PRODUCTION OF SECONDARY BUTYL ALCOHOL

AND DESIGN OF DISTILLATION COLUMN

A PROJECT REPORT

Submitted by

S
NO NAME REG.NO
:
1 GOPAL K (611517139031)
2 FAYSAHMED S (611517139029)
3 KANISHKAR C (611517139044)
4 KISHOREKUMAR A (611517139048)
In partial fulfilment for the award of the degree
Of
BACHELOR OF ENGINEERING
In

PETROCHEMICAL ENGINEERING
MAHENDRA INSTITUTE OF ENGINEERING AND
TECHNOLOGY
NAMAKKAL

ANNA UNIVERSITY: CHENNAI 600 025

APRIL 2021
 ANNA UNIVERSITY : CHENNAI

BONAFIDE CERTIFICATE

Certified that this project report “PRODUCTION OF SECONDARY

BUTYL ALCOHOL AND DESIGN OF DISTILLATION COLUMN” is
the bonafide work of “GOPAL.K,FAYSAHMED.S,KANISHKAR.C and
KISHOREKUMAR.A” who carried out the project work under my supervision.

SIGNATURE SIGNATURE
Mr.A.ELAMARAN,M.E., Mr.A.SENTHIL RAJA,M.E.,
SUPERVISOR HEAD OF DEPARTMENT
ASST.PROFESSOR PROFESSOR
DEPT OF PETROCHEMICAL ENGG DEPT OF PETROCHEMICAL ENGG
MAHENDRA INST. OF ENGG&TECH MAHENDRA INST. OF ENGG&TECH
MALLASAMUDRAM, MALLASAMUDRAM,
NAMAKKAL – 637 503 NAMAKKAL – 637 503

Submitted for the University Practical Examination held on …………….

INTERNAL EXAMINER EXTERNAL EXAMINER

 PAGE
CHAPTR TABLE OF CONTENTS NO
NO. TITLE
ABSTRACT I
LIST OF TABLES II
LIST OF FIGURES III

LIST OF SYMBOL VI

1 INTRODUCTION 1
1.1 COMPANY PROFILE 1
1.2 PROPERTIES 2
1.2.1 N-Butene 2
1.2.2 Secondary butyl alcohol 3
1.2.3 Sulphuric Acid 3
1.3 MANUFACTURING PROCESS 4
1.3.1 Direct Hydration 4
1.4 APPLICATION OF SBA 5
1.5 ADVANTAGES 6
1.6 DISADVANTAGES 6
1.7 CONSEMPTION PATTERN 7
2 MANUFACTURING METHOD 9
2.1 SBA SYNTHESIS 9
2.1.1 Acid Blending 10
2.1.2 Esterification 10
2.1.3 Prehydrolysis Column 11
2.1.4 Hydrolysis Column 11
2.1.5 Neutralization Column 11

2.1.6 Butene Recovery System 12

1
 2.2 SBA DISTILLATION 13
2.2.1 SBE-Water Distillation 14
2.2.2 SBA-Heavies Column 14
2.2.3 SBA-SBE Section 15
2.2.4 Water-SBA Distillation 15
3 MATERIAL BALANCE 16
3.1 1ST STAGE REACTOR 16
3.2 1ST STAGE DECANTER 17
3.3 2ND STAGE REACTOR 19
3.4 2ND STAGE DECANTER 20
3.5 BUTENE WASH COLUMN 21
3.6 PREHYROLYSIS 22
3.7 HYDROLYSIS 23
3.8 NEUTRALIZATION COLUMN 24
3.9 SBE-WATER COLUMN 26
3.10 ACCUMULATOR 1 27
3.11 SBA RETUNE COLUMN 29
3.12 SBA-HEAVIES COLUMN 30
3.13 ALCOHOL EXTRACTION COLUMN 31
3.14 ACCUMULATOR 32
3.15 SBA STRIPPING COLUMN 32
4 ENERGY BALANCE 33
4.1 1ST STAGE REACTOR 33
4.2 2ND STAGE REACTOR 35
4.3 BUTANE WASH COLUMN 37
4.4 PREHYDROLYSIS 39

4.5 HYDROLYSIS 40

2
 4.6 NEUTRALIZATION COLUMN 42
4.7 SBE-WATER COLUMN 44
4.8 SBA RETURN COLUMN 47
4.9 SBA-HEAVIES COLUMN 49
4.10 ALCOHOL EXTRACTION COLUMN 51
5 DESIGN OF EQUIPMENTS 52
5.1 DESIGN OF DISTILLATION COLUMN 52
5.1.1 McCabe Thiele Method 53
5.1.2 Binary Distillation Sieve Tray
Efficiency 56
5.1.3 Number of Actual Stages 56
5.1.4 Calculation of Column Height 56
5.1.5 Top Section 57
5.1.5.1 Flooding Velocity 57
5.1.5.2 Actual Vapour Velocity 58
5.1.5.3 Vapour Volumetric Flow Rate 58
5.1.5.4 Bubbling Area 58
5.1.5.5 Cross Sectional Area 58
5.1.5.6 Column Diameter 59
5.1.6 Bottom Section 59
5.1.6.1 Flooding Velocity 59
5.1.5.2 Actual Vapour Velocity 60
5.1.5.3 Vapour Volumetric Flow Rate 60
5.1.5.4 Bubbling Area 60
5.1.5.5 Cross Sectional Area 61
5.1.5.6 Column Diameter 61

5.1.7 Provisional Plate Design 61

3
 5.1.7.1 Down Comer Area 61
5.1.7.2 Net Area of the Column 61
5.1.7.3 Active Area 61
5.1.7.4 Hole Area 62
5.1.7.5 Weir Length 62
5.1.8 Design Summary 62
6 PROCESS ECONOMICS 63
6.1 COST ESTIMATION 63
6.2 DIRECT COST 63
6.2.1 Equipment Cost 64
6.2.2 Land cost 64
6.2.3 Instrument and Installation Cost 64
6.2.4 Electrical and Instrument Cost 65
6.2.5 Building process and Auxiliary 65
6.2.6 Service facilities and yard improvement 65
6.3 INDIRECT COST 65
6.3.1 Engineering Supervision 66
6.3.2 Construction Expense and
Construction Fees 66
6.3.3 Contingency 66
6.4 ESTIMATION OF TOTAL
PRODUCTION COST 66
6.4.1 Production cost 66
6.4.2 Direct production cost 67
6.4.3 Raw material cost 67
6.4.4 Operating labour Cost 67

6.4.5 Direct Supervisory and Clinical Cost 67

4
 6.5 UTILITIES 68
6.5.1 Maintenance and Repair Cost 68
6.5.2 Patents and royalties Cost 68
6.5.3 Fixed Charges 68
6.5.4 Plant overheads 68
6.5.5 Depreciation 68
6.5.6 Insurance 68
6.5.7 General Expenses 69
6.5.8 Distribution and Selling Cost 69
6.5.9 Research and Development 69
6.5.10 Financing 69
6.6 PAYBACK PERIOD 70
6.6.1 Gross Earning Cost 70
6.6.2 Net Profit 70
7 PLANT SAFETY 71
7.1 PROCESS SAFETY 71
7.2 FIRE SITUATION 71
7.3 TYPES OF FIRE 72
7.3.1 Class A 72
7.3.2 Class B 73
7.3.3 Class C 73
7.4 CHEMICAL HAZARD PRECAUTION 73
7.4.1 Methyl Ethyl Ketone 73
7.4.2 Secondary Butyl Alcohol 74
7.4.3 Hydrogen 74
7.4.4 Caustic Soda Solution 75

7.4.5 Sulphuric Acid 75

5
 7.5 ACCIDENTAL RELEASE MEASURES 76
7.5.1 Small Spill 76
7.5.2 Large Spill 76
8 CONCLUTION 77

9 REFERENCE 78

6
 ABSTRACT

Secondary butyl alcohol is one of the major product produced in cetex

petrochemicals. Cetex petrochemicals uses indirect hydration process to
produce secondary butyl alcohol. Cetex petrochemicals is one and only industry
in south Asian countries to produce methyl ethyl ketone. For that process,
secondary butyl alcohol is the major reactant. As the demand of secondary butyl
alcohol is increasing throughout the world, the cetex petrochemical is in dire
need of new way to increase the production rate. So our project will be concern
about the way of increasing the production rate by altering the design of
distillation column condenser which is playing an important role in purification
of secondary butyl alcohol, produce from the synthesis process.

7
 LIST OF THE TABLE
PAGE
TABLE NO TITLE OF THE TABLE NO.
1.1 N-butane properties 2
1.2 SBA Properties 3
1.3 Sulphuric acid properties 3
3.1 1ST Stage reactor input 16
3.2 1ST Stage reactor output 17
3.3 1ST Stage decanter input 18
3.4 1ST Stage decanter top product 18
3.5 1ST Stage decanter bottom product 19
3.6 2ST Stage reactor input 19
3.7 2ST Stage reactor output 20
3.8 2ST Stage decanter input 20
3.9 2ST Stage decanter top product 21
3.10 2ST Stage decanter bottom product 21
3.11 Butane wash column input 22
3.12 Butane wash column top product 22
3.13 Butane wash column bottom product 22
3.14 Prehydrolysis column input 22
3.15 Prehydrolysis column output 23
3.16 Hydrolysis column input 24
3.17 Hydrolysis column output 24
3.18 Neutralization column input 25
3.19 Neutralization column top product 25
3.20 Neutralization column bottom product 26
3.21 SBE-Water column input 26
3.22 SBE-Water column distillate 27
3.23 SBE-Water column bottom product 27

3.24 Accumalator1 input 27

8
3.25 Accumalator1 top output 28
3.26 Accumalator1 bottom output 28
3.27 SBA-Return column input 29
3.28 SBA-Return column distillate 29
3.29 SBA-Return column bottom product 29
3.30 SBA-Heavies column input 30
3.31 SBA-Heavies column distillate 30
3.32 SBA-Heavies column bottom product 31
3.33 Alcohol extraction column input 31
3.34 Alcohol extraction column top product 31
3.35 Alcohol extraction column bottom product 32
3.36 Accumulator 2 output 32
3.37 SBA stripping column input 32
3.38 SBA stripping column top product 33
3.39 SBA stripping column bottom product 33
4.1 1ST Stage reactor input 34
4.2 1ST Stage reactor output 34
4.3 2ST Stage reactor input 36
4.4 2ST Stage reactor output 36
4.5 Butane wash column input 37
4.6 Butane wash column output 38
4.7 Prehydrolysis column input 39
4.8 Prehydrolysis column output 39
4.9 Hydrolysis column input 41
4.10 Hydrolysis column output 41
4.11 Neutralization column input 43
4.12 Neutralization column output 43
4.13 SBA-Water column input 44

4.14 SBA-Water column distillate 45

9
4.15 SBA-Water column bottom product 45
4.16 SBA-Return column input 47
4.17 SBA-Return column distillate 47
4.18 SBA-Return column bottom product 48
4.19 SBA-Heavies column input 49
4.20 SBA-Heavies column distillate 50
4.21 SBA-Heavies column bottom product 50
4.22 Alcohol extraction column input 51
4.23 Alcohol extraction column top product 51
4.24 Alcohol extraction column bottom product 52
5.1 SBA vs Heavies data 53
5.2 Equilibrium data 53

5.3 Design summary of distillation column 62

10
 LIST OF FIGURES
S.No. Title of the figure Page No.
Fig 1.1 Consumption pattern 7
Fig 2.1 Raw SBA synthesis 9
Fig 2.2 SBA distillation 13

Fig 5.1 McCabe Thiele method 55

 LIST OF SYMBOLS
S.No. SYMBOL DESCRIPTION
1 Μ Viscosity,kg/ms
2 A Area,m2
3 Ρ Density,kg/m3
4 D Diameter of the vessel,m
5 Α Relative volatility
6 Σ Surface tension, dyn/cm

7 Uc Maximum vapour velocity

 CHAPTER 1

INTRODUCTION

1. 1 COMPANY PROFILE

Cetex Petrochemicals Ltd is the only manufacturer of Methyl Ethyl Ketone

(MEK) and Secondary Butyl Alcohol (SBA) in south Asian countries. Since its

Establishment in 1990 with German technology, Cetex has expanded rapidly in the

last 10 years to include a diverse portfolio of products such as pharma

intermediates, aroma chemicals, fuel additives and treatment chemicals. Cetex

petrochemicals located in Manali, the Industrial area of Chennai, Tamilnadu. Cetex

is close to Chennai and Ennore ports and therefore has the competitive advantage

of efficient logistics.

Their raw material is received through pipeline from Chennai Petroleum

Corporation Limited (CPCL), an integrated petrochemical refinery complex,
located 2km away from their facility. Their major products find versatile
applications in the manufacture of paints, printing inks, adhesives, coatings, aroma
chemicals, and specialty intermediate in pharma industries and lube additives.
Plant has capacity to Produce 10,000 TPA of MEK and 10,000 TPA of

SBA. In India, Cetex is the only Manufacturer of Methyl Ethyl Ketone (MEK) and

Secondary Butyl Alcohol (SBA) with ISO 9001:2008, ISO 14001:2004 and BS

OHSAS 18001; 2007 certification. Product quality of Cetex is at par with

international levels and Cetex has no history of project rejection since its inception.

The company is well committed to safe environmental practices. Cetex practices

deep rooted TPM, TQM and five years initiatives.

13
 Cetex gives top priority to workers safety and equipment management. The

company is well equipped with safety systems and trained man-power. It has been

reported that there have been no untoward incidents or safety malpractices for the

past 12 years. As a part of our system requirements, they conduct regular audits to

monitor the quality of products and services offered to their customers.

Cetex has been conferred some of the country's highest awards for the good

standards of safety set by this plant. It has won the Star Safety Award for the good

standards of safety set by this plant. It has won the Star Safety Award for the year

2000 to 2002 from the National Safety Council. It has also been awarded the state

government award for safety for three consecutive year's from1998 and 1999, by

the government of Tamil Nadu.

1.2 PROPERTIES

1.2.1 N-Butene
Table 1.1 N-Butene properties

Name N-Butene

Family Hydrocarbon
Formula C4H8

Nature LPG

Boiling point -2 C

Specific gravity 0.6213

Flash point 73 C

Molecular weight 56.03

Density 0.586 Kg/cm

Appearance Colourless

Odor Aromatic

s 14
1.2.2 Secondary Butyl Alcohol
Table 1.2 SBA properties

Name Secondary butyl alcohol

Family Hydrocarbon
Formula C4H10O
Nature Liquid
Boiling point 98 to 100 C

Specific Gravity 0.808

Flash Point 23.6 C
Melting Point -115 C

Density 0.808 g cm

1.2.3 Sulphuric Acid

Table 1.3 Sulphuric acid properties

Name Sulphuric acid

Family Acid

Formula H2SO4

Nature Liquid

Specific Gravity 1.834

Molecular Weight 98.04

Density 0.586 Kg/cm

15
 Appearance Colourless to yellowish

1.3 MANUFACT URING METHODS

 Indirect hydration of N-butene with sulphuric acid

 Direct hydration of n-butene to secondary butyl alcohol

catalyzed by strong acidic ion exchange resins

1. 3.1 Direct hydration

It is a heterogeneous catalyzed process. The hydration of n-butene to secondary

butyl alcohol catalysed by strong acidic ion exchange resin is an Alternative route
to the conventional homogenous indirect hydration process catalyzed by sulphuric
acid.

C4 H8+H2O CH3-CH2-CH-(OH)-CH3 + H2SO4

(Secondary-Butyl Alcohol)

Disadvantages
 High pressure must be used to compensate the high temperature.

 The condition used in direct hydration is more vigorous because of a

relative low activity of the catalyst demanding to use high temperature to

obtain reasonable reaction rate.

Advantages
 The main advantage of direct hydration is elimination of sulphuric

acid.

 Environment friendly

16
1.3.2 Indirect hydration

It is a homogeneous catalyst process. For a long time the hydration of butane

on the industrial scale has been catalyzed by sulphuric acid. It is a two-step process

in which the first step is absorption of butane in concentrated sulphuric acid that

used to formation of alkyl halogen sulphate followed by dilution with water and

hydrolysis.

CH3CH=CHCH3 + H2SO4 C4H7 –OSO3 H

(Butene) (Monobutyl ester)
C4 H7-OS03H + CH3CH=CHCH3 C4H9-S04-C4 H9
(Monobutyl ester) (Butene) (Dibutyl ester)
C4 H9-S0 4-C4H9+2H2O 2CH3 -CH (OH)-CH3 +
H2so4
(Dibutyl ester) ( Secondary butyl alcohol )

Advantage
 Low temperature and pressure

 Use of olefins at low hydrocarbon feed

Disadvantages

 Use of highly corrosive reagent that requires large energy

consumption for regeneration.

1.4 APPLICATION OF SBA

 Used as a solvent in paints and industries

 Used as a solubiliser for the production of cleaning

compounds
 Used in printing works
 In manufacture of dyes, adhesives,
miningchemical,surfactant
17
  Used as a raw material for lube additives

 Used as a coupling agent for water reducible cleaning

formulations
 In manufacture of Methyl Ethyl Ketone

1.5 ADVANTAGES
 Low toxicological potential
 Biodegradable
 Low retention in flexible films (polyethylene and
polypropylene), reducing blocking after painting, with
better organoleptic advantages than that of n-butanol
and
Isobutanol
 Enables better solubilisation of resins, allowing less viscous
formulas and/or with less active solvent.
 With regard to the dilution rate (toluene), it helps the active
solvent in accepting diluent. Regarded as a linking agent, it
has better performance compared to n-butanol and
isobutanol (60% soluble in water)
 Low retention in flexible packages (application of
flexographic inks).
1.6 DISADVANTAGES
 Several explosions have been reported during the
conventional distillation of 2-butanol, apparently due to the
build-up of peroxides with the boiling point higher than that
of pure alcohol (and therefore concentrating in the still pot
during distillation).
 As alcohols, unlike ethers, are not widely known to be
capable of forming peroxide impurities, the danger is likely

to be overlooked. Secondary butyl alcohol is flammable.

18
  Its vapour can readily form an explosive mixture in air. It

is harmful by inhalation.

1.7 CONSUMPTION PATTERN

Solvent in paintPrinting worksSolubilizer in Manufactor of MEK

cleaning agentsManufactor of dyes

13%

7%
37%

19%

24%
Fig 1.1 Consumption Pattern

Secondary butyl alcohol (SBA) is a solvent for ester gum, many nature

resins and vegetables oils; in the presence of aromatic hydrocarbons it forms a

good solvent mixture of alkylated coating and lacquers based on ethyl cellulose.

As a latent solvent in nitrocellulose lacquers, it provides good gloss and

levelling properties. The mutual solvency of secondary butyl alcohol for water

and oil has made it useful as a coupling agent in the formulation and preparation

of industrial cleaning compounds, oil treating chemical, paint removers and oil-

water emulsion breakers.

19
 SBA also acts as a chemical intermediate in the manufacture of methyl

ethyl ketone, ore floatation agent, fruit essence, perfumes, dye-stuffs and

wetting agents. Other uses for SBA are as a solvent in the manufacture of

polypropylene, for special greases, in printing inks and in adhesive for plywood

laminates.

It used as solvent in the remover, varnish and paint industry. Its addition

into paints, in small quantities, reduces viscosity and retards the formation of oil

residues (known as blush) on the surface SBA is used in solvents and in esters

to a limited extent; larger amounts are oxidised to methyl ketone (2-butanone),

an important solvent for manufacture of plastics, fabrics, and explosive

It is used in solvent and in plasticizers. Its esters are also used in fruit

flavourings. In smaller quantities, it is used in flavouring and perfumes.

20
 CHAPTER 2
MANUFACTURING PROCESS
2.1 SECONDARY BUTYL ALCOHOL STNTHESIS

Fig 2.1 Raw SBA synthesis

21
2.1 Acid blending

Acid blending is the first step which has to be done before the esterification

reaction. The esterification reaction needs sulphuric acid of concentration 75%

because higher concentration acid leads to formation of polymer and lower

concentration reduces the conversion rate of the butane.

The raw sulphuric acid is generally at a concentration of 98%. In order to

obtain the desired concentration range 98% acid is blended with 60% spent acid
from hydrolysis chamber to get a concentration of 75%. The blended acid is stored
in carbon storage vessel.

2.2.2 Esterification

The esterification reaction is carried out is two stage reactor. In first stage
reactor fresh butane is fed from top of the reactor and acid rich ester from decanter
2 is fed to bottom of the reactor. The butane and sulphuric acid will react and form
dibutyl ester.

This mixture is then store in decanter I where it is allowed to settle. Two

phases will form in the decanter I based on its density compared to ester it will
form the upper layer. The upper layer contains butane, unreacted butane, ester
which is fed to second stage reactor from top of the reactor and fresh 75% acid is
fed from the reactor bottom.

The product mixture from second stage reactor was allowed to settle in
decanter 2 where two layers were formed. The lower layer is acid rich layer which
is fed to the first stage reactor and the upper layer contains unreacted butane and
butane. This is then washed in a wash water column where butane is separated and
send to the LPG recovery system and washed water which contains acid and some
amount of unreacted butane is fed to the pre -hydrolysis column.

22
2.1.3 Prehydrolysis column

Ester on hydrolysis will give acid and alcohol. It is an endothermic

reaction. Here, it is partially hydrolysed in the presence of water at a pressure of
2.5 bar. The ester from the decanter 1 enters the pre-hydrolysis column. Before
entering the column it is mixed with wash water from column in a mixer. The
water enters the column through the flow control. Both stream are contacted
counter-currently. Hydration of acid leads to increase in temperature and pressure.
The pre -hydrolysed diluted ester leaves the bottom of column
automatically due to high pressure. This leads to decrease in pressure and thereby
unreacted butane was released from the ester. This butane is neutralized and used
as reactant for esterification.

2.1.4 Hydrolysis column

The diluted pre-hydrolysed ester enters the glass column. In this column the

completely hydrolysed to secondary butyl alcohol and acid. The reboiler which

uses hot oil as heat source provides the vapour steam in the glass column. The feed

continuously enters the glass column and it is contacted with vapour counter

currently. The ester is hydrolyzed into SBA and H2SO4. The top product is

vapours of SBA with some traces of acid. The bottom product is 60% spent

sulphuric acid which is used for acid blending.

2.1.5 Neutralization column

The SBA vapours from hydrolysis column enters the neutralization column
in lower section, in order to make SBA completely acid -free. The raising vapours
are first neutralized with circulated caustic from vessel in the top of section of the
column for removal of SO4 from SBA vapours with butane gas leaves the top of
the column and they are condensed in a condenser and the liquid is collected in a
vessel.
2.1.6 Butene recovery system

The SBA vapour coming out of the top of the column are condensed in
condenser. Here the butane is separated from the SBA liquid. The SBA liquid is
collected in raw SBA accumulator where two layers was formed. The upper layer
is enriched with raw SBA. It is pumped by a pump for distillation. The lower layer
is water with some traces of SBA which flows of the vessels where it is stored for
further purification.

24
2.2 SECONDARY BUTYL ALCOHOL DISTILLATION

Fig 2.2 SBA Distillation

25
2.2.1 SBA- Water Azeotropic Distillation Column

The azeotropic distillation is used because the boiling point of SBA (99o C)
and water (100o C) is close. The raw SBA collected in SBA accumulator is
pumped to upper section of SBE-Water column C151. The SBE-Water column is
operated at atmospheric pressure. In this column the SBA is separated from water
and heavies but complete separation is not possible. The SBE with SBA and water
is going overhead on vapour phase, forming a ternary azeotrope. Here ether act as a
entrainer.

A reboiler is provided for the purpose of supplying the vapours. Each tray
provides a stage of contact between the two streams. The vapours use the heat to
the liquid. The vapours from column are enriched with ether, water and little
amount of SBA. Whereas the residue contain SBA, heavies and some amount of
water. The vapours leaving the column is condensed in overhead condenser E152.
The condenser liquid is separated into two layers in a decanter V151.

The upper layer is organic which consist of ether and the lower aqueous
layer consist of water and some amount of SBA. The lower aqueous layer is
separated and stored in a vessel V152. In V152, the water rich SBA from SBA
accumulator is also stored.
2.2.2 SBA-Heavies Column

The bottom product from SBE- Water column is pumped to SBA-

heavies C152 by a pump for the separation of SBA from heavies through the flow
control valve. The heat required to the distillation column at bottom heated with
steam. This supply of heat is controlled by the flow controlled valve. The pure
SBA is fed to the top of the column where SBA is vaporised and the heavies is
separated as residue. This heavies goes to the intermediate column C153 in order
to remove the remaining SBA.
 The pure SBA stream leaving the top of the intermediate distillation
column is again fed C152 as reflux in order to increase the purity of SBA. The
heavies are separated in the bottom of the column. The product is sent to the
cooler and then stored in tank.
2.2.3 SBE-SBA section

The organic layer of vessel V151 which contains some SBA goes to the
bottom of extract column C154 through the pump. The water coming from
exchanger enter the top of the column. As water is miscible with SBA and
immiscible with ether. The SBA is washed away along with water ant it is stored in
V152. The ether leaves from top of the column. This ether is used as the third
component in SBE-Water azeotropic distillation column.
2.2.3 Water-SBA Distillation

Water and SBA mixture collected in the vessel V152 is pumped to SBA
striping column where SBA is stripped out, the necessary heat is supplied with
steam heated reboiler E-156. The vapours leaving C-155 at top contains water also.
They enter C-156 where the MEK is separated as a mixture with SBA and water.
The necessary heat is supplied with steam heated reboiler E -159, the vapours are
condensed by E -160. The bottom product in C-155 which is water and SBA is
partly used as reflux for C-155 and is partly returned to SBA accumulator.

27
 CHAPTER 3

MATERIAL BALANCE

Basis: 1500 kg/h of SBA production

3.1 1st STAGE REACTOR:

C4H7-OSO3H + CH3CH=CHCH3 C4 H9-SO4-C4H9

(Monobutyl ester) (Butene) (Dibutyl ester)

Table 3.1 1st stage reactor input

Component Weight % Mass flow rate(kg/h)

Butene 26.64 708.4

Acid rich ester 73.33 1950.63

Total 2659.03

Output:

Table 3.2 1st stage reactor output

Component Weight % Mass flow rate(kg/h)

UR Butene 2.76 73.656

Butane 3.5 93.2085

28
 Polymer 0.61 16.23

Ester 80.02 2127.825

Water 6.18 164.415

Sulphuric acid 6.37 169.551

Dissolved butene 0.53 14.148

Total 2659.03

3.2 1st STAGE DECANTER:

Input:
Table 3.3 1st stage decanter input

Component Weight % Mass flow rate(kg/h)

UR butene 2.76 73.656

Butane 3.5 93.2085

Polymer 0.61 16.23

Ester 80.02 2127.825

Water 6.18 164.415

Sulphuric acid 6.37 169.551

Dissolved butene 0.53 14.148

Total 2659.03

29
Top product:
Table 3.4 1st stage decanter top product

Component Weight% Mass flow rate(kg/h)

UR butane 40.23 73.656

Butane 50.9 93.2085

Polymer 8.86 16.23

Total 183.0945

Bottom product:
Table 3.5 1st stage bottom product

Component Weight% Mass flow rate(kg/h)

Ester 85.94 2127.825

Water 6.64 164.415

Acid 6.84 169.551

Dissolved butene 0.57 14.14

Total 2475.931
3.3 2nd STAGE REACTOR:

CH3CH=CHCH3+H2SO4 C4H7-OSO3H
(Butene) (Monobutyl ester)

Input:

Table 3.6 2st stage reactor input

Component Weight% Mass flow rate(kg/h)

UR butane 3.54 73.656

Butane 4.48 93.2085
Polymer 0.78 16.23
Fresh acid 63.66 1323.975
Recycle acid 27.54 594.776

Total 2101.8455

Output:

Table 3.7 2st stage reactor output

Component Weight% Mass flow rate(kg/h)

Butane 3.61 93.2085

Polymer 0.66 16.98
Acid 0.56 11.7645

Acid rich ester 93.78 1950.63

31
 UR butane 1.41 29.4825

Total 2102

3.4 2nd STAGE DECANTER:

Input:

Table 3.8 2st stage decanter input

Component Weight% Mass flow rate (kg/h)

Butane 3.61 93.2085

Polymer 0.66 16.98

Acid 0.56 11.7645

Acid rich ester 93.78 1950.63

UR Butane 1.41 29.4825

Total 2102

Top product:

Table 3.9 2nd stage decanter top product

Component Weight% Mass flow rate(kg/h)

Butane 61.55 93.2085

32
 Polymer 11.21 16.98

Acid 7.77 11.7645

UR butene 19.49 29.482

Total 151.42

Bottom product:

Table 3.10 2nd stage decanter bottom product

Component Weight% Mass flow rate(kg/h)

Acid rich ester 100 1950.63

3.5 BUTANE WASH COLUMN:

Input:

Table 3.11 butane wash column input

Component Weight% Mass flow rate(kg/h)

Butane 27.4 93.2085

Polymer 4.99 16.98

Acid 3.46 11.7645

UR butene 8.66 29.482

Water 55.47 188.67

Total 340.11

33
Top output:

Table 3.12 Butane wash column top product

Component Weight% Mass flow rate(kg/h)

Butane 66.75 93.2085

Polymer 12.16 16.98

UR Butene 21.09 29.482

Total 139.645

Bottom output:

Table 3.13 Butane wash column bottom product

Component Weight% Mass flow rate(kg/h)

Wash water 100 11.13

3.6 PREHYDROLYSIS COLUMN:

Input:

Table 3.14 Prehydrolysis column input

Component Weight% Mass flow rate(kg/)

Ester 79.65 2127.825

Wash water 13.65 364.77

Sulphuric acid 6.34 169.551

34
 Dissolved butene 0.529 14.14

Total 2671.286

Output:

Table 3.15 Prehydrolysis column output

Component Weight% Mass flow rate(kg/h)

Ester 76.6 2127.825

Wash water 13.65 364.77

Sulphuric acid 6.34 169.551

Dissolved butene 0.19 5.283

Excaped butene 0.331 8.857

Total 2671.286

3.7 HYDROLYSIS COLUMN:

C4H9-SO4-C4H9 + 2H2 2CH3-CH2-CH(OH)-CH3+H2SO4

(Dibutyl ester)
(Secondary-Butyl Alcohol)

35
Input:

Table 3.16 hydrolysis column input

Component Weight% Mass flow rate(kg/h)

Ester 79.92 2127.825

Water 13.70 364.97

Sulphuric acid 6.3 169.551

Dissolved butene 0.18 5.283

Total 2662.429

Output:

Table 3.17 Hydrolysis column output

Component Weight% Mass flow rate(kg/h)

SBA 56.33 1500

Water 4.91 130.497

SBE 0.92 24.576

Acid 0.059 1.578

Butene 0.198 5.283

Spent acid 37.108 987.985

i-pentanol 0.469 12.51

Total 2662.429

36
3.8 NEUTRALIZATION COLUMN:

Input:

Table 3.18 Neutralization column input

Component Weight% Mass flow rate

SBA 80.56 1500

Water 7.00 130.497

SBE 1.319 24.576

Acid 0.0847 1.578

Butene 0.2837 5.283

i-pentanol 0.671 12.51

Caustic 10.07 187.5

Total 1861.944

Top output:

Table 3.19 Neutralisation column top output

Component Weight% Mass flow rate(kg/h)

SBA 89.66 1500

Water 7.80 130.497

SBE 1.469 24.576

37
 Butene 0.315 5.283

i-pentanol 0.747 12.51

Total 1672.866

Bottom output:

Table 3.20 Neutralization column bottom output

Component Weight% Mass flow rate(kg/h)

WASTE 100 189.078

3.9 SBE-WATER COLUMN:

Input:

Table 3.21 SBE-Water column input

Component Weight% Mass flow rate(kg/h)

SBA 89.95 1500

Water 7.82 130.497

SBE 1.473 24.576

i-pentanol 0.75 12.51

Total 1667.583

38
Distillate:

Table 3.22 SBE-Water column distillate

Component Weight% Mass flow rate(kg/h)

SBA 89.07 1264.725

SBE 1.73 24.576

Water 9.19 130.497

Total 1419.79

Bottom product:

Table 3.23 SBE-Water column bottom product

Component Weight% Mass flow rate(kg/h)

SBA 94.9 235.25

Heavies 5.04 12.51

Total 247.76

3.10 ACCUMULATOR 1:

Input:

Table 3.24 Accumulator 1 input

Component Weight% Mass flow rate(kg/h)

SBA 89.07 1264.735

39
 SBE 1.73 24.576

Water 9.19 130.497

Total 1419.79

Top output:

Table 3.25 Accumulator 1 top output

Component Weight% Mass flow rate(kg/h)

SBA 96.62 963.86

SBE 2.46 24.576

Water 0.906 9.0435

Total 997.4825

Bottom output:

Table 3.26 Accumulator 1 bottom output

Component Weight% Mass flow rate(kg/h)

SBA 71.24 300.89

Water 28.75 121.4535

Total 422.3435

40
3.11 SBA RETURN COLUMN:

Input:

Table 3.27 SBA Return column input

Component Weight% Mass flow rate(kg/h)

SBA 94.94 235.25

Heavies 5.04 12.51

Total 247.76

Distillate:

Table 3.28 SBA Return column distillate

Component Weight% Mass flow rate(kg/h)

SBA 99.92 230.765

Heavies 0.017 0.165

Total 230.93

Bottom product:

Table 2.29 SBA Return column bottom product

Component Weight% Mass flow rate(kg/h)

SBA 26.64 4.485

Heavies 73.35 12.345

41
 Total 16.85

3.12 SBA HEAVIES COLUMN:

Input:

Table 3.30 SBA-Heavies column input

Component Weight% Mass flow rate(kg/h)

SBA 26.64 4.485

Heavies 73.75 12.345

Total 16.85

Distillate:

Table 3.31 SBA-Heavies column distillate

Component Weight% Mass flow rate(kg/h)

SBA 99.89 4.485

Heavies 0.106 0.00485

Total 4.4898

42
Bottom product:

Table 3.32 SBA-Heavies column bottom product

Component Weight% Mass flow rate(kg/h)

Heavies 100 12.3402

3.13 ALCOHOL EXTRACTION COLUMN:

Input:

Table 3.33 Alcohol extraction column input

Component Weight% Mass flow rate(kg/h)

SBA 82.77 963.86

SBE 21.1 24.576

Water 15.11 175.95

Total 1164.389

Top product:

Table 3.34 Alcohol extraction column top product

Component Weight% Mass flow rate(kg/h)

SBE 93.12 24.576

Water 6.87 1.815

Total 26.394

43
Bottom product:

Table 3.35 Alcohol extraction column bottom product

Component Weight% Mass flow rate(kg/h)

SBA 84.69 963.86

Water 15.30 174.135

Total 1137.995

3.14 ACCUMULATOR 2:

Input:

Table 3.36 Accumulator 2 output

Component Weight% Mass flow rate(kg/h)

SBA 81.05 1264.75

Water 18.4 295.5885

Total 1560.33

3.15 SBA STRIPPING COLUMN:

Input:

Table 3.37 SBA stripping column input

Component Weight% Mass flow rate(kg/h)

SBA 81.05 1264.75

44
 Water 18.94 29.5885

Total 1560.33

Top product:

Table 3.38 SBA stripping column top product

Component Weight% Mass flow rate(kg/h)

SBA 92.60 1264.75

Water 7.35 100.9885

Total 1365.7385

Bottom product:

Table 3.39 SBA stripping column bottom product

Component Weight% Mass flow rate(kg/h)

Water 100 194.6

Input from the Reaction = Output from the Reactor

45
 CHAPTER 4

ENERGY BALANCE

4.1 1st STAGE REACTOR:

C4H7-OSO3 + CH3CH=CHCH3 C4 H9-SO4 -C4H9

(monobutyl ester) (butane) (DIbutyl ester)

Inlet temperature =35 oC

Outlet temperature =50oC

Reference temperature =25OC

Input:
Table 4.1 1st stage reactor input
Component Mass flow Specific heat ΔT Q(KJ/h)
rate(kg/h) Capacity
(KJ/KgoK)
Butane 708.4 0.083 10 587.92
Acid rich 1950.63 1.42 10 27698.946
Ester

Total 28286.866

Output:

Table 4.2 1st stage reactor output

Component Mass flow Specific heat capacity ΔT Q(KJ/h)

rate(kg/h) (KJ/KgoK)

UR butane 73.656 0.083 25 152.83

46
 Butane 2.32 25 5406.093
93.2085
Polymer 2.152 25 873.174
16.23
Ester 0.288 25 15320.34
2127.825
Water 4.186 25 17206.03
164.415
Sulphuric acid 1.42 25 6019.06
169.551
Dissolved 0.83 25 293.571
14.148
Butene
Total 45271.20

Q reaction = outlet heat – inlet heat = 45271.2 – 28286.866

=16984.35 KJ/h

Cooling water requirement:

Water inlet temperature: 303 K

Water outlet temperature: 313K

Q = m*Cp*ΔT

m = Q/Cp*ΔT

m = 405.9 Kg/h

4.2 2ND STAGE REACTOR:

CH3CH=CHCH3+H2SO C4H7-OSO3H

4 (Butene) (Monobutyl ester)

Inlet temperature = 43oC

Outlet temperature = 55oC
47
Reference temperature = 25oC

Input:

Table 4.3 2nd stage reactor input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

Butane 93.2085 2.32 18 3892.366

Polymer 16.23 2.152 18 628.68

Fresh acid 1323.975 1.42 18 33840.8

Total 38471.886

Table 4.4 2nd stage reactor output

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

Butane 93.2085 2.32 30 6487.4

Polymer 16.98 2.152 30 1096.22

Acid 11.7645 1.42 30 501.14

Acid rich 1950.63 0.82 30 47985.4

ester

48
 UR butane 29.4825 0.083 30 73.41

Total 56143.5

Q reaction =outlet heat-inlet heat = 56143.5 - 38471.886

=17671.614 KJ/h

Cooling water requirement

Water inlet temperature: 305K

Water outlet temperature: 318K

Q=m*Cp*∆T

m=Q/Cp*∆T

m=324.738 Kg/h

4.3 BUTANE WASH COLUMN:

Inlet temperature =65OC

Outlet temperature =45OC

Reference =25OC
temperature Input:

Table 4.5 Butane wash column input

ComponentMass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

Butane 93.2085 2.32 40 8649.75

49
 Polymer 16.98 2.252 40 1461.63

Acid 11.7645 1.42 40 668.224

UR butane 29.482 0.082 40 97.78

Water 188.67 4.186 40 31545.624

Total 42423.005

Outlet:

Table 4.6 Butane wash column output

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) Capacity
(KJ/Kg oK)

Butane 93.2085 2.32 20 4323.87

Polymer 16.98 2.252 20 730.81

UR butane 29.482 0.082 20 48.88

Wash water 200.358 4.186 20 16749.92

Total 340.11 21854.498

Q reaction = outlet heat – inlet heat =21854.498 – 42423

= -20568.502 KJ/h

Heat inlet + heat added = heat outlet

42423 – 20568.502 = 21854.498

Heat input = Heat output

50
4.4 PREHYDROLYSIS COLUMN:

Inlet temperature = 50O

Outlet temperature = 65OC

Reference temperature = 25OC

Inlet:

Table 4.7 Prehydrolysis column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h)(KJ/Kg oK)

Ester 2127.825 0.228 25 12128.6

Wash water 364.77 4.186 25 38154.94

Sulphuric acid 169.551 1.42 25 6019.06

Dissolved 14.14 0.083 25 29.34

butane

Total 56331.94

Outlet:

Table 4.8 Prehydrolysis column output

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity
(KJ/Kg oK)
Ester 2127.825 0.228 40 19405.764

Wash water 364.77 4.186 40 60989.544

51
 Sulphuric acid 169.551 1.42 40 9630.49

Dissolved butane 5.2283 0.083 40 17.54

Escaped butene 8.857 0.083 40 29.41

Total 90072.74

Q reaction + outlet heat – inlet heat = 90072.74 – 56331.74

= 33740.8 KJ/h

Heat inlet + heat added = heat output

56331.74 + 33740.8 = 90072.74

Heat input = Heat output

4.5 HYDROLYSIS COLUMN:

C4H9-SO4-C4H9 + 2H2O 2CH3-CH2-CH(OH)-CH3 + H2SO4

(Dibutyl ester) (Secondary-Butyl Alcohol)

Inlet temperature = 65OC

Outlet temperature = 42OC
Bottom temperature = 14OC

Reference temperature
= 25OC

Input:

Table 4.9 Hydrolysis column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

52
 Ester 2127.825 0.228 40 19405.76
Water 364.97 4.18 40 60989.54
Sulphuric 169.551 1.42 40 9630.49
acid
Dissolved 5.283 0.083 40 17.54
butene

Total 90043.33

Output:

Table 4.10 Hydrolysis column output

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity

(KJ/Kg oK)

SBA 1500 0.184 17 4692

Water 130.497 4.186 17 9273.11

SBE 24.576 2.212 17 924.16

Acid 1.578 1.42 17 38.09

Butane 5.283 0.083 17 7.454

Spent acid 987.985 1.42 115 161337.78

i-pentanol 12.51 1.32 17 280.72

Total 176553.32

53
Q reaction = outlet heat – inlet heat = 176553.32 – 90043.33

=86509.9 KJ/h

Heat inlet + heat added = heat outlet

90043.33 + 86509.9 = 176553.32
Heat input = Heat output

4.6 NUTRALISATION COLUMN:

Inlet temperature = 107oC
Top temperature = 91OC
Bottom temperature = 160OC
Reference temperation = 25oC

Input:
Table 4.11 Nutralisation column
input
Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity

(KJ/Kg oK)

SBA 1500 0.184 82 22632

Water 130.497 4.186 82 44729.15

SBE 24.576 2.212 82 4457.7

Acid 1.578 1.42 82 183.74

Butene 5.283 0.083 82 35.96

i-pentanol 12.51 1.32 82 1354

 Caustic 187.5 0.028 82 430.5

Total 1861.944 73823.05

Output:

Table 4.12 Neutralization column input

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity

(KJ/Kg oK)

SBA 1500 0.184 66 18216

Water 130.497 4.18 66 36001.5

SBE 24.579 2.212 66 3587.9

Butene 5.283 0.083 66 28.94

i-pentanol 12.51 1.32 66 1089.87

Waste 189.078 0.032 66 399.33

Total 59323.55

Q reaction = outlet heat – inlet heat = 59323.55 – 73923.05

= -14499.497 KJ/h

Heat inlet + heat added = heat outlet

73923.05 – 14499.497 = 59323.55

Heat input = Heat output

4.7 SBE WATER COLUMN:

Inlet temperature Top = 50OC

temperature Bottom = 90.1OC

temperature Reference = 110OC

temperature Input: = 25OC

Table 4.13 SBE Water column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBA 1500 1500 25 6900

Water 130.497 130.5 25 13656.5

SBE 24.576 24.576 25 1359.05

i-pentanol 12.51 12.51 25 412.83

Total 1667.583 22328.38

Distillate:

Table 4.14 SBE Water column distillate

Component Mass Specific heat ∆T Q(KJ/h)
capacity
Flowrate(kg/h) (KJ/Kg oK)

SBA 1264.725 0.184 65.1 15149.4

56
 SBE 24.576 2.212 65.1 3538.97

Water 130.497 4.186 65.1 35561.6

Total 1419.79 54249.97

Bottom product:

Table 4.15 SBE Water column bottom product

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity

(KJ/Kg oK)

SBA 235.25 0.184 85 3679.31

Heavies 12.51 1.32 85 1403.622

Total 247.76 5082.932

Heat load in condenser:

M = 24.525 kmol/hr

λ = 40 KJ/h

Q = mλ

= 24.525*40*1000

= 981000 KJ/h

Cooling water requirement:

Q = mCp∆T

57
 m = Q/Cp*∆T

= 981000/4.18*(40-35)

= 46937.8 Kg/h

Heat load in Condenser:

Heat load in reboiler = heat load in condenser + heat in bottom

+ heat in distillate – heat in feed

= 981000 + 5082.932 + 54249.97 – 22328.38

= 1018004.5 KJ/h

Steam requirement:

λ = 2001.68KJ/kg

Q = mλ

m = Q/λ

= 1018004.5/2001.68

= 508.57 kg/h

4.8 SBA RETURN COLUMN:

Inlet temperature = 108OC

Top temperature = 104OC

Bottom temperature = 110.7OC

Reference temperature = 25OC

Input:

Table 4.16 SBA column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBA 235.25 0.184 83 3592.738

Heavies 12.51 1.32 83 1370.5956

Total 4963.33

Distillate:

Table 4.17 SBA Return column distillate

Component Mass Specific heat ∆T Q(KJ/h)
Flowrate(kg/h) capacity
(KJ/Kg oK)

SBA 230.765 0.184 79 3354.4

Heavies 0.165 1.32 79 17.2062

Total 3371.6

Bottom product:

Table 4.18 SBA Return column bottom product

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

59
 SBA 4.485 0.184 85.7 70.723

Heavies 12.345 1.32 85.7 1396.51

Total 1467.24

Heat load in Condenser:

m = 4.5 kmol/h

λ = 40 KJ/h

Q = mλ

= 4.5*40*1000

= 183375 KJ/h

=183375/4.18* (40-35)

=874.35 Kg/h

Heat load in condenser:

Heat load in reboiler = heat load in condenser + heat in bottom

+ heat in distillate – heat in feed

= 183375 + 3371.6 + 1367.24 – 4963.33

= 183250.5 KJ/h
Steam requirement:

λ = 2001.68KJ/kg

Q = mλ

m = Q/λ

= 183250.5 / 2001.68

= 91.54 kg/h

4.9 HEAVIES COLUMN:

Inlet temperature = 108OC

Top temperature = 104OC

Bottom temperature = 110.7OC

Reference temperature = 25OC

Input:

Table 4.19 Heavies column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBA 4.485 0.184 90 74.2726

Heavies 12.345 1.32 90 1466.6

Total 1540.86
Distillate:

Table 4.20 Heavies column distillate

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBA 4.485 0.184 83.5 68.9

Heavies 0.0048 1.32 83.5 0.529

Total 69.43

Bottom product:

Table 4.21 Heavies column bottom product

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

Heavies 12.34 1.32 122.6 1997.04

Q reaction = outlet heat – inlet heat = 2066.47 – 1540.86

= 535.6KJ/h

Heat inlet + Heat added = Heat outlet

1540.86 + 525.6 = 2066.47

Heat input = Heat output

4.10 ALCOHOL EXTRACTION COLUMN:

Inlet temperature = 90OC

Outlet temperature = 45OC

Reference temperature = 25OC

Input:

Table 4.2.2 Alcohol extraction column input

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBA 963.86 0.184 65 11527.76

SBE 24.576 2.212 65 3533.96

Water 175.95 4.186 65 47874.24

Total 1164.389 62935.96

Top product:

Table 4.23 Alcohol extraction top product

Component Mass Specific heat ∆T Q(KJ/h)
capacity
Flowrate(kg/h) (KJ/Kg oK)

SBE 24.576 2.212 20 1087.12

Water 1.815 4.186 20 151.95

Total 26.394 1239.37

Bottom product:

Table 4.24 Alcohol extraction column bottom product

Component Mass Specific heat capacity ∆T Q(KJ/h)

Flowrate(kg/h) (KJ/Kg oK)

SBE 963.86 0.184 20 3547

Water 174.135 4.186 20 14578.58

Total 1137.995 18125.58

Q reaction =outlet heat- inlet heat =19364.9-62935.96

Q =-43571 KJ/h

Heat Inlet + Heat Added = Heat Added

62935.96-43517=19364.9

Heat Input =Heat Output

 CHAPTER 5

DESIGHN OF EQUIPMENTS

5.1 DESIGHN OF DISTILLATION COLUMN

SBA Vs Heavies

Table 5.1 SBA vs Heavies dates

SBA Heavies
Antoine equation Antoine equation

Log PA=A-[B/(T+C)] Log PA=A-[B/(T+C)]

A=7.4743 A=7.6873

B=1314.19 B=137.18

C=186.51 C=137.18

Boiling point =99.5 OC Boiling point = 150 OC

5.1.1 McCabe Thiele Method

Generation of vapour liquid equilibrium data

X= (Pt-PB)/(PA-PB)

Y= (PAX/Pt)

Table 5.2 Equilibrium data

TOC PA mm Hg PB mm Hg Relative X Y
volatility
99.5
760 71.5 2.61 1 1

65
 104.5 908.5 94.5 3.02 .9536 .998

109.5 1082.92 123.38 2.57 0.758 .868

114.5 1238.41 159.38 2.48 .653 .795

119.6 1512.52 203.835 2.39 .551 .7125

124.5 1773.15 258.835 2.31 .419 .62

129.5 3056.25 234.30 2.24 .354547 .5162

134.5 2400 403.84 2.16 .3547 .5162

139.5 2774.38 498.92 2.11 .259 .3994

144.5 3191.96 611.78 2.05 .1656 .270

150 3706.36 760 2.8 0 0

Average α value: 2.43

The high α value clearly states that impurities can be easily distillate from
the product

Mole fraction of feed, distillate and product are given by,

XF = 0.6

XD = 0.99

XB = 0.045

To find the intercept

Y=XD/(R+1)

Given Reflux ratio = 2.3

Now Y=0.99/3.3

Y=0.30
GRAPH ;

Fig 5.1 McCabe thiele Method

67
From the graph:

No. of theoretical stages=13

5.1.2 Binary Distillation Sieve Tray Efficiency:

Connell’s Equation is used to find the column efficiency

E=0.492(α*µf)-0.245

Where, α is used to find the column efficiency

µf is viscosity relative volatility

µf=0.492 cp

E=0.375

5.1.3 Number of actual stages

No. of actual plates = 13/0.375

No. of actual plates = 34

Total no. of plates = 34+1=35

5.1.4 Calculation of Column height

Tray spacing is given as 0.5m

Height = no. of trays * Trays spacing

=35*0.5

=17.5 m

68
 5.1.5 Top section

Average molecular weight = 1218.675/16.4718

Mavg=73.99

5.1.5.1 Flooding velocity

The flooding velocity through sieve tray tower can be determine by the
following equation

Uc = Kv ((ρL- ρv)/ ρv)0.5(σ/0.02)0.2

Where ρL = Density of liquid phase = 799 kg/m3

Pv = Density of the vapour phase = 2.36

Kg/m3
σ = Surface tension of liquid = 0.055
N/m3
Kv = Sieve plate empirical constant
The value of Kv is calculated from standard plot of Kv vs F-factor F-

factor is calculated by the following equation

F = (L/V)(ρL/ρv)0.5

Where L= liquid flow rate = R*D= 2.3*16.4718

L= 37.885 kmol/hr

V= Vapour flow rate = (D*(R+1) =

3.3*16.4718 V= 54.35694 kmol/hr

F= (37.885/54.35694)(2.36/799)0.5

= 0.037

Assuming tray spacing = 0.45 m

For F= 0.037 and tray spacing = 0.45 m

Kv = 0.08

Flooding velocity, Uf = 0.08((799-2.36)/2.36)0.5(0.055/0.2)0.2

= 1.7994 m/s

5.1.5.2 Actual vapour velocity

Actual vapour velocity = 0.85*Flooding velocity

= 0.85*1.7994

Actual vapour velocity = 1.5295 m/s

5.1.5.3 Vapour volumetric flow rates

The volumetric flow rate of vapour at the top is given by

Qtop = (V*Mavg/ρv)

= (54.34694*73.985)/2.36

= 1704.07 m3/hr

5.1.5.4 Bubbling area

Bubbling area = Vapour volumetric flow rate / Actual vapour velocity

= 0.47335/1.52949

Bubbling area = 0.30948 m2

5.1.5.5 Cross sectional area of the top section

The bubbling area is 0.7 times the cross sectional area

Cross sectional area = 0.30948/0.7

Cross sectional area = 0.4421 m2

70
5.1.5.6 Column diameter

Dtop = (4* cross sectional /π )0.5

= (4*0.4421/ 3.14)0.5

= 0.750475 m

5.1.6.1 Flooding velocity

The flooding velocity through sieve tray tower can be determine by the

following equation.

Where ρL = Density of the liquid phase = 721 Kg/m3

ρv = Density of the vapour phase = 3.31 kg/m3

σ = Surface tension of the liquid = 0.043 N/m

Kv= Sieve plate empirical constant

The value of Kv is calculated from the standard plot of K v vs F-factor

F-factor is calculated by the following equation

F= (L/V)(ρI /ρL)0.5

Where L= liquid flow rate = R*B = 2.3 *0.7456

L= 1.71488 kmol/hr

V= Vapour flow rate = B*(R+1) = 3.3 * 0.7456

 V=2.46048 kmol/ hr

F= (1.71488/2.46048)(3.21/721)0.5

= 0.0465

Assuming tray spacing = 0.45m

For F= 0.0465and tray spacing = 0.45

m Kv= 0.08

Flooding velocity, Uf = 0.08 ((721-3.21)/3.21)0.5(0.043/0.02)0.2

= 1.3942 m/s

5.1.6.2 Actual vapour velocity

Actual vapour velocity = 0.85* Flooding velocity

= 0.85* 1.3942

Actual vapour velocity =1.1851 m/s

5.1.6.3 Vapour volumetric flow rates

The volumetric flow rate of vapour at the top is given by

Qtop = (V*Mavg/ρv)

=(2.46048*79.945)/3.21

=61.28 m3/hr

Bubbling area = vapour volumetric flow rate / Actual vapour velocity

= 0.01702/1.1851

Bubbling area = 0.01436 m2

72
5.1.6.5 Cross sectional area of the bottom selection

The bubbling section area is 0.7 times the cross sectional area

Cross sectional area = 0.01436/0.7

Cross sectional area = 0.02052 m2

5.1.6.6 Column diameter

Dtop = (4*cross sectional area /π )0.5

= (4*0.02052/3.14)0.5

= 0.1616 m

5.1.7 Provisional plate design

Column diameter D = 0.750475

Column area A = 0.4421 m2

5.1.7.1 Down comer area

Ad = 0.12*A

= 0.12 * 0.4421

=0.053052 m2

5.1.7.2 Net area of the column

An = A-Ad

= 0.4421-0.053052

=0.389048 m2

5.1.7.3 Active Area

Aa = A-(2*Ad)

= 0.4421 – (2*0.053052)

73
 =0.336 m2

5.1.7.4 Hole Area

Ah = 0.074*Aa

= 0.074*0.336

= 0.0249 m3

5.1.7.5 Weir length

Lw = 0.77 D

= 0.77 *0.750475

Lw = 0.5779 m

5.1.8 Design Summary

Table 5.3 design summary

Total number of trays 35

Height of the column 17.5 m

Column diameter 0.750475 m

Area of the column 0.4421 m

Weir length 0.5779 m

 CHAPTER 6

PROCESS ECONOMICS

6.1 COST ESTIMATION

Specification

Basis: 1500 kg/hr of secondary butyl alcohol

No of working days per year = 300 days

Production of SBA per year = 10,800,000 kg

Cost of SBA per kg = Rs. 90

So, gross sale of one more year = 10800000 *90

= Rs.972000000

Turnover ratio = gross annual sales/ fixed capital

investment For a chemical industry,

Turnover ratio = 1

So, gross annual sales = fixed capital investments

Therefore fixed capital investment = Rs. 972000000

Fixed capital investment cost = Direct cost + Indirect cost

6.2 DIRECT COST

It is 70% of fixed capital investment

Direct cost = 972000000 * 0.7

= Rs. 68040000
 It consists of,
Equipment

Installation

Piping

Insulation

Painting

6.2.1 Equipment cost

It is 34.5% of fixed capital

Therefore equipment cost = 972000000 * 0.345

= Rs. 335340000

6.2.2 Land cost

It is 1% of fixed capital

Therefore land cost = 972000000 * 0.01

= Rs. 9720000

6.2.3 Instrument and installation cost

These cost account to 20% of the equipment cost

= 335340000 * 0.2

= Rs. 67068000

6.2.4 Electrical and instrument cost

These cost accounts to 29% of the equipment cost

= 335340000 * 0.29

= Rs. 97248600

76
6.2.5 Building, Process and Auxiliary
costs

These costs account to 31% of the equipment cost

= 335340000 * 0.31

= Rs. 103955400

6.2.6 Service facilities and Yard improvement

This cost is 20% of equipment cost

= 335340000 * 0.20

= Rs. 67068000

6.3 INDIRECT COST

These are expenses which are not including with material and labour of
actual installation of complete facilities. This account for 30% of fixed capital
investment
= 0.3 * 972000000

= Rs. 291600000

The indirect cost consists of

Engineering supervision
Construction expenses and construction fees

Contingency

6.3.1 Engineering supervision

It is 20% of the fixed capital investment

= 0.2 * 972000000

= Rs. 194400000
6.3.2 Construction expense and construction fees

It is 5% of fixed capital investment

= 0.05 * 9724000000

= Rs. 48600000

6.3.3 Contingency

It is 5% of fixed capital investment

= 0.05 * 972000000

= Rs. 48600000

6.4 ESTIMATION OF TOTAL PRODUCTION COST

Total annual income = Rs. 972000000

Total gross earning = 15% of total income

= 0.15 * 972000000

= Rs. 145800000

6.4.1 Production cost

Production cost = total annual income – gross earning

= 972000000 – 145800000

= Rs. 826200000

Total production cost= Direct production cost +fixed charges

+plant overhead

6.4.2 Direct Production Cost

It is 75% of total production cost

= 0.75 * 826200000
 = Rs. 619650000

6.4.3 Raw Material Cost

Cost of Butene for 5478 kg = Rs. 62055000

Cost of sulphuric acid for 10152.95 = Rs. 41370000

Total = 62055000 – 41370000

= Rs. 1034250000

6.4.4 Operating labor cost

It is 15% of total production cost,

= 826200000 * 0.15

= Rs. 123930000

6.4.5 Direct supervisory and clinical cost

It is 5% of the total production cost,

= 826200000 * 0.05

= Rs. 41310000

6.5 UTILITIES

6.5.1 Maintenance and Repair cost

It is 8% of total production cost,

= 0.08 * 826200000

= Rs. 66096000

6.5.2 Patents and Royalties Cost

79
 it is 8% of total production cost,

= 0.08 * 826200000

= Rs. 66096000

= 0.2 * 826200000

= Rs. 165240000

6.5.4 Plant Overheads

This includes cost for following general plant and overheads payroll.

Overheads packing, medical services, safety and protection, restaurant,

recreation, salvage, laboratories and storage facilities.

This cost is 5% of production cost,

= 0.05 * 826200000

= Rs. 41310000

Depreciation for machinery is 10% of the fixed capital cost

= 0.15 * 826200000

= Rs. 145800000

= 0.03 * 972000000

= Rs. 29160000

Total depreciation = Rs. 174960000

80
6.5.6 Insurance

It is 1% of fixed capital cost

=0.01 * 972000000

= Rs. 9720000

6.5.7 General Expenses

Administrative cost includes cost for excecutive offices, clinical

wages, legal fees, office supplies and communication.

It is 5% of total production cost

= 0.05 * 826200000

= Rs. 41310000

6.5.8 Distribution and Selling cost

It include cost for sales officers, sales men and shipping

It is 7% of total production cost

= 0.07 * 826200000

= Rs. 41310000

6.5.8 Research and Development

This cost 1% of production of cost,

= 0.01 * 826200000

= Rs. 8262000

81
6.5.10 Financing

It is 2% of total production cost,

=0.02 * 826200000

= Rs. 16524000

6.6 PAYBACK PERIOD

6.6.1 Gross Earning Cost

It is the net profit obtained after deduction of tax from goods earning

Tax payable = 30% of gross profit

= 0.3 * 826200000

= Rs. 247860000

6.6.2 Net Profit

Net profit = Gross - tax

= 826200000 - 247860000

= Rs. 9130909

Payback period = Depreciated fixed capital investment/(Annual profit +

Average depreciation)/ year

= 972000000 / (9130909 + 1749600)

= 5.28 years

Payback period = 5 years 120 days

 CHAPTER 7

PLANT SAFETY

7.1 PROCESS SAFETY

All plant personnel shall comply with normal safety rules which generally
apply on all the petrochemical plants. Chiefs shall strictly enforced all
applicable safety regulations to safeguard personnel and equipment under there
change.
 All personnel employed in the plant should become acquainted
with the dangers of chemical poisoning and recommended
measures for such emergencies. This is also not necessary for each
person or visiting within the fenced in area of the plant.
 In addition they have to be possession of a valid permanent or
temporary company identification card which is to be carried
constantly and shown on request while within the fence limits.
Entering and leaving is permitted though the main gate guards.
 Within the entire area of the plant there is strictly no smoking.
People who have consumed alcohol or other intoxicants are to
leave the plants under proper guidance immediately. Matches,
lighters and cigarettes are to be deposited with the man at the gate.
 Within the plant limits the Tamil Nadu regulations apply. Right of
way at intersections has the vehicle coming from the left.
 Cars shall not be parked on pit-covers or in front of fire hydrants.
Parking is generally allowed only on marked parking area or places
specially allocated to the drivers.
 Personnel is strongly advised to be dressed in accordance with
safety requirements.

83
7.2 FIRE SITUATION

Leaks and flammable liquid spills are potential fires require emergency action from

the operator, on learning of the leak or spill, the operator,

Alert the supervisor for possible shut down

If the location of leak is known, shut down the affected system, isolate the
section of pipe or equipment which has failed. In acid and caustic service,
maintenance man and supervisors must wear safety dress with eye
protection
If source of leaking is not known, shut down the system in the affected
area until location of source has been determined
Notify maintenance super intendant and plant super intendant
The maintenance crew shall be careful to adhere to the procedure
established for doing emergency work

7.3 TYPES OF FIRE

Fuel, oxygen and ignition heat be present to start and sustain the fire. If

any of these three factor is removed, burning stops.

7.3.1 Class A

Fires of ordinary combustible materials as wood, paper and rubbish are

most effectively extinguished with water. The quenching effect reduces heat to
less than ignition temperature.
7.3.2 Class B

Fires of flammable liquids, oil, greases and paints require blanketing

effect to cut off the supply of oxygen. This is done with a dry chemical

extinguisher or with foam.

 If alcohol and ketones are burning in large fires also nebulized water and
alcohol resistant foam can be used. All equipment to be used for generating foam
be designed by the engineering contractors.

7.3.3 Class C

A fire originating at electrical equipment like motors, transformers, circuits,

breakers, cables, electric boards etc. Must be extinguished by smothering with non-
conductive substances. Recommended is dry powder, carbon dioxide, chlorinated or
fluorinated hydrocarbons filled in extinguishers, which can be directly used on still
energized equipment.

Normally do not use water or foam. Only when the electrical department

confirms that all equipment in the emergency area has been de-energized, the

use of nebulized water or foam will be possible even when the fire is feeding on

the oil transforms.

7.4 CHEMICAL HAZARD PRECAUTIONS:

7.4.1 Methyl Ethyl Ketone (MEK)

MEK is colourless liquid with sweet and aromatic colour. The liquid
evaporates quickly, is combustible and partly miscible with water. Rubber and several
plastic materials will be attacked by the MEK and vapours. Liquid and are an irritant
for eyes and skin. Inhalation of vapours in high concentration for long time causes
narcotic reaction. For short time (about 30min) 0.3% MEK vapour content in air is
tolerable. Maximum permanent allowable concentration is 200ppm.
In case of Poisoning, the person must be brought into fresh air and soiled cloths taken off.

If the eyes are also contaminated, flushing with water for about

85
15mins is indispensable. In any case physician should be called, especially
when MEK is swallowed.

MEK vapours mixed with air are explosive within 1.5 to 11.4% volume

MEK content and the ignition temperature is 515°C.

Although MEK is miscible with water, formation of explosive and narcotic mixtures

above the surface is possible. Hence care should be taken not to pour out the MEK but also

with the open mixtures of MEK and water.

7.4.2 Secondary Butyl Alcohol (SBA)

This liquid is also an irritant to eyes and skin with effect comparable of MEK

maximum permanent allowable concentration is 500ppm,

7.4.3 Hydrogen

Hydrogen is colourless gas without colour. Lower density than air and
have no poisonous qualities.
With air, highly explosive mixtures are formed (oxyhydrogen gas) and the

concentration range is 4-75% volume hydrogen in air. Forming of such mixers must be

prevented especially in edges and beyond ceilings.

7.4.4 Caustic Soda Solution (NaOH)

Caustic soda is a colourless, viscous liquid not combustible but it has a deleterious

effect to skin, mucous membranes and especially to eyes. Maximum permanent allowable

concentration is 2 mg/m3. In case of poisoning, the person must be brought into fresh air

and solid clothes taken off. Contacted parts on the need to be flushed thoroughly

especially the eyes not less than 15 mins. In any case a physician should be called.
7.4.5 Sulphuric Acid

Sulphuric acid is a colourless, oily liquid not combustile but it has deleterious

effect to skin and eyes. Concentrated acid spilled on wood, cotton or paper cause a

rapid reaction, heat and coke formation with possible fire maximum permanent

allowable concentration is 1 mg/m3.

In case of poisoning the person should be attended described for NaOH.

Sulphuric acid is totally miscible with water. If spilled or contacted to water a

rapid reaction with heat formation will follow. Acid water solutions have in a wide range

deleterious effect to skin and are corrosive.

For safety equipment, one body-shower shall be installed between C-103

and C-104 and one may be installed close to the loading facilities. Eye-showers

shall be on body showers also and distributed in critical areas as well as in control

rooms and laboratory.

7.5 ACCIDENTAL RELEASE MEASURES

7.5.1 Small Spill

Dilute with water and mop up, or absorb with an inert dry material and

place in an appropriate waste disposal container

7.5.2 Large Spill

Flammable liquid. Keep away from heat. Keep away from sources of ignition.

Stop leak if without risk. Absorb with dry earth, sand or other non-combustible material.

Do not touch spilled material. Prevent entry into sewers, present at a concentration level

above threshold Limit Value.

87
 CHAPTER 8

CONCLUSION

The project gives the detailed discussion of synthesis and purification of

secondary butyl alcohol.
The condenser design has 1400mm shell diameter with 116 tubes of 25mm OD*

20mm* 3m long and also has a triangural pitch of 21.75mm.

The actual area required for the condenser is 19.25 m2.

The distillation has a design with height 17.5m, number of plates 35,

column diameter 0.750475m and plate efficiency of 37.5%.

A detailed work of material balance and energy balance were carried out

for various equipment in the industry.

 CHAPTER 9

REFERENCES

1. Perry, R.H and D. GREEN, eds.; Perry's Chemical

Engineering Handbook 6th ed.'Mc Graw Hill, New York, 1984

2. George T. Austin; 5th ed.' "Shreve's Chemical Process Industries"

3. Couston, J.M and Richardson J.F; 6th ed.'Fluid Flow, Heat Transfer
and Mass Transfer-Volume 1, B.H.
4. Sinnot R.K., 3rd ed., Chemical Engineering Design-Volume 6, B.H.

5. Harry Silla; 2nd ed., 'Chemical Process Engineering Design

and Economics', Marcel Dekker Inc., New York, 2003.

6. Warren Lee McCabe, Julian Smith and Peter Harriot; 7th ed., "Unit Operations of

Chemical Engineering@, Mc Graw Hill, New YORK, 1956.