟 = = 6790
8.281 × 10−2
𝐿 6.1
= = 279.816
𝑑𝑖 21.8 × 10−3
From Figure (7-3) 𝑗ℎ = 0.007
𝑁𝑢 = 0.007 (13100)(6790)0.33 = 1690.706
1690.706 × 0.0828
ℎ𝑖 = = 6423.065 𝑊 ⁄𝑚2. . 𝐾
21.8 × 10−3
Step 10:
Shell-side heat transfer coefficient:
Kern’s method will be used.
As a first trial take the baffle spacing = 𝐷𝑠 *0.2 = 580.3882 * 0.2 = 116.0776, say 116 mm. This
spacing should give good heat transfer without too high a pressure drop.

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(31.25−25)
𝐴𝑠 = × 116.0776 × 580.3882 = 13474.02 𝑚𝑚2 = 13.474 𝑚2
31.25
1.1
𝑑𝑒 = (31.252 − 0.917 × 252 ) = 17.751 𝑚𝑚
25
35949.74 1
Volumetric flowrate on shell-side = × 1.5 = 6.66 𝑚3 ⁄𝑠
3600
6.66
Shell-side velocity = 13.47 = 0.494 𝑚⁄𝑠

0.494 × 1.5 × 17.751 × 10−3

𝑅𝑒 = = 652.0093, (0.6 × 103 )
2.02 × 10−5
Using segmental baffles with a 25% cut. This should give a reasonable heat transfer coefficient
without too large a pressure drop.
From Fig+-ure (7-6), 𝑗ℎ = 0.0143.
Neglecting the viscosity correction:
2.86 × 10−2
ℎ𝑠 = ( ) × 0.143 × 652 × (20.5)1/3 = 407 𝑊 ⁄𝑚2 . ℃
17.75 × 10−3
Step 11:
Overall coefficient:
25
1 1 25 25 × 10−3 ln (21.8) 1
= ( + 0.0003) × + + + 0.0003
𝑈𝑜 6423.065 21.8 2 × 45 407
= 0.00325 𝑚2 . ℃/𝑊
∴ 𝑈𝑜 = 307.7025 𝑊 ⁄𝑚2 . ℃
(𝑈𝑜,𝑎𝑠𝑠𝑢𝑚𝑒𝑑 – 𝑈𝑜,𝑐𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑 )
Error = × 100 (7.25)
𝑈𝑜,𝑐𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑

(307.7025−300)
𝐸𝑟𝑟𝑜𝑟 = × 100 = 2.567 %
300

The error is too small so it can be neglected.

Step 12:
Pressure drop:
Tube-side:
From Figure (7-8) 𝑗𝑓 = 0.03
∴ ∆𝑝𝑡 = 57.0363 𝑘𝑃𝑎
Shell-side:
From Figure (7-5)
𝑗𝑓 = 0.194

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From equation (7.23), neglecting viscosity correction:

∆𝑝𝑠 = 61.24 𝑘𝑃𝑎

The design calculations are summarized in table below

Table 7-5: Design summary for E-(101).

Shell-Side Fluid Mixture of (N2,O2)

Tube-Side Fluid Mixture of (Cumene, Phenol & AMS)
Flow Rate For shell-Side fluid 135337.10 Kg/hr
Flow Rate For Tube-Side Fluid 35949.74 Kg/hr
Fouling Factor In Shell 0.0003 (W/m2.s)-1
Fouling Factor In Tubes 0.0003 (W/m2.s)-1
Specific heat For shell-Side fluid 29.09 KJ/Kg. ℃
Specific heat For Tube-Side Fluid 329.98 KJ/Kg. ℃
Thermal conductivity For shell-Side fluid 0.029 W/m.K
Thermal conductivity For Tube-Side Fluid 0.083 W/m.K
Density For shell-Side fluid 1.51 Kg/m3
Density For Tube-Side Fluid 643.73 Kg/m3
Viscosity For shell-Side fluid 0.02 Cp
Viscosity For Tube-Side Fluid 1.70 Cp
Temperature In (Shell-Side Fluid) 62.00 ℃
Temperature Out (Shell-Side Fluid) 52.98 ℃
Temperature In (Tube-Side Fluid) 37.00 ℃
Temperature Out (Tube-Side Fluid) 52.00 ℃
𝛥Tm 12.76 ℃
Required Duty 341.81 KW
Heat Transfer Area, Ao 93.99 m2
Overall Coefficient (assumption) 300.00 W/m2. ℃
Tube-Side Heat Transfer Coefficient 6423.07 W/m2. ℃
Shell-Side Heat Transfer Coefficient 407.00 W/m2. ℃
Material of Construction Carbon Steel

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Tube Outer Diameter 25.00 mm

Tube Internal Diameter 21.80 mm
Tube Length 6100.00 mm (6.1 m)
Tube Pitch 31.25 mm
Number of Tubes 196.00
Number of shell And tube Passes 1-2 shell and tube
Shell Internal Diameter 580.39 mm
Baffle Spacing 116.077 mm
Baffle Cut 35.00%
Overall Coefficient (calculation) 307.70 W/ m2. ℃
Error 2.57 %
Tube-Side Pressure Drop 0.57 bar
Tube side velocity 1.60 m/s
Shell -Side Pressure Drop 0.61 bar
Shell side velocity 0.49 m/s
Head Type Floating Head

The same procedure used for design of E-100 is used for the rest of the heat exchangers
and the results for each heat exchanger are tabulated below.
Cooler 1 (E- 102)
Table 7-6: Design summary for E-(102).

Temperature in (tube-side fluid) (Air) 52.99 ℃

Temperature out (tube-side fluid) 37.00 ℃
Temperature in (shell-side fluid) 25.00℃
Temperature out (shell-side fluid) 30.00 ℃
Fouling factor in tube 0.0003 (W/m2.s)-1
Fouling factor in shell 0.0003 (W/m2.s)-1
Duty 606.00 kW
Overall Coefficient (assumption) 100.00 W/m2.℃
Heat transfer area 654.48 m2
Tube-side heat transfer coefficient 128.47 W/m2℃

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Shell-side heat transfer coefficient 1509.45 W/m2.℃

Overall heat transfer coefficient 105.00 W/m2.℃
Tube outer diameter 50 mm
Tube internal diameter 47 mm
Tube length 6.10 m
Tube pitch 0.06 mm
Number of tubes 682.00
Number of shell and tube passes 1shell –2 tube passes
Shell inside diameter 1.90 m
Baffle spacing 0.379M

Boiler 1 (E- 103)

The design calculations are summarized in table below

Table 7-7:Design summary for E-(103).

Temperature in (tube-side fluid) 52.00 ℃

Temperature out (tube-side fluid) 55.00 ℃
Temperature in (shell-side fluid)(Steam) 127. 00 ℃
Temperature out (shell-side fluid)(Steam) 127.00 ℃
Fouling factor in tube 0.0003 (W/m2.s)-1
Fouling factor in shell 0.0003 (W/m2.s)-1
Duty 68.00 KW
Overall Coefficient (assumption) 100.00 W/m2.℃
Heat transfer area 9.30 m2
Tube-side heat transfer coefficient 1353.62 W/m2℃
Shell-side heat transfer coefficient 130.44 W/m2.℃
Overall heat transfer coefficient 110.00 W/m2.℃
Tube outer diameter 50.00 mm
Tube internal diameter 47.00 mm
Tube length 6.10 m
Tube pitch 0.06 m
Number of tubes 10.00
Number of shell and tube passes 1shell –2 tube passes

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Shell inside diameter 0.34 m

Baffle spacing 0.67 m

Heat Exchanger 2 (E- 104)

The design calculations are summarized in table below

Table 7-8: Design summary for E-(104).

Mixture of ( Cumene, ACP, Phenol, Acetone,

Shell-Side Fluid
AMS & H2O)
Tube-Side Fluid Mixture of ( Cumene, Phenol & AMS)

Flow Rate For shell-Side fluid 1947.37 Kg/hr

Flow Rate For Tube-Side Fluid 36152.50 Kg/hr

Fouling Factor In Shell 0.0003 (W/m2.s)-1

Fouling Factor In Tubes 0.0003 (W/m2.s)-1

Specific heat For shell-Side fluid 280.90 KJ/Kg. ℃

Specific heat For Tube-Side Fluid 166.70 KJ/Kg. ℃

Thermal conductivity For shell-Side fluid 0.05 W/m.K

Thermal conductivity For Tube-Side Fluid 0.15 W/m.K

Density For shell-Side fluid 276.28 Kg/m3

Density For Tube-Side Fluid 914.12 Kg/m3

Viscosity For shell-Side fluid 0.014 Cp

Viscosity For Tube-Side Fluid 0.85 Cp

Temperature In (Shell-Side Fluid) 96.00 ℃

Temperature Out (Shell-Side Fluid) 65.00 ℃

Temperature In (Tube-Side Fluid) 55.00 ℃

Temperature Out (Tube-Side Fluid) 56.94 ℃

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𝛥Tm 20.90 ℃

Required Duty 40.86 KW

Heat Transfer Area, Ao 9.77 m2

Overall Coefficient (assumption) 200.00 W/m2. ℃

Tube-Side Heat Transfer Coefficient 387.13 W/m2. ℃

Shell-Side Heat Transfer Coefficient 676.62 W/m2. ℃

Material of Construction Carbon Steel

Tube Outer Diameter 25.00 mm

Tube Internal Diameter 21.80 mm
Tube Length 2440 mm (2.44 m)

Tube Pitch 31.25 mm

Number of Tubes 51.00
Number of shell And tube Passes 1-2 shell and tube

Shell Internal Diameter 331.83 mm

Baffle Spacing 66.37 mm

Baffle Cut 35.00%

Overall Coefficient (calculation) 204.12 W/ m2. ℃

Error 2.06 %
Tube-Side Pressure Drop 0.51 bar
Tube side velocity 1.15 m/s
Shell -Side Pressure Drop 0.56 bar
Shell side velocity 0.45 m/s
Head Type Floating Head

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Boiler 2 (E- 105)

The design calculations are summarized in table below

Table 7-9:Design summary for E-(105).

Temperature in (tube-side fluid) 56.94 ℃

Temperature out (tube-side fluid) 120.00 ℃
Temperature in (shell-side fluid) 127.00 ℃
Temperature out (shell-side fluid) 127.00 ℃
Fouling factor in tube 0.0003 (W/m2.s)-1
Fouling factor in shell 0.0003 (W/m2.s)-1
Duty 1330.00 KW
Overall Coefficient (assumption) 100.00 W/m2.℃
Heat transfer area 485.90 m2
Tube-side heat transfer coefficient 247.8799 W/m2℃
Shell-side heat transfer coefficient 238.4327 W/m2.℃
Overall heat transfer coefficient 109.592 W/m2.℃
Tube outer diameter 50.00 mm
Tube internal diameter 47.00 mm
Tube length 6.10 m
Tube pitch 0.06 m
Number of tubes 507.00
Number of shell and tube passes 1shell –2 tube passes
Shell inside diameter 1.66 m
Baffle spacing 0.33 m

Pumps
Pump Selection
Pumps can be classified into two general types:
1. Dynamic pumps, such as centrifugal pumps.
2. Positive displacement pumps, such as reciprocating and diaphragm pumps.
The single-stage, horizontal, overhung, centrifugal pump is by far the most commonly used
type in the chemical process industry.
Pump selection is made on the flow rate and head required, together with other process
considerations, such as corrosion or the presence of solids in the fluid.(1)

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Figure 7-7: Centrifugal pump selection guide. *Single-stage >1750 rpm, multi-stage 1750
rpm(1)
The chart shown in Figure 7.7 can be used to determine the type of pump required for a
particular head and flow rate.
Power requirement
To transport a liquid from one vessel to another through a pipeline, energy has to be
supplied to:
1. Overcome the friction losses in the pipes;
2. Overcome the miscellaneous losses in the pipe fittings (e.g. bends), valves, instruments
3. etc.;
4. Overcome the losses in process equipment (e.g. heat exchangers);
5. Overcome any difference in elevation from end to end of the pipe;
6. Overcome any difference in pressure between the vessels at each end of the pipeline.
The total energy required can be calculated from the equation:
∆𝑃 ∆𝑃𝑓
𝑔∆𝑧 + 𝜌
− 𝜌
− 𝑊 = 0 …………………………………………………………. (7.26)

𝑊=work done, J/kg

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∆𝑃𝑓 = pressure drop due to friction, including miscellaneous losses, and equipment losses,
N/m2,
∆𝑃= difference in system pressures (P1 – P2), N/m2,
𝜌= liquid density, kg/m3,
∆𝑧= difference in elevations (z1 – z2), m,
𝑔= acceleration due to gravity, m/s2.

∆𝑃×𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒
𝑃𝑜𝑤𝑒𝑟 = ……………………………………………………. (7.27)
𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦

The efficiency will depend on the type of pump used and the operating conditions. For
preliminary design calculations, the efficiency of centrifugal pumps can be determined using
Figure. 7.8. (1)

Figure 7-8:Centrifugal pump efficiency

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Pump P-101 (Cumene)

Height= 6.67*10-3 m
Work = 0.065 Kj/kg
Power = 0.724 kW
Power in Hysys= 0.724 Kw
Error=0%
Centrifugal pump with 75% efficiency
Pump P-102 (Cleavage)

Height= 0.011 m
Work = 0,103 Kj/kg
Power = 1.38 KW
Power in Hysys =1.38 KW
Error =0%
Centrifugal pump with 75% efficiency

Compressor
Compressors are used to handle large volumes of gas at pressure increases from 10.32 kPa
(1.5lbg/in2) to several hundred kPa (lbg/in2).
We can divide compressors into two major categories:
1. Continuous-flow compressors.
a. Centrifugal compressors
b. Axial flow compressors
2. Positive displacement compressors
a. Rotary compressors
b. Reciprocating compressors (2)

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Figure 7-9:Compressor coverage chart based on the normal range of operation of commercially
available types shown. Solid lines: use left ordinate, head. Broken lines: use right ordinate,
pressure. To convert cubic feet per minute to cubic meters per hour, multiply

Centrifugal compressor (C-101)

Centrifugal compressors in general are used for higher pressure ratios and lower flow rates
compared to lower-stage pressure ratios and higher flow rates in axial compressors. The pressure
ratio in a single-stage centrifugal compressor varies depending on the industry and application. (2)
A compressor to be used to boost the pressure of air to feed plant’s oxidation process.
Suction pressure: 15 psia
Discharge pressure: 22 psia
Flow requirement: 114806 lm3/hr
Suction temperature: 298 k
“n” value
𝑐𝑝
𝑛= ……………………………………………………………………………………………………………………………… (7.28)
𝑐𝑝 −𝑅

n=1.4
Compressibility factor “z”
Critical Pressure (Pc) and Critical Temperature (Tc) – These two values are used to calculate a
value called compressibility (Z). Both Pc and Tc are published for most gasses.
Z=1

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Compression ratio
R=Pd/Ps …………………………………………………………………………… (7.29)
R=1.5, single stage will be used

Discharge temperature
𝑛−1
𝑇𝑑 = 𝑇𝑠 ∗ 𝑅 𝑛 ……………………………………………………………………… (7.30)
n=specific heat ratio of the gas.
𝑅=compression ratio
𝑇𝑑 =discharge temperature
𝑇𝑠 =suction temperature
𝑇𝑑 =335 R

Volumetric efficiency
1
𝑉𝐸% = 93 − 𝑅 − 8(𝑅 𝑛 − 1) ………………………………………. (7.31)

VE%=76%
Polytropic head
𝑛−1
𝑛 𝑧𝑅𝑇𝑆
(𝑅 𝑛 − 1) ……………………………………………………………… (7.32)
𝑛−1 𝑀𝑊
Polytropic head=36.8
Power
𝐹∗𝑃𝑜𝑙𝑦𝑡𝑟𝑜𝑝𝑖𝑐 ℎ𝑒𝑎𝑑
…………………………………………………………………… (7.33)
3600∗𝑉𝐸%
F=flow rate, kg/hr
Power=1821.42 KW
Power in Hysys=1850.5 KW
Error=1.60%

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References

[1] Sinnott, R., Coulson, J. and Richardson, J., 2005. Chemical Engineering Design. Oxford:
Elsevier Butterworth-Heinemann.
[2] Edgar, T., 2008. Perry's Chemical Engineers' Handbook. [New York]: McGraw-Hill.

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Chapter 8: Process Simulation

In this chapter, a simulation will be created for the process presented in previous chapters.
The simulation will created in HYSYS v10.
The material and energy balance results from the simulation will be compared to the values
obtained from chapter 3 and 4.
Building the Simulation
+ Figure 8.1 shows the PFD for phenol production process. Antoine was selected as a
thermodynamic model (Guideline HYSYS v10 Manual, Sim. Basis).
The tables below are separated into two major parts:
Part 1: Table 8.1, HYSYS results, phenol production unit.
Part 2: Table 8.2, HYSYS results, overall energy and cooling water requirements.

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Figure 8-1:PFD in hysys for phenol production process

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Part (1):
Table 8-1:Comparison between simulation and hand calculation

Stream no. 1 2

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.00 0.00 0.00 0.00

Temperature(C) 25.00 25.00 27.79 30.00

Pressure (kpa) 101.32 101.32 101.32 101.32

Molar flow (kgmole/h) 200.00 200.00 214.91 216.89

Stream no. 3 4

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.00 0.00 1.00 1.00

Temperature(C) 39.24 56.03 37.00 37.00

Pressure (kpa) 151.98 151.98 151.98 151.98

Molar flow (kgmole/h) 250.07 248.61 4692.68 4692.68

Stream no. 5 6

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.00 0.00 1.00 1.00

Temperature(C) 61.36 59.00 37.00 37.00

Pressure (kpa) 253.31 253.31 151.98 151.98

Molar flow (kgmole/h) 237.04 248.60 4506.29 4493.13

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Stream no. 7 8

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.27 0.27 0.00 0.00

Temperature(C) 95.39 100.00 76.00 70.50

Pressure (kpa) 101.32 101.32 101.32 101.32

Molar flow (kgmole/h) 435.58 455.00 180.00 190.00

Stream no. 9 10

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.00 0.00 0.00 0.00

Temperature(C) 175.50 176.00 108.08 110.00

Pressure (kpa) 101.32 101.32 101.32 101.32

Molar flow (kgmole/h) 241.29 245.84 35.15 31.71

Stream no. 11 12

HYSYS EXCEL HYSYS EXCEL

Vapor fraction 0.00 0.00 0.00 0.00

Temperature(C) 180.77 180.00 168.00 168.00

Pressure (kpa) 101.32 101.32 101.32 101.32

Molar flow (kgmole/h) 206.10 211.00 16.89 16.89

13 14
Stream no.
HYSYS EXCEL HYSYS EXCEL
Vapor fraction 0.00 0.00 0.00 0.00
Temperature(C) 181.94 181.00 181.58 181.00
Pressure (kpa) 101.32 101.32 101.32 101.32
Molar flow (kgmole/h) 189.24 193.00 181.00 184.87

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Stream no. 15 16 17
HYSYS EXCEL HYSYS EXCEL HYSYS EXCEL
Vapor fraction 0.00 0.00 1.00 1.00 0.00 0.00
Temperature(C) 191.5 199.00 25.00 25.00 65.00 65.00
Pressure (kpa) 101.32 101.32 101.32 101.32 101.32 101.32
Molar flow (kgmole/h) 8.24 12.00 58.00 58.53 14.91 16.00

Part (2):
Table 8-2: Comparison between simulation and hand calculation

Equipment HYSYS EXCEL

Pumps Actual work (kw)
P-101 7.24E-01 0.72
P-102 1.38 1.38
Compressors Actual work (kw)
C-101 1850.53 1821.42
Reactors Actual work (kw)
R-101 -6845.65 -6590.16
R-102 -12923.99 -13164.27
R-103 -504.20 -480.90
Distillations Actual work (kw)
Qc Qr Qc Qr
T-101
3458.00 3428.00 4028.39 4976.80
Qc Qr Qc Qr
T-102
7261.00 7126.00 6390.22 6.90E+03

T-103 Qc Qr Qc Qr
7583.00 7575.00 9511.95 9.57E+03
Qc Qr Qc Qr
T-104
923300.00 923100.00 1223563.00 1.22E+06

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Boilers Steam flow (kg/s)

E-102 311.92 108.90
E-104 2915.98 2119.05
Coolers Cooling water flow (kg/s)
E-101 8556.25 4692.69

Comments
 The differences between the values obtained from the hand calculation and the ones
obtained from Hysys can be explained in the following points.
 The binary interaction parameters between hydrocarbons are assumed zero in the Excel
model, Hysys doesn’t make this assumption.
 The characterization of C7+. In the Excel model the heat capacity of n-decane was used in
the enthalpy calculations. Hysys uses “Cavett”.
 The calculation Level. The number of trials performed in the Excel model are relatively
small compared to Hysys (Especially the in the throttling valves when calculating the exit
temperature).
 The ideal gas law was used in the calculation of the compressors exit temperature, Hysys
uses a rigorous constant entropy flash instead.
 For the enthalpy calculations, the reference enthalpy is the heat of formation in HYSYS,
in the hand calculations 298 k was taken as reference temperature which leads to zero
values, so comparison is not possible.

Equipment Work
The difference in the compressors work, is a result of differences in
 Molar flow rates.
 Composition.
The difference in the reactors work, is a result of differences in
 Molar flow rates.
 Composition.
 Heat enthalpies
The difference in the distillations work, is a result of differences in
 Molar flow rates.
 Composition.
 Heat enthalpies
The differences in the cooling water requirements
 The temperature differences.
 Molar flow rates.

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Chapter 9: Process Control

Introduction
Process controls is a mixture between the statistics and engineering discipline that deals with
the mechanism, architectures, and algorithms for controlling a process. (1)
The role of process control has changed throughout the years and is continuously shaped by
technology. The traditional role of process control in industrial operations was to contribute to
safety, minimized environmental impact, and optimize processes by maintaining process variable
near the desired values .Generally, anything that requires continuous monitoring of an operation
involve the role of a process engineer.(1)

Importance and objectives of control

1. Maintain the process at the operational conditions and set points.
2. Transition the process from one operational condition to another. (1)
Process control terms
As in any field, process control has its own set of common terms that you should be familiar
with and that you will use when talking about control technology.

Control loop
In the control loop, if a variable fall below the set point, an action should be taken to bring
the process back to the desired conditions. The control loop will remain static until other
disturbance occurs.
The control loop consists of:
1. Measuring device (thermocouple, flow meter).
2. Controller (feedback or feed forward).
3. Regulating element (valve).
4. Set variable (a value entered to the controller to compare it with the measured value).

Controlled process variables

1. Temperature.
2. Pressure.
3. Flowrate.
4. Level.
5. Density.
6. PH of fluid.

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Input Variable
This variable shows the effect of the surroundings on the process. It normally refers to those
factors that influence the process.
These are broken down into two types of inputs.
a. Manipulated inputs: variable in the surroundings can be control by an operator or the control
system in place.
b. Disturbances: inputs that can not be controlled by an operator or control system. There exist
both measurable and immeasurable disturbances. (1)
Output variable
Also known as the control variable .These are the variables that are process outputs that effect the
surroundings.

• Cascade: A control system with 2 or more controllers, a "Master" and "Slave" loop. The output
of the "Master" controller is the set point for the "Slave" controller.
• Dead Time: The amount of time it takes for a process to start changing after a disturbance in the
system.
• Derivative Control: The "D" part of a PID controller. With derivative action the controller
output is proportional to the rate of change of the process variable or error.*
• Error: In process controls, error is defined as: Error = set point - process variable.
• Integral Control: The "I" part of a PID controller. With integral action the controller output is
proportional to the amount and duration of the error signal.
• PID Controller: PID controllers are designed to eliminate the need for continuous operator
attention. They are used to automatically adjust system variables to hold a process variable at a set
point. Error is defined above as the difference between set point and process variable.
• Proportional Control: The "P" part of a PID controller. With proportional action the controller
output is proportional to the amount of the error signal.
• Set point: The set point is where you would like a controlled process variable to be. (1)

Table 9-1:Types of controllers suitable for the common variables.

Variable Controller
Flow and liquid pressure PI
Gas pressure P
Liquid level P or PI
Temperature PID
Composition P,PI,PID

Types of Instrument
Various types of instruments are available for control purposes, those are usually designated
by symbols in the process piping and instrumentation diagram (P&ID), Table (9-2) demonstrate
the standard letter codes used to represent used instruments.

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Table 9-2:Symbols used in P&IDs.

Letter 1st position 2nd and/or 3rd position

T Temperature Transmitter
P Pressure -
L Level -
E - Element
F Flow -
I Current Indicator
C Concentration Controller
A Analysis Alarm
R Radiation Recorder

Line and function symbols

Different types of lines are used in process flow diagrams, piping and instrumentation
diagrams, and loop diagrams to indicate the type of connection between field devices and the
control system. As illustrated in Figure (9-1), a solid line is used to represent a physical connection
to the process, two slashes shown as points along a line are used to indicate a pneumatic signal,
Dashed line is used to indicate an electric signal.

Figure 9-1:Different types of lines

Types of Controllers' Actions

Continuous controlling is obtained using controllers operating by one of three basic
controlling actions, proportional, integral, derivative, or any combination of them. Each of the
three actions or combinations has significant characteristics and the selection of controller type
depends on the effect required. Characteristics of controller types and listed in Table (9-3).

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Table 9-3:Basic features of control actions.

Controller Characteristics
P Simple, long recovery time, unstable at high sensitivity gain.
I Eliminates offset completely, automatic re-set, reduces system stability.
D Early anticipation of proportional action, short recovery time after
disturbance, provides stability to system, reduces time lag, not suitable
for sharp changes.
PI Eliminates off-set, provides an un-stable system.
PD Has the properties of P-action with the D-action providing the early
anticipation of proportional action.
PID Combines all actions, eliminates off-set, short recovery time.

Process equipment control

Heaters control E (102)
Objective

Its purpose is to heat the oxidation stream before it enters the cleavage reactor to 61 ℃.

Procedure

The outlet stream temperature is measured using the thermocouple then the transmitter
sends the measured value to the controller, the controller compares the measured value to the set
point. If the temperature is increased above 61 ℃ decrease the steam flowrate, else if the
temperature is decreased below 120 ℃ increase the steam flowrate.

Table 9-4:Elements of control loop for heater temperature.

Process Heater
Controller Automatic (PID)
Controlled variable Outlet stream temperature
Measuring Element Thermocouple
Regulating element Valve (pneumatic)
Manipulated Element Steam flowrate
Load variables Leakage, ambient & feed temperature
Set point For E-(102), T =61 ℃.

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Figure 9-2:Heater temperature control loop.

E (105)
Objective

Its purpose is to heat the cleavage stream before it enters the acetone column to 120 ℃.

Procedure

The outlet stream temperature is measured using the thermocouple then the transmitter
sends the measured value to the controller, the controller compares the measured value to the set
point. If the temperature is increased above 120 ℃ decrease the steam flowrate, else if the
temperature is decreased below 120 ℃ increase the steam flowrate.

Table 9-5: Elements of control loop for heater temperature.

Process Heater
Controller Automatic (PID)
Controlled variable Outlet stream temperature
Measuring Element Thermocouple
Regulating element Valve (pneumatic)
Manipulated Element Steam flowrate
Load variables Leakage, ambient & feed temperature
Set point For E-(105), T =120 ℃.

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Figure 9-3:Heater temperature control loop.

Coolers control E (102)

Objective
Its purpose is to cool the air stream before it enters the cleavage reactor to 37 ℃.
Procedure
Hot stream is being monitored using a thermocouple then the transmitter sends the measured
value to the controller, the controller compares the measured value to the set point. If the
temperature is increased above the set point, increase the cooling water flowrate. Else if the
temperature decreased below the set point decrease the cooling water flowrate.
Table 9-6:Elements of control loop for cooler temperature.
Process Cooling
Controller Automatic (PID)
Controlled variable Outlet stream temperature
Measuring Element Thermocouple
Regulating element Valve (pneumatic)
Manipulated Element Cooling water flowrate
Load variables Ambient temperature, leakage, feed temperature
Set point For E-(101), T = 37 ℃

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Figure 9-4:cooler temperature control loop.

Control of heat exchangers E (101)

Objective
The heat exchanger is used to exchange heat between the air stream and the oxidation
effluent.
Procedure
The temperature controller could use a signal valve to allow more or less of the heating or
cooling media to bypass the exchanger according to the set point.
E (104)
Objective
The heat exchanger is used to exchange heat between the cleavage effluent and the AMS
column distillate.
Procedure
The temperature controller could use a signal valve to allow more or less of the heating or
cooling media to bypass the exchanger according to the set point.

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Table 9-7: Elements of control loop for heat exchangers temperature.

Process Heat exchanging
Controller Automatic (PID)
Controlled variable Outlet stream temperature
Measuring Element Thermocouple
Regulating element Valve (pneumatic)
Manipulated Element Heating or cooling utility flowrate
Load variables Ambient temperature, inlet temperature
Set point According to heating media:
For E-(104), T =152.5 ℃
For E-(101), T =66.37 ℃
According to cooling media:
For E-(104), T =55℃
For E-(101), T =51.85 ℃

Figure 9-5:Heat exchangers temperature control loop.

Control of reactors R (101), R (102), R (103)

The reactor is the heart of most chemical production facilities. Other operations such as
heat transfer, separation, and purification are all dependent on the reactor’s production or demands
for services.

Most reactors have fixed feed rate, as determined by market demand and constraints. All
other operations are then dependent on the reactor’s production rate. Therefore, it is essential that
the reactor operation be stable. If the reactor is run efficiently, with steady product of uniform

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quality, all other operations may proceed smoothly and the plant should be profitable. But if a
critical parameter is offset, product quality will suffer and all downstream plant operations will be
upset.

Temperature control
Objective
The two reactions are exothermic, and hence, it must fulfill certain conditions of reactants to
obtain the required conversion. If the required heat of reaction is not provided in the required
amount, the progress of reaction will be affected.
Procedure
It’s found that if the temperature must be kept at 120 ℃ to get the maximum conversion
yield in the first reactor , 55 ℃ in the second and 65℃ in the third. The temperature of the inlet
stream to R (101) , R (102) and R (103) is measured using a thermocouple to indicate deviation,
the measured temperature is then sent to a controller by a transmitter, the controller then compares
the measured value with the set value, if the temperature measured is lower than 37 , 55 and 65
℃ for the fisrt , second and third reactors respectively, then the flowrate of steam is increased, and
if it is higher, the steam flowrate is decreased by adjusting the steam inlet valve.
The sensitivity analysis shows the exothermic reaction is sensitive to change in temperature,
but can withstand some variation without crucial impact on conversion, and hence an automatic
(PID) controller is used. The use of the derivative action is necessary for exothermic reactions
since temperature changes affect the stability of reactor easily.
Table 9-8:Elements of control loop for reactor temperature.

Process Reactor
Controller Automatic (PID)
Controlled variable Outlet stream temperature
Measuring Element Thermocouple
Regulating element Valve (pneumatic)
Manipulated Element Steam flowrate
Load variables Feed Temperature
Set point For R-(100), T = 37 ℃
For R-(101), T = 55 ℃
For R-(102), T = 65 ℃

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(a) (b),(c)

Figure 9-6:reactors temperature control loop,(a)oxidation tower,(b)cleavage

reactor,(c)hydrogenation reactor .

Pressure control

Objective
The reactors are designed to withstand certain pressure, if the pressure rises due to
unexpected expansion of gases in the reaction media, then the pressure must be relived to prevent
any hazard of explosion and maintain plant safety. In addition to safety considerations, the pressure
of reactants play a crucial role in obtaining the required conversion, thus the pressure must not
deviate from its set value of 1.5 , 2.5 and 1 atm at inlet stream for the R (101) , R (102) and R (103)
respectively.
Table 9-9: Elements of control loop for reactor pressure.

Process Reactor
Controller Automatic (PID)
Controlled variable Reactor pressure
Measuring Element Electric transducer
Regulating element Relief valve
Manipulated Element Reactor pressure
Load variables Reactor temperature
Set point For (R-100), P = 1.5 atm
For (R-101), P = 2.5 atm
For (R-102), P = 1 atm

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(a) (b),(c)
Figure 9-7:Reactors pressure control loop,(a)oxidation tower,(b)cleavage
reactor,(c)hydrogenation reactor .

Control of distillation columns T (101), T (102), T (103), T (104)

All distillation columns have to be carefully operated in order to achieve the required
production rates and product quality. The three main objectives of column control can be stated
as:
1. Set stable conditions for the column operation.
2. Regulate conditions in the column so that the product always meets the required
specifications.
3. Achieve the above objectives most efficiently, by maximizing product yield and
minimizing energy consumption.
Pressure control
Objective
Pressure is often considered the prime distillation control variable, as it affects temperature,
condensation, vaporization, compositions, volatilities and almost any process that takes place
inside the column. For columns operating below atmosphere the separation process is highly
sensitive to pressure disturbance.

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Procedure
The manometer measures the pressure of the drum and the transmitter sends the measured
value to the controller to compare it to the set point. If the pressure is below set point a control
valve regulates the amount of bleed air used to maintain the pressure on the reflux accumulator. If
the pressure is below set point the controlled rate of air or gas is bled into the vacuum line just
ahead of the ejector thus increasing the pressure and if it’s higher the valve is closed and pressure
is decreased. Using the pressure of the accumulator for control involves fewer time lags than if the
column pressure were used as the control variable.

Table 9-10:Elements of control loop for distillations pressure.

Process Distillation column

Controller Automatic (PI)
Controlled variable Pressure of the drum
Measuring Element Manometer
Regulating element Valve (pneumatic)
Manipulated Element Rate of air bled to vacuum line
Load variables Feed flowrate or feed temperature
Set point For T-(101), P = 1 atm
For T-(102), P = 1 atm
For T-(103), P = 1 atm
For T-(104), P = 1 atm

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Figure 9-8:Distillation column pressure control loop.

Temperature control
Objective
Column temperature control is perhaps the most popular way of controlling product
compositions. In this case, the temperature is required to provide good response to column
disturbances, and to protect the column from disturbances occurring in the heating medium. The
re-boiler boil-up is regulated to achieve desired product purity and to maintain a constant boil-up
rate.

Procedure
The thermocouple measures the temperature and the transmitter transfers the measured value
to the controller to compare it with the set point that was sent from the analyzer. If the temperature
is below the set point, the valve is opened to increase the steam flowrate into the re-boiler; this has
the effect of increasing the heat transfer rate and thus increasing the temperature and preventing
off product composition.
The fast temperature controller action renders this control method less sensitive to upsets
and step changes in an analyzer-only control system. Another advantage is that analytical control
is a way to sidestep the problems of temperature control. Although additional investment is needed
for the analytical equipment, savings in operating cost usually results.

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Table 9-11:Elements of control loop for distillations temperature.

Process Distillation column

Controller On-line analyzer controller together
with temperature controller (both
PID), Feedback control.
Controlled variable Composition of bottom feed
Measuring Element Thermocouple
Regulating element Valve
Manipulated Element steam flowrate
Load variables Feed flowrate or feed temperature,
change in the ratio of gas to liquid
Set point For T-(101), 𝑥𝐵 = 0.789
For T-(102), 𝑥𝐵 = 0.906
For T-(103), 𝑥𝐵 = 0.974
For T-(104), 𝑥𝐵 = 0.621

Figure 9-9:Distillation column temperature control loop.

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Level control : Drum level control

Objective
Drum level control is critical to ensure that the proper amount of reflux will return to the
distillation tower. Poor liquid level can cause expensive operating problems and product
degradation.
Procedure
The level transmitter sends the measured height of liquid in the drum to the level controller.
The level controller compares the measured level with the set point level and sends a pressure
signal to the valve. The valve stem moves up and down, changing the distillate flowrate through
the valve.
Table 9-12:Elements of control loop for distillations drum level.

Process Distillation column

Controller Automatic (PID)
Controlled variable Drum level
Measuring Element Orifice
Regulating element Valve
Manipulated Element Distillate flowrate
Load variables Feed flowrate or feed temperature,
change in the ratio of gas to liquid,
valve characteristics
Set point 85% of the holdup volume

Figure 9-10:Distillation column drum level control loop.

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Column base level control

Objective
Level measurement at the bottom of a distillation tower controls the bottoms product rate.
Poor level control could allow liquid to back up over the stripping trays causing damage and
reduced yield and may cause pump cavitation. Another reason is to keep a liquid level in the bottom
of the column, to prevent running the re-boiler dry.
Procedure
The level transmitter sends the measured height of liquid in the column bottom to the level
controller. The level controller compares the measured level with the set point level and sends a
pressure signal to the valve. The valve stem moves up and down, changing the bottom flowrate
through the valve.
Table 9-13: Elements of control loop for distillations base level.

Process Distillation column

Controller Automatic (PID)
Controlled variable Liquid level
Measuring Element Orifice
Regulating element Valve
Manipulated Element Bottom flowrate
Load variables Feed flowrate or feed temperature,
change in the ratio of gas to liquid,
valve characteristics
Set point A set point that maintain a fairly tight
range to prevent flooding the bottom
tray and to maintain sufficient pump
suction head for the bottoms pump out

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Figure 9-11:Distillation column base level control loop.

Figure 9-12:Distillation column control loop.

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Figure 9-13:PID.

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References

[1] 2007. Chemical Process Dynamics And Controls. University of Michigan.

[2] Elamin Abou-Goukh, D., n.d. Process Dynamics And Control.

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Chapter 10: Safety, Health and Environment

Safety
Hazard Introduction
The term hazardous properties may be broadly classified into two principal categories namely
toxicity and flammability and explosively.

The term toxicity refers to substances that produce poisoning or adverse health effects upon
acute or chronic exposure. It includes mutagenicity and carcinogenic potential, teratogenicity and
corrosively or irritant actions.

Animal data on the median lethal dose (LD50) by various routes of administration is good
indicator of the degree of toxicity of a substance. Substances that exhibit acute oral LD50 values of
<100 mg/kg in rats or mice are termed highly toxic compounds. Those that have LD50 values of
100–500 mg/kg and >500 mg/kg are termed moderate and low toxicants, respectively.

The flammable properties of substances in air include their flash point, vapor pressure, auto
ignition temperatures, and flammability range. Liquids that have a flash point of <100°F (37.8°C)
are termed flammable, whereas liquids that have a flash point of 100– 200°F (37.8–93.3°C) are
termed combustible. A violent reaction that produces flame can cause an explosion under more
severe conditions.

Hazardous substances can be disposed of in an approved landfill disposal site, although such
disposal of highly toxic compounds can lead to groundwater contamination. Incineration in a
chemical incinerator equipped with an afterburner and scrubber is a widely used practice for the
destruction of toxic wastes. Biodegradation of toxic compounds to nontoxic products in soils,
waters, treatment plants, and bioreactors has become treatment for toxic waste in recent years.
Other processes that are used include treatment with molten metals, wet oxidation, ultraviolet (UV)
light-catalyzed oxidation using hydrogen peroxide or ozone, and De chlorination or
desulfurization.

Handling and Storage of Hazardous Chemical:

Cumene:

Cumene is highly flammable in presence of heat, sparks or flames. Vapors may form explosive mixture
with air.

Since Cumene is highly toxic, irritant and corrosive, eyewash stations and safety showers are
ensure proximal to the work-station location. Personal protection such as vapor respirator, face
shield, gloves and boots is put on when handling the chemical.

For safe storage store in area without drain or sewer access, separated from strong oxidants and
acids, cool and keep in the dark.

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Cumene Peroxide

Cumene Peroxide is a strong oxidizing agent. Cumene Peroxide is flammable, corrosive,

irritant, health and environmental hazardous.

For safe storage, store in a well-ventilated place. Keep container tightly closed. Store at
temperatures not exceeding 60 °C / 140 °F. Store away from other materials.

Phenol

Phenol is corrosive, acute toxic and health hazard. Combustible material may burn but doesn’t
ignite readily.

For safe storage store in a cool, dry, ventilated area and away from sources of heat or ignition.

α – methylstyrene

α – methylstyrene is flammable, irritant and environmental hazard.

For safe storage avoid contact with heat, sparks flame or other ignition sources.

Dimethyl benzyl Alcohol (DMBA)

DMBA is irritant, acute toxic and health hazard.

For safe storage DMBA should be handled in containment and done over absorbent pads. The
fume hood or other approved containment must be cleaned upon completion of tasks. When
transporting DMBA, the vials should be placed in secondary, sealed, plastic, labeled, non-
breakable containers.

Acetophenon

Acetophenon is irritant and toxic.

For safe storage keep container tightly closed in a dry and well-ventilated place and separated
from strong oxidants.

Acetone

Acetone is an irritant, volatile, flammable organic solvent.

For safe storage keep in closed containers, and keep away from heat, sparks, and flames.

Oxygen

Oxygen is Strong oxidizer

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For safe storage keep fireproof, separated from combustible substances and reducing agents
and cool.

Nitrogen

Nitrogen is compressed gas, may explode if heated.

For safe storage keep container tightly closed in a dry and well-ventilated place. Containers
which are opened must be carefully resealed and kept upright to prevent leakage.

Hydrogen

Hydrogen is extremely flammable gas.

For safe storage keep in a cool, dry, well-ventilated location. Outside or detached storage is
preferred. Isolate from oxygen, halogens and other oxidizing materials.

Methanol

Methanol is highly flammable liquid, acute toxic and health hazard.

For safe storage keep container tightly closed in a dry and well-ventilated place. Containers
which are opened must be carefully resealed and kept upright to prevent leakage.

Hazard and Operability Studies (HAZOP)

An important element of any system for the prevention of major accidents is conducting a
hazard and operability study (HAZOP) at the detail design stage, of the plant in general and the
operating and safety control systems in particular. HAZOP’s seek to minimize the effect of an
atypical situation in the operation/process by ensuring that control and other safety systems such
as functional safety (e.g. emergency safe shutdown) are in place and work with a high level of
reliability to achieve a safe outcome from a situation that could have resulted in a major accident.

The HAZOP process is used to identify potential hazards and operational problems in terms
of plant design and human error. The technique is applied during final design of the process and
plant items before commencement of construction.

HAZOP’s have also proven to provide financial benefits to the plant owner/operator by
minimizing the time and money spent in installing add on control and safety systems, the need for
which may become evident at the time of plant commissioning in the absence of a HAZOP. On
the operability front benefits are gained by implementing at design stage, the remedial
recommendations to operability issues identified during the HAZOP.

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Procedure

HAZOP studies are normally carried out by a team of experienced people, who have
complementary skills and knowledge; led by a team leader who is experienced in the technique.
The team examines the process vessel by vessel, and line by line, using the guide words to detect
any hazards, a list of guide words are illustrated in table 7.1. The information required for the study
will depend on the extent of the investigation. A preliminary study can be made from a description
of the process and the process flow sheets. For a detailed, final, study of the design, the flow-
sheets, piping and instrument diagrams, equipment specifications and layout drawings would be
needed. Possible causes of the possible events are derived and consequences effect of such events
is discussed and required recommendation and follow-up sheet is generated for implementation
purpose.

Table 10-1:A List of Guide Words and Their Meaning

Guide word
Meaning Comments
No or NOT
The complete negation of No part of the intentions is achieved but nothing
these intention else happens
MORE Quantitative increases These refer to quantities and properties such as
flow rates and temperatures, as well as activities
like “HEAT” and “REACT”.
LESS A quantitative decrease Same as MORE comments
AS WELL A quantitative increase All the design and operating intentions are
AS achieved together with some additional activity
PART OF A quantitative decrease Only some of the intentions are achieved; some
are not.
REVERSE The logical opposite of the This is mostly applicable to activities, for
intention example reverse flow or chemical reaction. It
can also be applied to substances, e.g. “PO SO
instead of “A T DOTE” or “D” instead of “L ”
optical isomers.
OTHER Complete substitution No part of the original intention is achieved.
THANA Something quite different happens

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Table 10-2: Compressor HAZOP

Guide word Deviation Possible cause Consequence Action required

Less Air flow rate Supply valve Compressor Consider low
closed cavities alarm level
Possible fire due shutdown on
to overheating Compressor
More Air Flow rate Supply valve Upset in reactor Consider high
Thermal stress alarm level
on compressor shutdown on
compressor
Temperature Less air flow rate Possible fire Same as less

As well As Composition Impurity in air Upset in reactor Study possible

impurities

Table 10-3: Reactor HAZOP

Guide word Deviation Possible cause Consequence Action required

Less Feed flow rate Valve closed or Reduce product Consider low
line rupture yield and quality flow alarm
Consider bypass
Steam flow rate Rupture in steam Coke deposition on
line catalyst(damage to Consider low
catalyst flow alarm
Pressure High pressure Reduces product
drop due to yield and quality Consider high
increase in flow level alarm
velocity
Flow rate Valve opened 1. Reduce product
quality. 2. if
More significantly high
solid catalyst Consider high
entraining may level alarm
occur.
Rupture in valve Possible fire if
or line composition more
than flammability
limit
Temperature Compressed air 1. reduce product
more than required quality and yield by Consider low
promoting side level alarm for
reaction air and coolant
Coolant flow rate Damage to catalyst flow
less than required
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Pressure Reactor feed

pressure more than Same as more Install relief
required temperature valve
closed relief valve
if present

Table 10-4: Cooler HAZOP

Guide word Deviation Possible cause Consequence Action required

Less Feed flow rate Supply valve output cooled
closed more than
required may Consider low
alter flash flow alarm in
separation feed line and
More Feed flow rate Supply valve Output not cooler utility
open cooled as
required may
alter flash
separation
Temperature Feed is hotter Same as more Consider high
than required flow rate flow alarm for
cooler utility
As well as Output Utility leak or Contamination of consider periodic
composition tube corrosion product checking &
Possible reaction maintenance on
May alter cooler
consequence
processes

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Table 10-5: Distillation HAZOP

Guide word Deviation Possible cause Consequence Action required

Less Feed flow rate Supply valve Overheating in re Consider low
closed boiler level alarm
shutdown
Temperature Less vapor from Alter separation Consider low
re boiler more process quality level alarm in re
cooled reflux boiler utility and
from condenser high level alarm
cool feed in condenser
utility
Pressure Less vapor from Alter separation consider low
re boiler Relief process quality level alarm in re
valve open boiler
More Feed flow rate Supply valve Damage to trays Consider high
open if significantly level alarm
high shutdown
Alter separation
process quality
Temperature More vapor from Acrylic acid may
re boiler polymerize if
o
more than 90 C
Alter separation
process quality
Pressure More vapor from Alter separation
re boiler Relief process quality
valve closed
As well as product Impurities due to Alter separation Consider
Composition utility leak in process quality checking
condenser or re possible reaction condensers and
boiler Rupture in re boilers
distillation periodically
vessel

Health
Effect to Human
Cumene

Cumene is a skin and eye irritant. Acute (short-term) inhalation exposure to Cumene may cause
headaches, dizziness, drowsiness, slight incoordination, and unconsciousness in humans. Cumene
has a potent central nervous system (CNS) depressant action characterized by a slow induction
period and long duration of narcotic effects in animals.

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Cumene Peroxide

Inhalation of vapor causes headache and burning throat. Liquid causes severe irritation of eyes;
on skin, causes burning, throbbing sensation, irritation, and blisters. Ingestion causes irritation of
mouth and stomach.

Phenol

Phenol is highly irritating to the skin, eyes, and mucous membranes in humans after acute
(short-term) inhalation or dermal exposures. Phenol is considered to be quite toxic to humans via
oral exposure. Anorexia, progressive weight loss, diarrhea, vertigo, salivation, a dark coloration
of the urine, and blood and liver effects have been reported in chronically (long-term) exposed
humans. Animal studies have reported reduced fetal body weights, growth retardation, and
abnormal development in the offspring of animals exposed to phenol by the oral route.

α – methylstyrene

Generally, alpha-methyl styrene is an irritant to the eyes, skin, & upper respiratory tract.
Inhalation causes irritation of respiratory tract, headache, dizziness, light-headedness, and
breathlessness. Ingestion causes irritation of mouth and stomach. Contact with liquid irritates eyes.
Prolonged skin contact can cause severe rashes, swelling, and blistering.

Dimethyl benzyl Alcohol (DMBA)

DMBA is a highly potent carcinogen, neoplastigen (contributes an abnormal proliferation of

cells), tumorigenic and teratogen (causes developmental malformations), that causes cancer and
heritable genetic damage and is used to induce cancer in animal models. DMBA may absorbed
through skin, may cause reproductive damage. Contact can irritate and burn the skin, eyes, nose,
throat and lungs. DMBA may damage the liver and kidneys.

Acetophenon

Acetophenon is an Irritant to Eyes, Nose, Throat and Skin (Moderate). Also can cause
Nervous System Disturbances (Narcosis)

Acetone

Acetophenon is an Irritant to Eyes, Nose, Throat and Skin (Mild)

Oxygen

Inhalation of 100% oxygen can cause nausea, dizziness, irritation of lungs, pulmonary edema,
pneumonia, and collapse. Liquid may cause frostbite of eyes and skin.

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Nitrogen

Inhalation can cause asphyxiation, if atmosphere does not contain oxygen; dizziness,
unconsciousness, or even death can result. Contact of liquid with skin or eyes causes frostbite
burns.

Hydrogen

Vapors may cause dizziness or asphyxiation without warning. Some may be irritating if inhaled
at high concentrations. Contact with gas or liquefied gas may cause burns, severe injury and/or
frostbite. Fire may produce irritating and/or toxic gases.

Methanol

Exposure to excessive vapor causes eye irritation, head- ache, fatigue and drowsiness. High
concentrations can produce central nervous system depression and optic nerve damage. 50,000
ppm will probably cause death in 1 to 2 hrs. Swallowing may cause death or eye damage

Effect to Environment
Cumene

Cumene evaporates when exposed to air. In the air it is reacted quickly into other chemicals, in
the water and soil bacteria break it down. It has moderate acute (short-term) toxicity on aquatic
life, and high acute toxicity to birds. Insufficient data are available to predict the toxicity of
Cumene to plants and land animals. It has moderate chronic (long-term) toxicity to aquatic life.
Cumene is expected to minimally bioaccumulate.

Cumene Peroxide

Cumene Peroxide is toxic for microorganisms. It represses the cell growth and degradative
activity of strains able to utilize other phenolic wastewater components has baneful effect on the
microflora of activated sludges and exerts negative influence on the aqueous microbocenoses.

Phenol

Acute toxic effects may include the death of animals, birds, or fish, and death or low growth
rate in plants. Longer term effects may include shortened lifespan, reproductive problems, lower
fertility, and changes in appearance or behavior.

α – methylstyrene

AMS is moderately toxic to aquatic organisms (e.g., fish, invertebrates and algae). AMS is
considered as not readily biodegradable and it has moderate bioaccumulation potential. The
predicted environmental concentration is lower than the predicted no effect concentration;
therefore, AMS is currently considered to have low potential risk to the environment.

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Dimethyl benzyl Alcohol (DMBA)

The preparation of DMBA including reconstitution, weighing, and diluting should be

performed in a fume hood or biological safety cabinet (class II Type B). Work should be done over
absorbent pads.

Acetophenon

No significant effects have been found. It is expected to have very high to moderate mobility
in soil.

Acetone

Acetone has a slight toxicity when exposed to aquatic life. Acetone has caused membrane
damage, a decrease in size and decrease in germination of various agricultural and ornamental
plants. The effects on birds or land animals have not been fully determined. Acetone is not
expected to bioaccumulate in plants, animals or humans.

Oxygen

Highly concentrated sources of oxygen promote rapid combustion and therefore are fire and
explosion hazards in the presence of fuels.

Nitrogen

Excess nitrogen in the atmosphere can produce pollutants such as ammonia and ozone, which
can impair our ability to breathe, limit visibility and alter plant growth. When
excess nitrogen comes back to earth from the atmosphere, it can harm the health of forests, soils
and waterways.

Hydrogen

Its generation leads to the emission of greenhouse gases at the same level as in the combustion
of fossil fuels. On the other hand, hydrogen obtained from renewable energy, such as solar-
hydrogen, is environmentally friendly, because its generation and combustion do not lead to carbon
emission.

Methanol

Methanol may affect animals, birds and fish, leading to their death. Exposure can also cause
low growth rate in plants. Long term methanol exposure can affect the fertility of biota and affect
their appearance or behavior.

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References

[1] Zafarullah K. Cheema, Purification of Phenol, 2013

[2] Pradyot Patnaik, A Comprehensive Guide To The Hazardous Properties Of Chemical

Substances, 2016.

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Chapter 11 : Plant location and layout

Introduction
The geographic location of the final plant must be taken into account when a process is designed
or developed. A suitable site must be found for a new project, and the site and equipment layout
planned. Provision must be made for the ancillary buildings and services needed for plant
operation; and for the environmentally acceptable disposal of effluent. These considerations are
discussed briefly in the following sections.

Plant Location and Site Selection

The location of the plant can have a crucial effect on the profitability of a project and the scope
for future expansion. Many factors must be considered when selecting a suitable site. The principal
factors to consider are:

1) Location, with respect to the marketing area.

2) Raw material supply.
3) Transport facilities.
4) Availability of labor.
5) Availability of utilities: water, fuel, power.
6) Availability of suitable land.
7) Environmental impact and effluent disposal.
8) Local community considerations.
9) Climate.
10) Political and strategic considerations.

A brief discussion of these principal factors will be given in the following sections:

Marketing Area

For materials that are produced in bulk quantities, such as cement, mineral acids, and fertilizers,
where the cost of the product per metric ton is relatively low and the cost of transport is a significant
fraction of the sales price, the plant should be located close to the primary market. This
consideration is much less important for low-volume production and high-priced products, such as
pharmaceuticals.

Raw materials

The availability and price of suitable raw materials will often determine the site location. Plants
producing bulk chemicals are best located close to the source of the major raw material; where this
is also close to the marketing area.

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Transport

The transport of materials and products to and from the plant will be an overriding consideration
in site selection. If practicable, a site should be selected that is close to at least two major forms of
transport: road, rail, waterway (canal or river), or a sea port. Road transport is being increasingly
used, and is suitable for local distribution from a central warehouse. Rail transport will be cheaper
for the long-distance transport of bulk chemicals. Air transport is convenient and efficient for the
movement of personnel and essential equipment and supplies, and the proximity of the site to a
major airport should be considered

Availability of labor
Labor will be needed for construction of the plant and its operation. Skilled construction
workers will usually be brought in from outside the site area, but there should be an adequate pool
of unskilled labor available locally; and labor suitable for training to operate the plant. Skilled
tradesmen will be needed for plant maintenance. Local trade union customs and restrictive
practices will have to be considered when assessing the availability and suitability of the local
labor for recruitment and training.

Utilities (services)

Chemical processes invariably require large quantities of water for cooling and general process
use, and the plant must be located near a source of water of suitable quality. Process water may be
drawn from a river, from wells, or purchased from a local authority. At some sites, the cooling
water required can be taken from a river or lake, or from the sea; at other locations cooling towers
will be needed. Electrical power will be needed at all sites. A competitively priced fuel must be
available on site for steam and power generation. Utilities may include:

 Electricity.
 Steam for process heating.
 Cooling water.
 Water for general use.
 Demineralized water.
 Compressed air.
 Inert gas supplies.
 Refrigeration.
 Effluent disposal facilities.

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Environmental impact and effluent disposal:

All industrial processes produce waste products, and full consideration must be given to the
difficulties and cost of their disposal. The disposal of toxic and harmful effluents will be covered
by local regulations, and the appropriate authorities must be consulted during the initial site survey
to determine the standards that must be met. An environmental impact assessment should be made
for each new project, or major modification or addition to an existing process.

Local community considerations:

The proposed plant must fit in with and be acceptable to the local community. Full consideration
must be given to the safe location of the plant so that it does not impose a significant additional
risk to the community. On a new site, the local community must be able to provide adequate
facilities for the plant personnel: schools, banks, housing, and recreational and cultural facilities.
The local community must also be consulted about plant water consumption and discharge and the
effect of the plant on local traffic.

Availability of suitable land

Sufficient suitable land must be available for the proposed plant and for future expansion. The land
should ideally be flat, well drained and have suitable load-bearing characteristics. A full site
evaluation should be made to determine the need for piling or other special foundations.

Climate

Adverse climatic conditions at a site will increase costs. Abnormally low temperatures will require
the provision of additional insulation and special heating for equipment and pipe runs. Stronger
structures will be needed at locations subject to high winds (cyclone/hurricane areas) or
earthquakes.

Political and strategic considerations:

Capital grants, tax concessions, and other inducements are often given by governments to direct
new investment to preferred locations; such as areas of high unemployment. The availability of
such grants can be the overriding consideration in site selection.

All of the above factors should be considered simultaneously in selecting the optimal plant
location.

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Site Layout
The physical layout of the plant should be designed to print coordination between the operation of
process equipment and the use of storage and material handling equipment. The process units and
ancillary buildings should be laid out to give the most economical flow of materials and personnel
around the site. Hazardous processes must be located at a safe distance from other buildings.
Consideration must also be given to the future expansion of the site. The ancillary buildings and
services required on a site, in addition to the main processing units (buildings), will include:

 Storages for raw materials and products: tank farms and warehouses.
 Maintenance workshops.
 Stores, for maintenance and operating supplies.
 Laboratories for process control.
 Fire stations and other emergency services.
 Utilities: steam boilers, compressed air, power generation, refrigeration, transformer
stations.
 Effluent disposal plant.
 Offices for general administration.
 Canteens and other amenity buildings, such as medical centers.
 Car parks.

When roughing out the preliminary site layout, the process units will normally be sited first and
arranged to give a smooth flow of materials through the various processing steps, from raw
material to final product storage. Process units are normally spaced at least 30 m apart [1]; greater
spacing may be needed for hazardous processes.

The location of the principal ancillary buildings should then be decided. They should be arranged
so as to minimize the time spent by personnel in travelling between buildings. Administration
offices and laboratories, in which a relatively large number of people will be working, should be
located well away from potentially hazardous processes. Control rooms will normally be located
adjacent to the processing units, but with potentially hazardous processes may have to be sited at
a safer distance.

The sitting of the main process units will determine the layout of the plant roads, pipe alleys and
drains. Access roads will be needed to each building for construction, and for operation and
maintenance.

Utility buildings should be sited to give the most economical run of pipes to and from the process
units.

Cooling towers should be sited so that under the prevailing wind the plume of condensate spray
drifts away from the plant area and adjacent properties.

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The main storage areas should be placed between the loading and unloading facilities and the
process units they serve. Storage tanks containing hazardous materials should be sited at least 70
m from the site boundary [1]

Plant Layout
The economic construction and efficient operation of a process unit will depend on how well the
plant and equipment specified on the process flow-sheet is laid out. The principal factors to be
considered are:

Economic considerations: construction and operating costs

The cost of construction can be minimized by adopting a layout that gives the shortest run of
connecting pipe between equipment, and the least amount of structural steel work. However, this
will not necessarily be the best arrangement for operation and maintenance.

Process requirements

An example of the need to take into account process considerations is the need to elevate the base
of columns to provide the necessary net positive suction head to a pump or the operating head for
a thermo reboiler.

Operation

Equipment that needs to have frequent operator attention should be located convenient to the
control room. Valves, sample points, and instruments should be located at convenient positions
and heights. Sufficient working space and headroom must be provided to allow easy access to
equipment.

Maintenance

Heat exchangers need to be sited so that the tube bundles can be easily withdrawn for cleaning and
tube replacement. Vessels that require frequent replacement of catalyst or packing should be
located on the outside of buildings. Equipment that requires dismantling for maintenance, such as
compressors and large pumps, should be placed under cover.

Safety

Blast walls may be needed to isolate potentially hazardous equipment, and confine the effects of
an explosion. At least two escape routes for operators must be provided from each level in process
buildings.

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Plant expansion

Equipment should be located so that it can be conveniently tied in with any future expansion of
the process. Space should be left on pipe alleys for future needs, and service pipes over-sized to
allow for future requirements.

Modular construction

In recent years there has been a move to assemble sections of plant at the plant manufacturer’s
site. These modules will include the equipment, structural steel, piping and instrumentation. The
modules are then transported to the plant site, by road or sea.

The advantages of modular construction are:

 Improved quality control.

 Reduced construction cost
 Less need for skilled labor on site.
 Less need for skilled personnel on overseas sites.
Some of the disadvantages are: [1]

 Higher design costs.

 More structural steel work.
 More flanged connections.
 Possible problems with assembly, on site.

Other services

A plant must be prepared for the convenience of it is employees and general administrative staff.
Rooms are made for recreational activities such as rest room, cafeteria, and change room for
workers. Providing a medical facility is important for safety of employees and to take care of any
sudden emergencies that might be happened. Other important parts needed for plant efficient
operation are administrative offices, laboratories, workshops and stores.

General considerations

Open, structural steelwork, buildings are normally used for process equipment; closed buildings
are only used for process operations that require protection from the weather

The arrangement of the major items of equipment will usually follow the sequence given on the
process flow sheet: with the columns and vessels arranged in rows and the ancillary equipment,
such as heat exchangers and pumps, positioned along the outside.

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Phenol plant layout:

Considering the site selection factors, the proposed plant site are in the industrial area, Khartoum-
North and this is for the following reasons:

 Proximity to markets.
 Proximity Wastewater treatment plant (AL Hagg Yousef).
 Availability of transportation facilities (roads, rail way) for transportation of employees
and products.
 Availability of adequate facilities for the plant personnel such as schools, housing, medical
care, and recreational and cultural facilities, so minimizing labor cost.
 Availability of sufficient suitable land for the proposed plant and for future expansion.

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Figure 11-1:Plant layout

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References

[1] GavinTowler & Ray Sinnott, Chemical Engineering Design Principles, Practice and
Economics of Plant and Process Design, Elsevier, 2008.

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Chapter 12: Cost and Economical Evaluation

Introduction [1]
A capital investment is required for any industrial process, and determination of the necessary
investment is an important part of a plant-design project. The total capital investment consists
of fixed-capital investment for physical equipment and facilities in the plant plus working
capital which must be available to start up the plant and operate it to the point when income is
earned.

An acceptable plant design must present a process that is capable of operating under conditions
which will yield a profit. Capital must be allocated for direct plant expenses, such as those for
raw materials. Besides direct expenses, other indirect expenses must be included such as
administrative salaries.

Thus, in an analysis of costs in industrial processes, capital-investment costs, manufacturing costs,

and general expenses including income taxes must be taken into consideration.

Factors Affecting Investment and Production Costs:

To accomplish costs determination the engineer must have a complete understanding of the many
factors that can affect costs, as example of these factors:

Sources of equipment.
Price Fluctuations.
Company Policies.
Operating Time and Rate of Production.
Governmental Policies.

Thus the engineer must keep up-to-date all factors that can affect investment and production costs.

The specifications of plant

In this chapter, the costing of equipment which has been designed will be estimated and the
feasibility of phenol production will be evaluated by profitability analysis to make sure the project
is economically attractive.

Assumptions of the chapter:

The plant life span is twenty years.

All costs in U.S. Dollar when it equals 145 SDG in August 2020.
The price of raw materials and product is fixed for the whole period of operatio

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Table 12-1:Materials prices.

Material Price $/kg

Cumene 1.496

Catalyst 2.1

Acetone 1

Phenol 1.8

ACP 1.31

Cost estimation
There are a number of different ways of estimating the cost of constructing a chemical plant.
Some require very little information and some require a complete listing of every item. All assume
a normal schedule and normal conditions. A normal schedule implies that the contractor and
engineers will be allowed to operate in the most efficient way. Any attempt to complete the plant
sooner will result in increased investment costs.

Methods used in capital estimation:

There are many methods to estimate the capital cost, but the one is used for estimating capital
cost for biodiesel production plant is bare module cost factors.

Module Costing Technique

The equipment module costing technique is a common technique to estimate the cost of a new
chemical plant. It is generally accepted as the best for making preliminary cost estimates and is
used extensively in this text. This costing technique relates all Raw material and product Price $/kg
costs back to the purchased cost of equipment evaluated for some base conditions. Deviations from
these bases Conditions are handled by using multiplying factors that depend on the following:

The specific equipment type

The specific system pressure
The specific materials of construction.

The bare module cost is the sum of the direct and indirect costs:

CBM=Cp0 *FBM

Where CBM = bare module equipment cost: direct and indirect costs for each unit

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FBM = bare module cost factor: multiplication factor to account for the items in Table 11.2 plus the
specific materials of construction and operating pressure.

Cp0 = purchased cost for base conditions: equipment made of the most common material,
usually carbon steel and operating at near ambient pressures.

Bare Module Cost for Equipment at Base Conditions

The Conditions specified for the base case are

1. Unit fabricated from most common material, usually carbon steel (CS)

2. Unit operated at near-ambient pressure

Cost estimation by Capcost:

Cost estimation is performed using CAPCOST program. CAPCOST is available with the book
“Analysis, synthesis, and design of chemical processes” of Richard Turton and coauthors. It is
based on the module coasting method, written in visual basic, as an Excel spread sheet
(CAPCOST_2017.xls).

The program gives the user an option list of equipments. It is required to enter the specific
information for the equipment; such as the capacity, operating pressure, and materials of
construction. The cost data is adjusted for inflation by entering the current value of the CEPCI.

The below steps are followed [2]:

1. Develop a list of all equipment specifications and utilities requirements. For a reactor, include
both its total volume and its heat transfer surface area. Select the material of construction for each
piece of equipment using Materials Selection.

2. Make a list of the flow rates of all feed streams, product streams, and waste streams. Note that
these must all be above 1-atm pressure. Liquids must be above their freezing points and below
their flash points.

3. Find the latest value of the Chemical Engineering Chemical Plant Index (CEPCI).

4. Find the current costs of industrial quantities of your raw materials, products, electricity, natural
gas, and fuel oil. Note that CAPCOST requires utility costs in $/GJ. Also find the current salary +
benefits for operators.

5. Open CAPCOST in Excel. Note that its macros must be operational. Save often while working,
as there have sometimes been bugs in CAPCOST that can cause problems. Because it may be
necessary to start over, it is also a good idea to rename the file each time you save it.

6. Go to the Equipment Summary page in CAPCOST (far left tab at bottom).

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7. Enter the value of CEPCI found in step 2.

8. Add all of the equipment from step 1. Note that all pressures are in barg or psig, i.e. gauge
pressure. (To convert from bar to barg, subtract 1.013. To convert from atm to psig, subtract 1 and
multiply by 14.7.) If CAPCOST doesn’t have a desired type of equipment, you will have to
estimate its price separately and enter it into CAPCOST as User Defined. Note the definitions. For
its built-in equipment and materials, CAPCOST automatically calculates the purchase price and
the bare module factor corrections for pressure and materials, as in Turton Appendix A. For
materials not included in CAPCOST, use the cost data at Materials Selection to estimate materials
factors.

a. Reactors: If your reactor type is not listed, enter both a vessel with its volume and a heat
exchanger with its heat transfer surface area. That is, each reactor will be listed twice in the list of
equipment.

b. Distillation columns: In addition to the column itself, include a reboiler, condenser, reflux
pump, and reflux accumulator. Make certain you include safety factors. For tray columns, divide
the number of theoretical trays by an efficiency.

c. Pumps: Don’t forget to specify a spare. Drivers (motors) are included with the pump in
CAPCOST, so do not list separate drivers as you will be counting them twice.

d. Heat exchangers: If you split a heat exchanger in order to model it, combine the two areas for
the real heat exchanger.

e. To edit or delete any piece of equipment, save and then click on Edit Equipment. Do not
highlight and delete or change as you would in a usual Excel file.

If your plant will have a large amount of some material that must be purchased initially in order
for the plant to operate, this should be included as a capital expense. Examples would include
catalyst, a liquid extraction agent that circulates, or a heat transfer fluid that circulates. Enter this
in CAPCOST as User Defined equipment, giving your calculated cost as both Purchased
Equipment Cost and Bare Module Cost with the Module Factors =1. On the Utilities Summary
page set its Module and Grass Roots costs to this same value. The amounts of this material lost or
replaced every year (“makeup”) must also be included as raw materials on the COM Summary
page. Suggest 1/10 of the total initial cost.

10. The sum of the bare module costs, i.e. installed equipment costs, is commonly called the Inside
Battery Limit (ISBL) plant cost.

11. Go to the User Options page in CAPCOST. These must be updated, using the information
found in step 4 above.

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a. Put in the correct number of operating hours per year. For a plant operating continuously, this
is NOT 365x24, because the plant must be shut down occasionally for maintenance.

b. Assume that the costs of cooling water, refrigerated water, refrigeration and waste disposal are
proportional to the cost of electricity and update accordingly.

c. Assume that the costs of steam and thermal systems are proportional to the cost of the likely
fuel, natural gas or fuel oil, and update accordingly.

d. Enter the operator salary found in step 4 as the cost of labor.

12. Go to the Utilities Summary page in CAPCOST and make certain all utilities have been
entered. Steam generated in the process is a savings and so should be entered as a negative value
on this page, (To make the cost negative, click on the cell, go to the formula bar, and insert a minus
sign after =).

a. Enter the Raw Material, Product and Waste stream information from steps 1 and 3 above. Also
include the annual replacement (make-up) of costly materials such as catalyst, extraction solvents,
or heat transfer liquids. you can change the contents of any cell. For makeup catalyst, for example,
delete the price and consumption and enter just the estimated annual cost.

b. Enter the Cost of Land and Annual Interest Rate specified by your instructor (or appropriate
for the planned location of the plant). Note that the “Annual Interest Rate” is NOT the interest
charged by banks, but rather the minimum rate of return required by your company for investments
in new facilities (sometimes called the Required Rate of Return).

c. Enter the Taxation Rate appropriate for the location of the plant. In the US, include both state
and federal corporate income taxes.

d. Click on the salvage value shown. This will bring up a menu. For the FCIL (total Fixed Capital
Investment not including the cost of land, i.e. depreciable investment), select Grass Roots if the
plant will be built on a totally new site, or Total Module Cost if it will be added to an existing site
already used for related production operations. This will utilize the appropriate value from the
Utility Summary.

Select the calculate options for everything else, unless you wish to input values manually. Check
the resulting Cost of Operating Labor to make certain it is reasonable (the number of operators per
shift X 3.5 X the annual wages + fringe benefits of an operator).

e. If the Revenue from sale of product(s) comes up negative (with parentheses around it), this is an
error and you must either change the product costs to positive or change the Revenue to positive.
f. Don’t change the Total Module Factor or the Grass Roots Factor unless you have a good reason
to do so.

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g. Enter values for Project Life, Construction Period, and Distribution of Fixed Capital Investment
as directed by your instructor.

h. Make certain that CAPCOST has not reset anything to its initial value.

13. Go to the Cash Flow Analysis page.

a. Click on Generate CFD (Cash Flow Diagram). On the menu, make the selections directed by
your instructor. Recommend Discounted and Five year MACRS depreciation A discounted cash
flow diagram takes into account the required rate of return. The project value (vertical axis) is the
sum of all the discounted cash flows from the beginning of construction. The last project value,
when production is stopped and the plant scrapped, is the Net Present Value (NPV). If this is
positive, presumably the company would want to proceed with a more detailed design. If it is
negative, you’d want to see if your design can be changed to make NPV > 0.

b. The Discounted Cash Flow Rate of Return is the rate of return for which NPV = 0. (If NPV is
negative, you may wish, instead, to determine by trial and- error the minimum required product
selling price, i.e. for NPV = 0. Rather than trial-and error, you can prepare a plot of NPV versus
product selling price.)

c. The Discounted Payback Period is the time at which the FCIL has been recovered, with all cash
flows discounted to the present at the minimum required rate of return (“interest” rate).

d. In the table, dk is the depreciation in year k, FCIL-Sdk is the book value of the fixed capital
investment, and Sdk is the sum of the depreciation for that year and for previous years. Make sure
R, the revenue from sales of product(s), is positive (without parentheses). COMd is the annual cost
of manufacturing from the COM Summary page, the cash flow after subtracting income taxes is
(R-COMd-dk)*(1t)+dk = (R-COMd) - (R-COMd-dk)t (R-COMd is the income before taxes, which
are paid at income tax rate t on this quantity minus the depreciation for that year), the discounted
cash flow is the cash flow divided by (1 + i)n, n is the number of years since the beginning of
construction, and the cumulative discounted cash flow is the sum of all the discounted cash flows
since the beginning of construction.

14. You can easily determine the influence of all parameters on your process economics by
repeating the CFD calculations using other values.

15. CAPCOST’s Monte Carlo Simulation page is set up to help you do this. Select the percent
uncertainties you believe there are in each parameter indicated, and then click on Run Economic
Analysis.

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Table 12-2: List of equipments.

Equipment Bare module cost ($M)

Compressor (C-101) 1.10

Cooler 1 (E-101) 0.14

Heat Exchanger (E-102) 0.04

Boiler 1 (E-103) 0.03

Boiler 2 (E-104) 0.11

Heat Exchanger (E-105) 0.03

Mixer 1 (M-101) 0.13

Mixer 2 (M-102) 0.15

Pump 1 (P-101) 0.03

Pump 2 (P-102) 0.03

Reactor 1 (R-101) 0. 15

Reactor 2 (R-102) 0. 40

Reactor 3 (R-103) 0.60

TIK-101 0.14

TIK-102 0.11

TIK-103 0.11

Distillation column 1 T-(101) 0.25

Distillation column 2 T-(102) 0.40

Distillation column 3 T-(103) 0.42

Distillation column 4 T-(104) 0.44

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Table 12-3: List of utilities costs.

Utility Cost ($/GJ)

Electricity 7.65

Low pressure steam 7.34

Medium pressure steam 7.46

Cooling water 0.38

Cost Estimation by hand calculation (Excel sheet): [2]

Estimation of capital investment cost (showing individual components)

The percentages indicated in the following summary of the various costs constituting the capital
investment are approximations applicable to ordinary chemical processing plants. It should be
realized that the values given can vary depending on many factors, such as plant location, type of
process, complexity of instrumentation, etc.

Total capital investment

A) Fixed-capital investment

I. Direct costs = material and labor involved in actual installation of complete facility (70-85% of
fixed-capital investment)

A. Equipment + installation + instrumentation + piping + electrical + insulation + painting

(50-60% of fixed-capital investment)

1. Purchased equipment (15-40% of fixed-capital investment)

2. Installation, including insulation and painting (25-55% of purchased-equipment cost)

3. Instrumentation and controls, installed (6-30% of purchased-equipment cost)

4. Piping , installed (10-80% of purchased-equipment cost)

5. Electrical, installed (10-40% of purchased-equipment cost)

B. Buildings, process and auxiliary (10-70% of purchased-equipment cost)

C. Service facilities and yard improvements (40-100% of purchased-equipment cost)

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D. Land (I-2% of fixed-capital investment or 4-8% of purchased-equipment cost)

Il. Indirect costs = expenses which are not directly involved with material and labor of actual
installation of complete facility (15-30% of fixed-capital investment)

A. Engineering and supervision (5-30% of direct costs)

B. Construction expense and contractor’s fee (6-30% of direct costs)

C. Contingency (5-15% of fixed-capital investment).

B) Working capital (10-20% of total capital investment)

*Estimation of total product cost (showing individual components)

The percentages indicated in the following summary of the various costs involved in the
complete operation of manufacturing plants are approximations applicable to ordinary chemical
processing plants. It should be realized that the values given can vary depending on many factors,
such as plant location, type of process, and company policies.

Percentages are expressed on an annual basis.

Total product cost:

I. Manufacturing cost = direct production costs + fixed charges + plant overhead costs

A. Direct production costs (about 60% of total product cost)

1. Raw materials (l0-50% of total product cost)

2. Operating labor (10-204 of total product cost)

3. Direct supervisory and clerical labor (l0-25% of operating labor)

4. Utilities (10-20% of total product cost)

5. Maintenance and repairs (2-10% of fixed-capital investment)

6. Operating supplies (l0-20% of cost for maintenance and repairs, or 0.5-1% of fixed capital
investment)

7. Laboratory charges (10-20% of operating labor)

8. Patents and royalties (0-6% of total product cost)

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B. Fixed charges (10-20% of total product cost)

1. Depreciation (depends on life period, salvage value, and method of calculationabout 10% of
fixed-capital investment for machinery and equipment and 2-3% of building value for buildings)

2. Local taxes (1-4% of fixed-capital investment)

3. Insurance (0.4-1% of fixed-capital investment)

4. Rent (8-12% of value of rented land and buildings)

C. Plant-overhead costs (50-70% of cost for operating labor, supervision, and maintenance, or 5-
15% of total product cost); includes costs for the following: general plant upkeep and overhead,
payroll overhead, packaging, medical services, safety and protection, restaurants, recreation,
salvage, laboratories, and storage facilities.

II. General expenses = administrative costs + distribution and selling costs + research and
development costs

A. Administrative costs (about 15% of costs for operating labor, supervision, and maintenance,
or 2-6% of total product cost); includes costs for executive salaries, clerical wages, legal fees,
office supplies, and communications.

B. Distribution and selling costs (2-20% of total product cost); includes costs for sales offices,

Salesmen, shipping, and advertising

C. Research and development costs (2-5% of every sales dollar or about 5% of total product
cost)

D. Financing (interest), (0-l0% of total capital investment)

III. Total product cost= manufacturing cost + general expense

IV. Gross earnings cost (gross earnings = total income - total product cost; amount of gross
earnings cost depends on amount of gross earnings for entire company and income-tax regulations;
a general range for gross-earnings cost is 30-40% of gross earnings)

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Total capital investment:

1. Fixed capital investment:

Table 12-4:Direct cost

Items Percent % Price ,$M

Purchased Equipment Cost 100.00 2.60

Purchased-Equipment Installation 47.00 1.22

Instrumentation and controls
36.00 9.36
(Installed)
Piping 68.00 1.77

Items Percent % Price ,$M

Electrical systems (Installed) 11.00 0.29

Buildings (Installed) 18.00 0.47

Yard improvement 10.00 0.26

Service facilities (Installed) 70.00 1.82

Land 8.00 0.02

Direct Costs = 9.57$M

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Table 12-5:Indirect cost

Items Percent % Price ,$M

Engineering and supervision 33.00 0.86

Construction expenses 41.00 1.07

Legal expenses 4.00 0.01

Contractor’s fee 22.00 0.57

Contingency 44.00 1.14

Indirect costs= 3.74$M

2. Working capital:

Table 12-6:Working capital

Items Percent % Price, $M

Working Capital 15.00 0.39

Total capital investment = 13.7 $M

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Total production cost:

A) Manufacturing cost:

Table 12-7:Manufacturing cost.

Items Percent % Price, $M

1. Direct Production costs - -

Raw materials 45.00 287.27

Operating Labor 15.00 0.42

Direct supervisory and
15.00 0.06
clerical labor
Utility 15.00 0.46

Maintenance and repairs 5.00 0.67

Operating Supplies 5.00 0.07

Laboratory Charge 15.00 0.06

2. Fixed charges - -

Depreciation (TCI-0.1*FCI)/n 0.62

Local taxes 1.50 0.20

Insurance 0.50 0.07

3. Plant overhead costs 4.00 0.46

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B) General expenses:

Table 12-8:General expenses

Items Percent % Price, $M

1.Adminstritive Expenses 25.00 0.29

2. Distribution and marketing expenses 10.00 35.79

3.Research And Development 50.00 17.89

4.Financing Interest 50.00 6.85

Table 12-9:Detailed about direct production cost.

Raw material cost($M) Utility cost($M)

Cumene = 287.23 Steam=0.45

Catalyst = 0.04 Cooling Water = 0.002

Phenol = 250.39 Electricity =0.001

ACP = 13.56

Acetone = 93.94

Project evaluation
As the purpose of investing money in chemical plant is to earn money, some means of
comparing the economic performance of projects is needed .by using hand calculation:

Net present value of the plant

[3]
For interest rate equal to 12% in Sudan :
𝑢𝑠𝑒𝑓𝑢𝑙
𝑛𝑒𝑡 𝑝𝑟𝑜𝑓𝑖𝑙𝑒 𝑓𝑜𝑟 𝑢𝑠𝑒𝑓𝑢𝑙 𝑙𝑖𝑓𝑒
NPV = ∑ − 𝑇𝐶𝐼
𝑛=1 (1+𝑖)𝑛

Where:

An = Net profit per year= 4.373 $M/year

i = Interest rate, n= any year,

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TCI= Total Capital Investment.

For the Phenol plant the NPV= 19.659 $M since the value is positive the project is profitable.

Net profit= 4.373 $M/year

Internal Rate of Return (IRR)

It is the discounting rate that makes the NPV = 0

Then, IRR = 31%

Acceptable project gives IRR > market discounting rate.

Profitability Index:
It is an indicator for the profit gained from each dollar has been spent:

𝑢𝑠𝑒𝑓𝑢𝑙
𝑛𝑒𝑡 𝑝𝑟𝑜𝑓𝑖𝑙𝑒 𝑓𝑜𝑟 𝑢𝑠𝑒𝑓𝑢𝑙 𝑙𝑖𝑓𝑒
∑
𝑛=1 (1+𝑖)𝑛
PI =
𝑻𝑪𝑰

Where PI=1.43 > 1 thus project is acceptable.

Payback period:
It is the period that the project takes to recover the Initial Investment but without regarding the
time value of money and potential risk.

𝐹𝑖𝑥𝑒𝑑 𝐶𝑎𝑝𝑖𝑡𝑎𝑙 𝐼𝑛𝑣𝑒𝑠𝑡𝑚𝑒𝑛𝑡 (𝐹𝐶𝐼)

PPB =
𝑝𝑟𝑜𝑓𝑖𝑡 𝑝𝑒𝑟 𝑦𝑒𝑎𝑟

The fixed capital investment (FCI) = 13.312 $M

The PBP = 3.044 years

Accounting rate of return:

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑎𝑛𝑛𝑢𝑎𝑙 𝑝𝑟𝑜𝑓𝑖𝑡
ARR =
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐼𝑛𝑣𝑒𝑠𝑡𝑚𝑒𝑛𝑡

Annual profit= 4.373 $M,

ARR= 31.91 % > i =12% indicates acceptable project.

242
CHAPTER TWELVE: COST AND ECONOMICAL EVALUATION ||PHENOL

Cost of labor:
According to Turton the operating labor requirement for chemical processing plants is given
by Equation:

NoL= (6.29+3.71 P2+0.23NnP)0.5

where NOL is the number of operators per shift, P is the number of processing steps involving
the handling of particulate solids—for example, transportation and distribution, particulate size
control, and particulate removal. Nnp is the number of non-particulate processing steps and
includes compression, heating and cooling, mixing, and reaction. In general, for the processes
considered in this text, the value of P is tow, and the value of NnP is given by:

NnP = 𝛴 Equipment

It was assumed that an operator worked on average 49 weeks/year and there Were three shifts
a day for a continuously running plant. Operator salary was estimated at $9,000/year .

NnP = 23

Operating labor = 134

Labor cost = 0.415 M$

243
CHAPTER TWELVE: COST AND ECONOMICAL EVALUATION ||PHENOL

Figure 12-1:cash flow diagram.

244
CHAPTER TWELVE: COST AND ECONOMICAL EVALUATION ||PHENOL

References

[1] Max S.Peters & Klaus D.Timmerhaus, Plant design and economics for chemical engineers, 4th
edition, McGraw-Hill, University of Colorado, 1991.

[2] Al, Turton R. Et. Analysis, Synthesis, And Design Of Chemical Processes. S.L.: Prentice Hall,
2013.

[3] Sudan Costumes Police, Report, 2019

245
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Chapter 13: Equipment Specification Sheets

Table 13-1: Pump -101 Specification sheet

Pump (1)
Identification Item: centrifugal
pump
Item No: P-101
No. Req’d: 2
Function Pump that discharges feed to MIX-101
Operation Continuous
Type Centrifugal
Design Data : Pressure (bar) 1.52
Temperature (°C) 120.98
Flow rate (kg/h) 29766.70
Power (kW) 0.72
Construction Material carbon steel
Purchased Cost: $ 11,600
Bare Module Cost: $ 29,900
Utilities (USD/yr): $ 249

Table 13-2:Pump -102 Specification sheet

Pump (2)
Identification Item: centrifugal
pump
Item No: P-102
No. Req’d: 2
Function Pump that discharges feed to E-103
Operation Continuous
Type Centrifugal
Design Data : Pressure (bar) 1.52
Temperature (°C) 55.00
Flow rate (kg/h) 35949.74
Power (kW) 1.39
Construction Material carbon steel
Purchased Cost: $11,900
Bare Module Cost: $30,600
Utilities (USD/yr): $ 474

246
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-3: E-101 Specification sheet

Heat Exchanger (1)

Identification Item: Heat exchanger
Item No.: E-101
No. Req'd: 1
Function Heating air
Operation Continuous
Type Shell and tube floating head
Heat transfer area (m2) 94.00
Number of shell 1
Shell diameter (m) 0.58
Design Data:
Tube length 6.10
Tube outside diameter (mm) 25.00
Tube Material/shell material Carbon steel/ stainless steel
Purchased Cost: $ 37,800
Bare Module Cost: $ 124,000

Table 13-4: E-102 Specification sheet

Heat Exchanger (2)

Identification Item: Cooler
Item No.: E-102
No. Rq'd: 1
Function Cooling air
Operation Continuous
Type Shell and tube floating head
Heat transfer area (m2) 654.48
Number of shell 1.00
Shell diameter (m) 1.90
Design Data: Tube length 6.10
Tube outside diameter (mm) 50.00
Tube Material/shell material Carbon steel/ stainless steel
Purchased Cost: $140,000
Bare Module Cost: $461,000
Utilities (USD/yr): $6,600

247
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-5: E-103 Specification sheet

Heat Exchanger (3)

Identification Item: Boiler 1
Item No.: E-103
No. Req'd: 1
Function Heating mixture of ( Cumene, CHP, DMBA, ACP, Phenol,
AMS & H2O)
Operation Continuous
Type Shell and tube floating head
Heat transfer area (m2) 9.30
Number of shell 1
Shell diameter (m) 0.34
Design Data:
Tube length 6.10
Tube outside diameter (mm) 50.00
Tube Material/shell material Carbon steel/ stainless steel
Purchased Cost: $30,400
Bare Module Cost: $100,000
Utilities (USD/yr): $26,010

Table 13-6:E-104 Specification sheet

Heat Exchanger (4)

Identification Item: Heat exchanger
Item No.: E-104
No. Req'd: 1
Function Heating mixture of (Cumene, ACP, Phenol, Acetone, AMS &
H2O)
Operation Continuous
Type Shell and tube floating head
Heat transfer area (m2) 94.00
Number of shell 1.00
Shell diameter (m) 0.33
Design Data:
Tube length 6.10
Tube outside diameter (mm) 25.00
Tube Material/shell material Carbon steel/ stainless steel
Purchased Cost: $30,100
Bare Module Cost: $100,000

248
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-7:E-105 Specification sheet

Heat Exchanger (5)

Identification Item: Boiler 1
Item No.: E-105
No. Req'd: 1
Function Heating mixture of (Cumene, ACP, Phenol, Acetone, AMS &
H2O)
Operation Continuous
Type Shell and tube floating head
Heat transfer area (m2) 485.90
Number of shell 1
Shell diameter (m) 0.33
Design Data:
Tube length 50.00
Tube outside diameter (mm) 6.10
Tube Material/shell material Carbon steel/ stainless steel
Purchased Cost: $107,000
Bare Module Cost: $352,000
Utilities (USD/yr): $508,700

249
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-8:R-101 Specification sheet

Reactor (1)
Identification Item: Reactor
Item No.: R-101
No. Req'd: 1
Function Conversion of cumene to CHP
Operation Continuous
Type Bubble Tower
Flow Rate (kmol/hr) 248.61
Temperature (°C ) 310.00
Pressure (kPa) 151.99
Materials handled Stream in: Stream out :
Cumene CHP
Air DMPA
AMS
Water
diameter (m) 1.61
Height (m) 4.83
Reactor volume 13.90
Design data: (m3) Residence 1029.48
time (minute)
material Carbon steel
Reactor purchase cost $ 37,200
Total bare module cost $140000

250
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-9:R-102 Specification sheet

Reactor (2)
Identification Item: Reactor
Item No.: R-102
No. Req'd: 1
Function Conversion of CHP to Phenol
Operation Continuous
Type CSTR
Flow Rate (kmol/hr) 192.17
Temperature (°C ) 328.00
Pressure (kPa) 233.05
Materials handled Stream in: Stream out:
CHP Phenol
DMPA Acetone
AMS
ACP
Water
AMS
diameter (m) 0.91
Height (m) 2.71
Design data: Reactor volume (m3) 1.74
Residence time (s) 219.08
Material Carbon steel
Reactor purchase cost $101,000
Total bare module cost $404000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-10:R-103 Specification sheet

Reactor (3)
Identification Item: Reactor
Item No.: R-103
No. Req'd: 1
Function Conversion of AMS to cumene
Operation Continuous
Type CSTR
Flow Rate (kmol/hr) 75.43
Temperature (°C ) 338.00
Pressure (kPa) 101.33
Materials handled Stream in: Stream out:
AMS Cumene
Phenol H2
H2
Reactor volume (m3) 4.25
Residence time (minute) 133.00
Design data: Material Carbon steel

Reactor purchase cost $151,000

Total bare module $608,000
cost

252
CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-11:T-101 Specification sheet

Distillation Column

Identification Item: Distillation Column

Item No: T-101
No. Req'd: 1
Function Remove acetone
Operation Continuous
Materials Handled Stream In: Streams out:
(Feed) (Distillate) ( Bottoms)
Flow Rate (kmol/hr) 455.55 207.07 245.85
Temperature (°C) 120 70.54 176.22
Composition (mole fraction)
Cumene 0.08 0.01 0.13
ACP 0.01 0.00 0.02
Phenol 0.42 0.92 0.79
Acetone 0.42 0.00 0.00
AMS 0.03 0.00 0.06
H2O 0.03 0.07 0.00
Design Data
Actual Stages 16.00
Diameter(m) 2.03
Height(m) 8.10
Shell Thickness (mm) 4.00
Reflux Ratio 1.15
Plate Type sieve
Materials of Construction carbon steel
Purchased Cost $147,000
Bare Module Cost $252,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-12:T-102 Specification sheet

Distillation Column

Identification Item: Distillation Column

Item No: T-102
No. Req'd: 1
Function Remove cumene
Operation Continuous
Materials Handled Stream In: Streams out:
(Feed) (Distillate) ( Bottoms)
Flow Rate (kmol/hr) 245.85 31.71 214.13
Temperature (°C) 176.22 152.30 180.90
Composition (mole fraction)
Cumene 0.13 0.99 0.00
ACP 0.02 0.00 0.02
Phenol 0.79 0.00 0.91
Acetone 0.00 0.00 0.00
AMS 0.06 0.05 0.07
H2O 0.00 0.05 0.00
Design Data
Actual Stages 95
Diameter(m) 1
Height(m) 39.7
Shell Thickness (mm) 2.995
Reflux Ratio 15.1
Plate Type sieve
Materials of Construction carbon steel
Purchased Cost $277,000
Bare Module Cost $397,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-13:T-103 Specification sheet.

Distillation Column

Identification Item: Distillation Column

Item No: T-103
No. Req'd: 1
Function Remove AMS
Operation Continuous
Materials Handled Stream In: Streams out:
(Feed) (Distillate) ( Bottoms
)
Flow Rate (kmol/hr) 214.13 54.65 197.24
Temperature (°C) 180.91 167.89 182.18
Composition (mole fraction)
Cumene 0.00 0.02 0.00
ACP 0.02 0.00 0.03
Phenol 0.91 0.12 0.97
Acetone 0.00 0.00 0.00
AMS 0.07 0.87 0.01
H2O 0.00 0.00 0.00
Design Data
Actual Stages 41
Diameter(m) 1.8
Height(m) 18.1
Shell Thickness (mm) 2.995
Reflux Ratio 42.6
Plate Type sieve
Materials of Construction carbon steel
Purchased Cost $ 253,000
Bare Module Cost $ 416,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-14:T-104 Specification sheet.

Distillation Column

Identification Item: Distillation Column

Item No: T-104
No. Req'd: 1
Function Phenol purification
Operation Continuous
Materials Handled Stream In: Streams out:
(Feed) (Distillate) ( Bottoms
)
Flow Rate (kmol/hr) 197.21 184.87 12.46
Temperature (°C) 182.18 181.84 187.99
Composition (mole fraction)
Cumene 0 0 0
ACP 0.0249 0.00113 0.378
Phenol 0.974 0.998 0.6215
Acetone 0 0 0
AMS 0.0008 0.0008 0
H2O 0 0 0
Design Data
Actual Stages 48
Diameter(m) 1.7
Height(m) 20.9
Shell Thickness (mm) 2.1
Reflux Ratio 40.5
Plate Type sieve
Materials of Construction carbon steel
Purchased Cost $ 269,000
Bare Module Cost $ 436,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-15:Compressor -101 Specification sheet.

compressor
Identification Item: centrifugal
pump
Item No: c-101
No. Req’d: 2
Function Increase the pressure of Air
Operation Continuous
Type Centrifugal
Design Data : Pressure in (bar) 1.01325
Pressure out (bar) ) 1.51988
Number of stages 1
Flow rate (kmole/h) 4692.68
Power (kW) 182
Construction Material carbon steel
Purchased Cost: $466,000
Bare Module Cost: $1120000

Table 13-16:Cumene storage tank TK-(101).

Storage Tank
Identification Item Storage tank
Item No. TK-(101)
No. Req'd 1
Function Stores cumene feed
Operation Continuous
Type Fixed roof
Design data Pressure (kPa) 101.325
Temperature (℃) 25
Storage volume (𝑚3 ) 785
Material of construction Carbon steel
Purchased cost $ 125,000
Bare module cost $ 137,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-17:Acetone storage tank TK-(102).

Storage Tank
Identification Item Storage tank
Item No. TK-(102)
No. Req'd 1
Function Stores acetone product
Operation Continuous
Type Fixed roof
Design data Pressure (kPa) 101.325
Temperature (℃) 25
Storage volume (𝑚3 ) 452
Material of construction Carbon steel
Purchased cost $ 99,900
Bare module cost $ 110,000

Table 13-18:phenol storage tank TK-(103).

Storage Tank
Identification Item Storage tank
Item No. TK-(103)
No. Req'd 1
Function Stores phenol feed
Operation Continuous
Type Fixed roof
Design data Pressure (kPa) 101.325
Temperature (℃) 25
Storage volume (𝑚3 ) 502
Material of construction Carbon steel
Purchased cost $ 104,000
Bare module cost $ 114,000

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CHAPTER THERTEEN: EQUIPMENT SPECIFICATION SHEETS ||PHENOL

Table 13-19:Cumene mixing tank MIX-(101).

Storage Tank
Identification Item Storage tank
Item No. MIX-(101)
No. Req'd 1
Function Mix cumene and recycle cumene
Operation Continuous
Type Fixed roof
Design data Pressure (kPa) 101.325
Temperature (℃) 25
Storage volume (𝑚3 ) 14
Material of construction Carbon steel
Purchased cost $94,900
Bare module cost $131,000

Table 13-20:Cumene mixing tank MIX-(102).

Storage Tank
Identification Item Storage tank
Item No. MIX-(102)
No. Req'd 1
Function Mix cumene and AMS
Operation Continuous
Type Fixed roof
Design data Pressure (kPa) 101.325
Temperature (℃) 25
Storage volume (𝑚3 ) 14
Material of construction Carbon steel
Purchased cost $ 106,000
Bare module cost $ 147,000

259
CHAPTER FOURTEEN: CONCLUSION AND RECOMMENDATION ||PHENOL

Chapter 14: Conclusion and Recommendation

Conclusion
The cumene Process was adopted and considered for the production of phenol. The Process
results in high yields of the product, acetone as byproduct and fuel. The project was aimed to adopt
a flow diagram that is economically, practically and thermodynamically superior.

Some modifications were done to the process to achieve the objective, such like recycling
cumene from cumene column and considered the recycle of AMS being converted in
hydrogenation reactor rather than discharge it to the environment. And finally, replacement of
sulphuric acid with ZSM-5 catalyst that’s accompanied with some economic and practical issues.

The proposed plant was assumed to produce 126 thousand tons per year phenol that will result
in a positive NPV of 19.659$M and an IRR of 31% over 20 years.

Process ancillaries were designed according to the requirements. Process control of equipment
was obtained to ensure tight control of critical process parameters.

HAZOP studies were performed at critical study nodes, and the environmental impacts of the
plants were considered, the results of the study indicated the process is not green and the plant has
to be allocated away from population residence.

Finally, layout considerations suggested that the plant should be allocated near the raw material
sources to reduce shipping costs; the plant is selected to take place in Khartoum North Industrial
Area.

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CHAPTER FOURTEEN: CONCLUSION AND RECOMMENDATION ||PHENOL

Recommendation
According to the outcomes of this project the following is recommended

• The country may take the phenol industry in consideration as it contributes positively in
the economic renaissance and used in many other manufacturing processes.

• Cumene process can be applied as a method of production of benzene as it gives high

yields, purities of the product, acetone as byproduct and fuel byproduct that can be used in energy
generation.

• The proposed plant can be adopted and a phenol production facility as it is economically
and practically feasible.

261
APPENDIXES A ||PHENOL

Appendix A. Estimation of Physical Properties

In column sizing correlations, estimates of the physical properties are required. It is
unlikely that experimental values will be found in the literature for all systems that are of
practical interest. All the physical properties required in the column sizing will be
covered in this section collectively.
A.1 Acetone distillation column T-(101)
A.1.1 Dynamic viscosity
Dynamic viscosity of pure liquid components:
𝐵
𝑙𝑜𝑔10 𝜇𝑙𝑖𝑞 = 𝐴 + + 𝐶𝑇 + 𝐷𝑇 2 (A.1)
𝑇

Where:
𝜇𝑙𝑖𝑞 ≡ Viscosity of liquid, cP (mN/m2 ).
𝐴, 𝐵, 𝐶 𝑎𝑛𝑑 𝐷 ≡ Regression coefficients for chemical compound.
𝑇 ≡ Temperature in K.
Dynamic viscosity of liquid mixture:
1 3
𝜇𝑚 = (∑ 𝑥𝑖 𝜇𝑖 3 ) (A.2)

Table A-1: Regression coefficients for viscosity calculations.

Component A B C D
Cumene -5.16E-04 8.11E-02 1.0454E-06 -1.05E-09
ACP -7.88E-04 1.25E-01 1.6116E-06 -1.3993E-09
Phenol 0.00015349 0.04262 -9.16E-07 6.23E-09
Acetone -7.21E-04 9.03E-02 1.84E-06 -0.010985
AMS -8.03E-04 1.27E-01 1.63E-06 -1.35E-09
H2O -1.22E-04 1.79E-01 1.77E-06 -1.26E-09

Table 0-2: Estimation of viscosity of benzene distillation column T-(101) feed.

𝑇𝑓 (𝐾) 𝜇 (cP) 1
Component 𝑥𝐹
𝑥𝐹 × 𝜇 3
Cumene 393 1 0.08 0.076
ACP 0.999 0.01 0.011
Phenol 1.002 0.43 0.426
Acetone 0.000 0.42 0.000
AMS 0.9998 0.03 0.0328
H2O 1.001927 0.03 0.033
∑ 5.003544 1 0.578

26
2
APPENDIXES A ||PHENOL

𝜇𝑚 = (0.57847)3 = 0.1936 mN.s/m2

A.1.2 Gas density
For prediction of vapour density of pure hydrocarbons and non-polar gases, the
corresponding state method of Pitzer is the most accurate method, with errors of less than
1 percent.
𝑃 1
𝜌= =𝑉 (A.3)
𝑍𝑅𝑇

For hydrocarbon and non-polar gas mixtures, the Pitzer pure component method can be
used to predict vapour density by replacing the true critical properties with pseudo critical
properties defined by Kay:
𝑇𝑐𝑚 = ∑ 𝑥𝑖 𝑇𝑐𝑖 (A.4)
𝑃𝑐𝑚 = ∑ 𝑥𝑖 𝑃𝑐𝑖 (A.5)
𝜔 = ∑ 𝑥𝑖 𝜔𝑖 (A.6)

Table 0-3: Data needed for gas density estimation.

Component 𝑇𝑐 (𝑘) 𝑃𝑐 (kPa) 𝜔 𝑀𝑤 (kg/mol)

Cumene 631.1 3209 0.3377 120
ACP 709 4060 0.3606 120
Phenol 694.25 6120 0.438 94
Acetone 508.2 4700 0.304 58
AMS 645 3360 0.3273 118
H2O 647.13 22120 0.344 18
Top section:
𝑇 = 343.54 k
𝑃𝑡 = 101.325 kPa
Table 0-4: Gas density estimation on top of T-(101).

Component 𝑥𝐷 𝑥𝐷 𝑇𝑐 (k) 𝑥𝐷 𝑃𝑐 (kPa) 𝑥𝐷 𝜔 𝑥𝐷 𝑀𝑤 (kg/mol)

Cumene 0.013158 8.303947 42.22368 0.004443 1.578947
ACP 0 0 0 0 0
Phenol 0 0 0 0 0
Acetone 0.916353 465.6908 4306.861 0.278571 53.1485
AMS 0 0 0 0 0
H2O 0.070489 45.61537 1559.211 0.024248 1.268797
∑ 1 519.6101 5908.295 0.307263 55.99624

𝑇
𝑇𝑟𝑚 = = 0.66
𝑇𝑐𝑚

263
APPENDIXES A ||PHENOL

𝑇
𝑃𝑟𝑚 = = 0.01715
𝑃𝑐𝑚

To calculate Z use the following equation can be used:

𝑇
𝑍 = 1 + 𝑃𝑟𝑚 [(0.1445 + 0.073𝜔𝑟 ) − (0.33 − 0.46𝜔𝑟 )𝑇𝑟𝑚 −1 − (0.1385 +
𝑟𝑚
0.5𝜔𝑟 )𝑇𝑟𝑚 −2 − (0.0121 + 0.097𝜔𝑟 )𝑇𝑟𝑚 −3 − (0.0073𝜔𝑟 )𝑇𝑟𝑚 −8 (A.7)
𝑍 = 0.974
𝜌 = 0.037 𝑘𝑚𝑜𝑙/𝑚3
𝜌 = 2.084 𝑘𝑔/𝑚3
Bottom section:
𝑇 = 449.217 𝐾
𝑃𝑡 = 101.325 kPa
Table 0-5: Gas density estimation on bottom of T-(101).

Component 𝑥𝐵 𝑥𝐵 𝑇𝑐 (𝑘) 𝑥𝐵 𝑃𝑐 (kPa) 𝑥𝐵 𝜔 𝑥𝐵 𝑀𝑤 (kg/mol)

Cumene 0.129072 81.45748 414.1928 0.043588 15.48867
ACP 0.020042 14.20997 81.37162 0.007227 2.405073
Phenol 0.789544 548.1409 4832.009 0.34582 74.21714
Acetone 0 0 0 0 0
AMS 0.060734 39.17353 204.0668 0.019878 7.16663
H2O 0.000607 0.393029 13.43439 0.000209 0.010932
∑ 1 683.3749 5545.075 0.416722 99.28844

𝑇
𝑇𝑟𝑚 = = 0.65735
𝑇𝑐𝑚

𝑇
𝑃𝑟𝑚 = = 0.018
𝑃𝑐𝑚

𝑍 = 0.96913
𝜌 = 0.0277 kmol/m3
𝜌 = 2.7534 kg/m3
A.1.3 Liquid density
Liquid density for pure components can be obtained by:
𝑇 𝑛
−(1− )
𝜌𝐿 = 𝐴 ∗ 𝐵 𝑇𝑐 (A.8)
Where:
𝜌𝐿 ≡ Saturated liquid density, g/ml.

264
APPENDIXES A ||PHENOL

𝐴, 𝐵 𝑎𝑛𝑑 𝑛 ≡ Regression coefficients for chemical compound.

𝑇 ≡ Temperature, K.
𝑇𝑐 ≡ Critical temperature, K.
Density of liquid mixture:
𝜌𝐿𝑚 = ∑ 𝑥𝑖 𝜌𝐿𝑖 (A.9)
Table 0-6: Data needed for liquid density estimation.

Component A B N 𝑇𝑐 (k)
Cumene 0.604 0.25912 0.2914 631.1
ACP 0.482 0.36511 0.2713 709
Phenol 0.41476 0.32162 0.3212 694.25
Acetone 0.27728 0.2576 0.2699 508.2
AMS 0.436 0.281 0.2896 645
H2O 0.3471 0.274 0.28571 647.13

Top section:
𝑇 = 343.54k
Table 0-7:Liquid density estimation on top of T-(101).

Component 𝜌𝐿 g/ml 𝜌𝐿 kmol/m3 𝑥𝐷 𝑥𝐷 𝜌𝐿 kmol/m3

Cumene 1.767957 1767.957 0.013158 0.193855
ACP 1.118452 1118.452 0 0
Phenol 1.031392 1031.392 0 0
Acetone 0.754189 754.1892 0.916353 11.91558
AMS 1.207224 1207.224 0 0
H2O 0.984842 984.8421 0.070489 3.856681
∑ 1 15.96612

𝜌𝐿 = 894.04 kg/m3

265
APPENDIXES A ||PHENOL

Bottom section:
𝑇 = 118.071
Table 0-8: Liquid density estimation on bottom of T-(101).

Component 𝜌𝐿 g/ml 𝜌𝐿 kmol/m3 𝑥𝐵 𝑥𝐵 𝜌𝐿 kmol/m3

Cumene 1.545928 1545.928 12.88273 1.662803
ACP 1.038215 1038.215 8.65179 0.173402
Phenol 0.934084 934.0837 9.937061 7.845747
Acetone 0.591988 591.9875 10.20668 0
AMS 1.071068 1071.068 9.076848 0.551275
H2O 0.873481 873.4808 48.52671 0.029472
∑ 10.2627

𝜌𝐿 = 1018.97 kg/m3
Surface tension
𝑇 𝑛
𝜎𝑖 = 𝐴 (1 − 𝑇 ) (A.10)
𝑐

𝜎𝑖 ≡ Surface tension for component i, dynes/cm; mN/m.

𝐴, 𝑇𝑐 𝑎𝑛𝑑 𝑛 ≡ Regression coefficients for chemical compound.
𝑇 ≡ Temperature, K.
Table A-9: Estimation of surface tension on top and bottom of T-(101).

Component A 𝑇𝑐 K N 𝜎𝑖 𝑡𝑜𝑝 mN/m 𝜎𝑖 𝑏𝑜𝑡𝑡𝑜𝑚 mN/m

Cumene 60.4 631.1 1.4784 2.359500884 13.53172633
ACP 48.2 709 1.389 0 0.162971971
Phenol 41.476 694.25 1.4268 0 4.042959033
Acetone 27.728 508.2 1.2093 9.221382646 0
AMS 43.6 645 1.539 0 0.867499033
H2O 34.71 647.13 1.521 5.447707326 0.02904776

The surface tension of liquid mixture is not a simple function of the pure component
surface tensions because the composition of the mixture surface is not the same as the
bulk, for no aqueous solutions of n components, the method of Winterfled, Scriven, and
Davis is applicable:
𝑛 𝑛
𝑥𝑖 𝑥𝑗 1
2
𝜎𝑚 = ∑ ∑ 𝜌 ( ) ( ) (𝜎𝑖 𝜎𝑗 )2 (A. 11)
𝜌𝐿𝑖 𝜌𝐿𝑗
𝑖=1 𝑗=1

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APPENDIXES A ||PHENOL
𝑛
1 𝑥𝑖
= ∑( ) (A. 12)
𝜌 𝜌𝐿𝑖
𝑖=1

Where:
𝜎𝑚 ≡ Surface tension of mixture, mN/m.
𝜌𝐿 𝑖,𝑗 ≡ Pure component liquid density of component i or j, kmol/m3 .

𝜎𝑖,𝑗 ≡ Pure component surface tension of component i or j, mN/m.

Top section:
𝜎𝑚 = 17.029 mN/m
Bottom section:
𝜎𝑚 = 18.638 mN/m

A.2 Energy balance

A.2.1 Heat capacity
𝐶𝑝 = 𝑎 + 𝑏𝑇 + 𝑐𝑇 2 + 𝑑𝑇 3 J/kmol.K (A.13)
𝑇 ≡ Temperature, K.

Table A-10: Heat capacity constants for gases.

Component A B c d
Cumene 139200 537.60 -0.40 0.00
O2 29,100.00 11.58 -0.01 0.00
N2 29,000.00 2.20 0.01 0.00
Methanol 42,930.00 83.01 -0.02 0.00
CHP 293570 0.00 0.00 0.00
DMBA 270000 0.00 0.00 0.00
ACP 0.00 0.00 0.00 0.00
Phenol 43,400.00 244,500.00 1,152.00 151,200.00
Acetone 71,960.00 201.00 -0.13 0.00
AMS 202200 0.00 0.00 0.00
H2O 3.35E+04 6.88E+00 7.60E-03 -3.59E-06
H2 2.88E+04 7.65E-02 3.29E-03 -8.70E-07

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APPENDIXES A ||PHENOL

Table A-11: Heat capacity constants for liquids.

Component Cp
Cumene 195,340.00
O2 0.00
N2 0.00
Methanol 0.00
CHP 295,596.00
DMBA 205,010.00
ACP 241,530.00
Phenol 101,720.00
Acetone 123,000.00
AMS 186,220.00
H2O 75400

Vapor pressure (Antoine's parameters)

𝑏
𝐿𝑛(𝑃 𝑘𝑃𝑎) = 𝑎 + 𝑇+𝑐 (A.14)

𝑇 ≡ Temperature, K.

Table A-12: Vapor pressure constants.

Component A b c
Cumene 7.10691 1577.97 220.977

ACP 7.39996 1901.19 218.697

Phenol 7.54098 1801.28 204.687

Acetone 7.31414 1315.67 240.479

AMS 7.12904 1641.01 220.782

H2O 7.96681 1668.21 228

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Components' formulas and molecular weights

Table A-13: Components’ formulas and molecular weights.

Component Formula Molecular weight

Cumene C9 H12 120
Oxygen O2 32

Nitrogen N2 28
Methanol CH3OH 32

CHP C9 H12 O2 152

DMBA C20 H16 136

ACP C8 H8O 120

Phenol C6 H6 94

Acetone C3 H6 𝑂 58
AMS C6 H6 118
H2O C9 H10 18

Hydrogen H2 2

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Appendix B. Economic indicators (CEPCI)

Figure B-1:Economic Indicators

270
 APPENDIX C ||PHENOL

Appendix C. MSDA
Appendix is attached with the file

271