Linear Alkyl Benzene Sulfonic Acid

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The project report discusses research on manufacturing linear alkyl benzene sulphonic acid and researching waste plastic pyrolysis.

The project report discusses research conducted on manufacturing linear alkyl benzene sulphonic acid and researching waste plastic pyrolysis as a means to produce fuel from plastic waste.

The objectives of the research were to develop a simple catalytic and non-catalytic process for depolymerising waste plastics into synthetic crude oil and to characterize the properties of the produced oil.

MANUFACTURE OF LINEAR ALKYL BENZENE SULPHONIC ACID

&
RESEARCH ON WASTE PLASTIC PYROLYSIS

A PROJECT REPORT

Submitted by

PRABHU S
(Reg.No.:810015239033)

In partial fulfillment for the award of the degree


of

BACHELOR OF TECHNOLOGY

In
PETROCHEMICAL TECHNOLOGY

UNIVERSITY COLLEGE OF ENGINEERING


BIT CAMPUS, ANNA UNIVERSITY
TIRUCHIRAPALLI - 620 024

ANNA UNIVERSITY: CHENNAI 600 025


APRIL 2019
BONAFIDE CERTIFICATE

Certified that this project report “MANUFACTURE OF LINEAR ALKYL BENZENE


SULPHONIC ACID” & “RESEARCH ON WASTE PLASTIC PYROLYSIS” is the bonafide

work of “PRABHU S (Reg.No.810015239033)” who carried out the project work


under my supervision.

SIGNATURE SIGNATURE
Dr. M. ARULMOZHI, M.E., Ph.D, Mrs. K. ANBARASI, M.Tech.,
HEAD OF THE DEPARTMENT ASSISTANT PROFESSOR,
Department of Petrochemical Technology Department of Petrochemical Technology
University College of Engineering University College of Engineering
BIT Campus, Anna University, BIT Campus, Anna University,
Tiruchirapalli-620024. Tiruchirapalli-620024.

Examined on:

INTERNAL EXAMINER EXTERNAL EXAMINER


DECLARATION

I hereby declare that the work entitled “MANUFACTURE OF LINEAR ALKYL BENZENE
SULPHONIC ACID” & “RESEARCH ON WASTE PLASTIC PYROLYSIS” is submitted in
partial fulfillment of the requirement of the degree in B.Tech. Anna university Tiruchirapalli , is a
record of the my own work carried out by me during the academic year 2015-2019 under the
supervision and guidance of Mrs. K. ANBARASI, M.Tech, Department of petrochemical technology,
Anna university BIT campus Tiruchirapalli. The extent and source of information are derived from the
existing literature and have been indicated through the dissertation at the appropriate places. The
matter embodied in this work is original and has not been for the award of any other degree or
diploma, either in this or any other university.

(Signature of the Candidate)


PRABHU S
Reg.No.810015239033

I certify that the declaration made by the above candidate is true.

(Signature of the Guide)


Mrs. K. ANBARASI, M.Tech.,
Assistant Professor,
Department of Petrochemical Technology,
Bharathidasan Institute of Technology,
Anna University,Tiruchirappalli.
ACKNOWLEDGEMENT

Any piece of work that has proved its way remains incomplete if the sense of gratitude
and respect is not being deemed to those who have proved to be supportive during its
development period. Though these words are not enough, they can at least prove way to help
understand the feeling of respect and admirance I have for those who helped the way through.
I take this opportunity to express my deep sense of gratitude and indebtedness to our
Head of the Department Dr. M. ARULMOZHI, M.E., Ph.D., for her valuable ideas, and
encouragement given to me in bringing this work successfully.
I articulate my heartfelt thanks and deep sense of reverence to my guide
Mrs. K. ANBARASI, M.Tech., for her valuable guidance, sincere encouragement and
support throughout this project. More than a student, she treated me as a friend whole through
my project work. Without whom it would not have been possible to finish the assigned project
on time and to complete this report successfully.
I also thank all our Staffs of Petrochemical Technology for their enthusiastic
encouragement.
I hearty thanks to my friends for helping me in this project directly or indirectly helped
me in making this project a complete success. Words are inadequate to express my heartfelt
gratitude to my parents in this pursuit.
ABSTRACT

The economy of nation is built up by growth of industries this project deals with the industrial
production of Linear Alkyl Benzene Sulphonic Acid (LABSA) by a process called falling film
sulphonation. Linear Alkyl Benzene Sulphonic Acid is key raw material for detergent manufacturing.
This project deal with the process description highlighted with study of fixed bed catalytic convertor
for sulphur tri oxide production. In the design part , two important equipments which are concerned
with the sulphur tri oxide production cycle namely fixed bed catalytic convertor , heat exchanger are
included apart from this project also gives enough details about safety aspects , process control , plant
layout and location etc, which gives innovative ideas about the falling film sulphonation plant.

i
TABLE OF CONTENTS

C. NO TITLE PAGE.NO

ABSTRACT i

TABLE OF CONTENTS I

LIST OF TABLES VI

LIST OF FIGURES VII

LIST OF SYMBOLS VIII

1. INRODUCTION

1.1 Company profile 2

1.1.1 UPL Products 2

1.1.2 Awards and Achievements 3

1.2 LABSA profile 3

1.2.1 LABSA storage 4

1.2.2 LABSA packing 4

1.2.3 LABSA applications 4

2. PHYSICAL AND CHEMICAL PROPERTIES 5

3. METHODS AND SELECTION OF PROCESS 7

3.1 Methods of LABSA Production 8

3.2 Selection of Process 9

4. PROCESS FLOW SHEET 12

5. PROCESS DESCRIPTION 14

5.1 Process equipment specification 15

5.2 Air compression and drying section 17

5.3 Heat exchanger 17

I
5.4 Hydrocyclone 17

5.5 Adsorption tower 17

5.6 SO2 production section 17

5.6.1 Sulphur melting 17

5.6.2 Oven 17

5.7 SO3 production section 18

5.7.1 Fixed bed catalytic convertor 18

5.8 Falling film sulphonating reactor 19

5.9 Ageing tank 19

5.10 Effluent treatment 19

6. MATERIAL BALANCE 20

6.1 Raw materials 21

6.2 Air precooler 21

6.3 Heat exchanger 22

6.4 Hydrocyclone 23

6.5 Adsorption tower 23

6.6 Process air 24

6.7 Oven 24

6.8 Fixed bed catalytic convertor 25

6.9 Falling film sulphonating reactor 30

6.10 Ageing tank 31

7. ENERGY BALANCE 33

7.1 Energy balance 34

7.2 Air precooler 34

II
7.3 Heat exchanger-1 35

7.4 Heat exchanger-2 36

7.5 Heat exchanger-3 36

7.6 Heat exchanger-4 37

7.7 Heat exchanger-5 38

7.8 Heat exchanger-6 39

7.9 Oven 40

7.10 Fixed bed catalytic convertor 41

7.11 Falling film sulphonating reactor 41

7.12 Energy balance Flow sheet 43

8. DESIGN OF EQUIPMENTS 44

8.1 Design of Fixed Bed Catalyst Convertor 45

8.1.1 Design summary of Convertor 52

8.2 Design of Shell and Tube heat exchanger 53

8.2.1 Design summary Shell and Tube heat exchanger 57

9. COST ESTIMATION 58

9.1 Estimation of Purchased Equipment Cost 59

9.2 Equipment cost 61

9.3 catalyst 62

9.4 Direct Cost 62

9.5 Indirect Cost 63

9.6 Total Capital Cost 63

9.7 Total Production Cost 64

9.8 Total Production Cost for the production per year 66

III
9.9 Gross earnings 67

9.10 Tax rate 67

9.11 Payback period 67

10. PLANT LOCATION AND PLANT LAYOUT 68

10.1 Plant location 69

10.2 Cost 69

10.3 Process Economics 69

10.4 Process Requirement 70

10.5 Operation 70

10.6 Maintenance 70

10.7 Raw Material Supply 70

10.8 Markets and Transportation 70

10.9 Power and Fuel Supply 70

10.10 Water Supply 71

10.11 Labor 71

10.12 Plant Layout 72

11. PROCESS SAFETY MEASURES 73

11.1 Hazard identification 74

11.2 First aid measures 75

11.3 Fire fighting measures 75

11.4 Accidental Release Measure 75

11.5 Environmental precautions 76

11.6 Personal protective equipment 76

IV
12. INSTRUMENTATION AND CONTROL 79

13. CONCLUSION 83

14. REFERENCES 85

RESEARCH PROJECT 87

15. INTRODUCTION 88

16. MATERIALS & EXPERIMENTAL SETUP 89

17. RESULTS & DISCUSSIONS 90

18. CONCLUSION 92

19. REFERENCES 93

V
TABLE NO. LIST OF TABLES PAGE NO.

1. Difference between Oleum and SO3 process 9


2. Nature of Solid LABSA 10
3. Nature of Liquid LABSA 10
4. Nature of Powder LABSA 11
5. Material balance for Heat exchanger 22
6. Material balance for Hydrocyclone 23
7. Material balance for Adsorption tower 24
8. Material balance for Oven 25
9. Material balance for Fixed bed catalytic convertor First bed 26
10. Material balance for Fixed bed catalytic convertor Second bed 27
11. Material balance for Fixed bed catalytic convertor Third bed 28
12. Material balance for Fixed bed catalytic convertor Fourth bed 29
13. Material balance for Falling film sulphonating reactor 30
14. Material balance for Ageing tank 31
15. Equipment cost 61

VI
FIGURE NO. LIST OF FIGURES PAGE NO.

1. Manufacture of LABSA Flow sheet 13


2. Material balance flow sheet 32
3. Energy balance flow sheet 43
4. Plant layout diagram 72
5. Personal protective equipments 78
6. Types of plastics with codes 88
7. Simple distillation apparatus 90

VII
LIST OF SYMBOLS AND ABBREVIATIONS

SYMBOLS ABBREVIATIONS

λS Enthalpy of vapour

CP Specific heat of fluid

ρ Density

μ Viscosity of fluid

D Diameter of pipe

v Velocity of fluid

A Area

V Volume of bed

£ Porosity

Ʈ Space time

Re Reynolds’s number

Pr Prandtl number

Nu Nusselt number

L Pipe length

VIII
CHAPTER 1

INTRODUCTION

1
Introduction

1.1 Company profile

Ultramarine & Pigments Ltd is one of the leading manufacturers of pigments and surfactants in India.
This Thirumalai group company specializes in the manufacture of inorganic pigments, organic
surfactants & dry mix detergents and has two manufacturing units in TamilNadu, at Chennai and
Ranipet.

The company is over 50 years old, so obviously there have been many milestones for us. The ones that
come to mind immediately – getting into the sulphonation business in 1975 and setting up a factory in
remote Ranipet (Tamil Nadu); in 1991, the company started a Blue (pigment) factory in Ranipet, so
we doubled our capacity; in 2001, we started making alpha olefin sulphonate (AOS), and had gotten
QMS (Quality Management System) and EMS (Environment Management System) certified. They
also started the ITES (Information Technology Enabled Services) business at the same time.

Over the past two decades, they have won many awards from industry associations and the state
government for productivity, quality, safety and environment. The Surfactants factory in Ranipet is
running at full capacity. With a focus on optimizing the product mix, and increased value addition for
the customer, the division has seen a 13% increase in both sales volume and profit over the previous
year. The Surfactants division increased its revenues by 7% to ` 159.69 crores in financial year 2017-
18, as compared to ` 149.47 crores in financial year 2016-17.UPL is setting up a greenfield surfactants
project with an annual installed capacity of 30,000 Tonnes in Naidupeta, Andhra Pradesh. The
estimated project capital outlay for the same is approximately ` 70 Crores.

1.1.1 ULTRAMARINE & PIGMENTS LTD (UPL)

Productions:

They have three major verticals in the company – pigments, surfactants and ITES.In terms of business
models, they are focused on quality and customer satisfaction They pride ourselves in giving our
customers a menu of products to choose from, be it blue, AOS(Alpha olefin sulphonate), sodium
lauryl sulphate (SLS), sodium lauryl ether sulphate (SLES), or linear alkylBenzene sulphonic acid
(LABSA). In surfactants, they make liquid, paste, noodles, powder and needles.

In pigments, they make high quality grades for use in industrial applications, and they cater to the local
markets for whitewash and laundry grades. They make over 50 grades of pigments, controlling for as
many physical and chemical properties as possible. They are looking at many new products, including
non-toxic pigments to expand our stable of mixed metal oxides, and speciality surfactants to serve the
personal care market.

2
1.1.2 AWARDS AND ACHIEVEMENTS

1. AOTS-CUMI TPM Annual award 2005 –II Prize


2. AOTS TPM Annual award 2006-III Prize
3. CII Kaizen completion-II Prize
4. Safety award by Govt.of Tamilnadu-I Prize(2007)
5. Safety award by Govt.of Tamilnadu-I Prize(2011)
6. CFBP Award for Fair Business Practices in 2014

1.2 Linear Alkyl Benzene Sulphonic acid (LABSA) Profile:

Linear alkyl Benzene Sulphonic Acid (LABSA) is key raw materials for manufacture of synthetic
detergent cakes, powders and liquid detergents LABSA is called as acid slurry especially soft acid
slurry. LABSA is of anionic detergents type, whose detergent property is due to the anionic group
present in the compound. In order to develop full detergents in the compounds, the anions are
neutralized with alkaline or basic materials. Detergents are compounds which have a tendency to
dissolve in water and also in oils and other non aqueous materials under certain conditions.

Hence most of them are combination of water attracting, or hydrophilic groups, on the one end of the
molecules, with water repelling or hydrophobic groups on the other. The hydrophilic or water
attracting groups make the compound soluble in water, where as hydrophobic or water repelling
groups make the compound in soluble. As a result, interfacial tension between water and oil is reduced
and an emulsion is produced. The hydrophobic portion of the compound is usually a hydrocarbon
group containing carbon atoms is straight or slightly branched chain.

The hydrophobic functional group may be an Anionic, Cationic, Zwitterionic, Semi polar or non ionic.
In Linear Alkyl Benzene Sulphonic acid(LABSA). The hydrophilic portion is linear alkyl benzene
(LAB) and the hydrophobic portion is sulphonic acid which is anionic is nature and so the LABSA is
of anionic detergent type. The detergency property of LABSA depends on the amount of active
matters, free acid colour and viscosity in the compound. In the present situation the extent of
biodegradability of detergents pays a major role and so many of the manufactures were concerned over
this concept in order to increase the bio degradability.

In the case of detergents the bio degradability depends on their molecules structure. Linear chain
molecular structure is more bio degradable than branches chain molecular structure. And so mostly all
the detergents manufacture were focusing on introducing many linear chained detergents compounds
like LABSA, AOS etc.

3
1.2.1 Storage:

The most appropriate temperature for pumping should be chosen from the graph of viscosity against
temperature. Generally 40to 50°C is recommended. Prolonged storage at elevated temperature should
be avoided as the colour can be affected.

1.2.2 Packing:

Steel drums /HMHDPE barrels varies 50 to 200Kg.

1.2.3 Applications:

1. LABSA is especially suitable for the manufacture of sulphonates for both liquid and powder
detergents of all types.
2. Linear alkyl benzene Sulphonates have high solubility and low salt content allows them to be
incorporated in a wide variety of Liquid detergent formulations as well as detergent powder of
high quality.
3. Sulphonates with different characteristics can be obtained by neutralizing with varying bases
such as caustic soda (or) amines.

4
CHAPTER 2
PHYSICAL AND CHEMICAL PROPERTIES

5
2. Linear alkyl benzene (LAB)

Physical properties

Empirical formula: R – CH –R’

Molecular weight: 235 plus (or) minus

Appearance : Colour less liquid

Odour : Odour less

Density at 15°C : 0.885-0.870

Flash point : above 125°C

Chemical properties (Composition wt %)

< C10 : 1 MAX

C10 : 30 MAX

C11 : 30 — 45

Paraffin content: 0.5 MAX

Linear Alkyl Benzene Sulphonic acid (LABSA) Properties:

Chemical Formula : C15 H29SO3H (variable)

Molecular Weight : 318 — 322

Appearance : Brown Liquid

Odour : Characteristic

Viscosity at 50°C : App 200mNs / m2 (CPS)

Flash point : 90°C Minimum

Active matter % (as LABSA) : 96.0 Minimum

Free oil (or) (NDOM %) : 1.5 Maximum

Free Sulphuric acid : 1.5 Maximum

6
CHAPTER 3
METHODS AND SELECTION OF PROCESS

7
3.1 DIFFERENT PROCESS OF MANUFACTURING

Linear alkyl benzene sulphonic acid (LABSA) is basically manufactured by sulphonating linear alkyl
benzene (LAB) with sulphuric acid (or) oleum (or) SO3.The different process is with respect to the
sulphonating agents used viz. H2SO4, Oleurn, SO3. In all the cases linear alkyl benzene (LAB) is
directly sulphonated with sulphonating agents.

The simple reactions were, C12H25

C12H25

+ H2SO4 C18H29SO3H +H2O

Sulphuric acid LABSA

LAB

C12H25

+ H2S2O7 C18H29SO3H +H2SO4

Oleum LABSA

LAB

C12H25

+ SO3 C18H29SO3H

Sulphur trioxide LABSA

LAB

LABSA manufactured by different properties varies in active matters free acids, in colour, viscosity
and biodegradability.

Thin Film Sulphonation Process :( LABSA production)

The raw materials required for LABSA (Linear Alkyl Benzene Sulphonic acid) are

1. Linear Alkyl benzene (LAB)

2. Sulphur

8
Source of the raw materials

1. LAB :

Benzene + alkyl halides Alkyl Benzene

This is bought from Tamil Nadu Petro products limited (TPL)

2. Sulphur :Solid Sulphur in rhombic form is imported from Canada

3.2 SELECTION OF PROCESS

The difference in detergent properties of LABSA Management by different processes is given in the
following table. Table: 1

S.No. Oleum / Sulphonic Acid Process Sulphur Trioxide Process


1. Colour is dark Colour is light

2. More caustic Soda is required to neutralize Less caustic soda is required to


free acids neutralize free acids

3. Contains 13-15% of free acid Contain 2 to 4% of free acid

4. PbSO4 is formed as treatment is done in lead No formation of PbSO4 as treatment id


vessel done in stainless steel vessel

5. Less foaming More foaming

6. Price is higher Price is cheaper

7. Active detergency 95% + 1%

8. Higher Moisture content Lower moisture content

The differ in detergent properties of LABSA in different forms Viz, Cake form, liquid form, powder
form by different process is given following table,

9
CAKES

Table: 2

S.No. SO3 PROCESS SLURRY OLEUM / SULPHONIC ACID


SLURRY

1. Cracking rate is very slow Cracking rate

2. Ease processing due to low viscosity Processing stringent

3. Cake colour is bright due to light colour of Cake colour is dark due to dark colour of
slurry slurry

4. More foaming in nature Less 1 foaming in nature

LIQUID

Table: 3

S.No. SO3 PROCESS SLURRY OLEUM / SULPHONIC ACID


SLURRY

1. Colour in this case is bright and uniform Colour in this case is dark and non
uniform

2. Viscosity can be easily brought under control Viscosity can't be controlled

3. No pungent odour Pungent odour


4. No sedimentation present Sedimentation present

10
POWDER

Table: 4

S.No. SO3 PROCESS SLURRY OLEUM / SULPHONIC ACID


SLURRY

1. Colour of powder is white and uniform Colour of powder is yellowish and non
uniform

2. More quantity of water can be added in mixing Less quantity of water can be added in
product ,can hold about 10-15% of moisture missing product, can hold 5% of
moisture without foaming lumps
3. Process is economic Process is not economic

This project is concerned in the manufacture of LABSA by S03 process. The detailed manufacture
procedure with material balance, Energy balance for each and every equipment was detail in the
following section.

11
CHAPTER 4
FLOW SHEET

12
Figure: 1 Manufacture of Linear Alkyl Benzene Sulphonic Acid Flow sheet

13
CHAPTER 5
PROCESS DESCRIPTION

14
5. PROCESS DESCRIPTION

There are 8 sections in LABSA production. There are

1. Air Compression & Drying

2. Sulphur Melting

3. SO2 / Steam production

4. SO3 production

5. Sulphonation

6. Ageing & hydrolysis

7. Neutralization

8. Effluent treatments

5.1 Process equipment specification:

1. FILTERS: -

Type -Mesh.

Size -15

2. PRECOOLER:-

Type -Finned Tube Heat Exchanger

3. COMPRESSOR : -

Type - Rotary Lobe Compressor

Inlet Air - 20°C

Quiet Air -80°C

4. HEAT EXCHANGERS : -

E II - Shell & Tube Heat Exchanger

Tube side - Air 80°C to 50°C

Shell side - Cold water 27°C to 32°C

15
E17 - Shell & tube Heat Exchanger

Tube Side -Air 50°C to 10°C

Shell Side - MEG 10°C to 20°C

5 ADSORPTION COLUMNS: -

Type of Packing: Stacked Packing

Packing : Activated Alumina

Size : 2-4mm dia

6. PUMPS: -

P11, P12, P13 -Centrifugal pumps.

Capacity - 4 m3 / hr

Head - 25 m

The manufacture of LABSA by using I.AB and SO3 raw materials is the latest technology means of
manufacturing, Practiced at minimum number of industries in the world. In India only one company
that to (Ultra marine pigments) is using this technology of manufacturing using specially designed
sulphonating reactor by Eurrestra India Ltd. Thane in collaboration with Busto Arsizio. Italy Ltd for
Ultra marine Pigment Ltd.The process of manufacture of LABSA is simple as it is direct sulphonation
of LAB (i.e.) direct reaction between LAB with SO3, But the reacting conditions, SO3 concentration
air properties are to be maintained in order to get the maximum quantity of the LABSA with good
quality assurance.

Some important considerations are,

1. Process air should be dry at the sometime with low temp and negligible moisture.

2. SO2 to dry air mole should be In the order of 4% (mole) for the reaction.

3. SO2 to SO3 converter.

4. Sulphonator section.

5. Ageing vessel and hydrolysis section.

16
5.2 AIR COMPRESSION AND DRYING SECTION

The process air is sucked from the atmosphere and the air is filtered by using filter (711). The filter
removes the dust particles present in the air. The entering temp of the air will be at 30°C and after
filtering the temp of the air will reduce to 27°C. After filtering the air must be cooled. The air is cooled
in the me cooler. There are two sections in the pre cooler E19B and E19B. By using external agents as
Glycol and water the air is cooled. In the first section (E19A) the air is cooled by using water from
(27°C to °C) and in the section (E19B) the air is cooled by using Glycol from (23°C -20°C) after
cooling, the cooled air is compressed in compressor, due to the high pressure developed in the
compressor the temp of the air increases from 20 to 80°C) and then the air is subjected to heat
exchanger.

5.3 HEAT EXCHANGER

The compressed air is one again cooled by using the heat exchanger. In the heat exchanger (E11) the
air is cooled by using water as external agents from (80 to50°C). In the heat exchanger (E17) the air is
cooled by using Glycol as external agents from (50 to 10°C). Since the dew point of the air is 19°C
about 20% of water in the air gets condensed.

5.4 HYDROCYCLONE (D21)

In hydro cyclone due to the centrifugal action. About 80% of the water gets separated from the air
there by 90% of drying is achieved. The moisture collected can be drained at regular intervals. Drained
water will pumped to cooling water for maximum utilization of chillness.

5.5 ADSORPTION TOWER (D11A to D11B)

The air is subjected adsorption tower, where actuated alumina is used as a adsorbing agent. Here 99%
of the remaining water in the air gets removed. And then the air is distributed to different sections as
process air, Barrier air, and dilution air and as washing air. The process air from the absorber is
subjected to the heat exclmnget (E32 and E33).Where the SO3 - air mixture is cooled from 239°C to
52°C there by the air subjected gets heated from 10°C to 52°C. The heated air is then subjected to SO2
production.

5.6 SO2 PRODUCTION SECTION

5.6.1 SULPHUR MELTING

The Rhombic form or sulphur is melted using steam in heating coils. The melting point sulphur is
116°C and so about 200°C of steam is subjected. Thus molten sulphur of about 119°C is produced.
This molten sulphur is subjected to the oven.

17
5.6.2 OVEN

The oven used is lined with fire bricks. Once the molten sulphur and process air subjected. The
mixture is ignited. The molten sulphur burns as blue flame thereby producing SO2. The reaction
temperature maintained at the oven is about 720°C the SO2 formed is cooled in the heat exchanger
(G31) from (720°C to 435°C). About 92% conversion is achieved here.

5.7 SO3 PRODUCTION SECTION

5.7.1 FIXED BED CATALYTIC CONVERTOR

In the fixed bed catalytic convertor contains four beds of vanadium pent oxide (V2O5) catalyst.

FIRST BED

The SO2- air mixture at 435°C is subjected to the fixed bed catalytic converter where in the first bed
75% of SO2 is converted into SO3 by catalytic action. The reaction is as follows.

V2O5 440°C V2O4 + ½ O2

SO2 + ½ O2 440°C SO3

The reaction temp is strictly maintained at 440°C in favor the reversible reaction of V2O5 catalyst. The
unreacted SO2 – air mixture is subjected to 2nd bed. The Exit temperature of exit stream is about
530°C. Subjected to 2nd bed. The Exit temperature of exit stream is about 530°C.

SECOND BED

The SO2 air mixture from the first bed at a temp of about 530°C is cooled to 440°C by heat exchanger.
The cooled SO2 mixture is further follows same procedure as in first bed to form SO3. Here only 15%
of conversion is achieved. The temperature of Exit stream is 500°C. The SO2- air mixture is cooled at
heat exchanger from 500°C to 440°C before subjecting to third bed.

THIRD BED

In the third bed only 6% of remaining SO2 - air mixture from second bed is converted to SO3. The SO3
formed here is about 440°C approximately and so it is directly subjected to fourth bed.

FOURTH BED

In the fourth bed only 2% of remaining SO2 - air mixture is converted to SO3. The SO3 thus formed is
about 440°C. The SO3- air mixture before subjecting to sulphonator it is cooled using 3 heat exchanger
(G32, E32, and E33), it is cooled from 440°C to 52°C.

18
5.8 FALLING FILM SULPHONATING REACTOR

The sulphonator for the production of LABSA from LAB and SO3 if of special type. Falling film
sulphonator which contains about 44 tubes is used. In which a thin film of linear alkyl benzene (LAB)
is subjected over which proportional amount of Barrier air is subjected and then SO3- air mixture is
subjected. The purpose of barrier to stop the Reaction is to stop the reaction between the reactants for
few seconds at the initial stage. The reaction taking place is,

C12H25 SO3 C12H25

+ SO3

LAB LABSA

In the sulphonator being the residence time of reactants is very low and so only 79% conversion is
achieved. The exit stream for sulphonator is directly subjected to ageing tank. The sulphonator is
maintained at temp of 40°C to 45°C in order to achieve maximum conversion for that cooling water is
circulated around the reactor.

5.9 AGEING TANK

Ageing tank is nothing but a jacketed vessel with agitator. Here un converted LAB and SO3 air
mixture is reacted. Here about 91% conversions achieved. LABSA formed is hydrolyzed in hydrolysis
tank by water in hydrolysis tank by water in order to stop the reaction. The final LABSA with 96%
active matter is used for further manufacture of detergents. For the detergent manufacture only about 7
to 16% of LABSA is used as key raw material in accordance with the required detergency properties.

5.10 EFFLUENT TREATMENT

The major effluent from the plant is Oleum and exhaust gas from the sulphonator. The oleum from is
sent to the scrubber where it is treated with NaOH for neutralization. The neutralized product is sent
into the solar pond and into the solar pond and allowed for solar evaporation. The exhaust gas from the
sulphonator is sent to the Electro Static Precipitator (ESP). A number of electrodes are connected with
each electrode. The positively charged ions are attracted by the anode and the negatively charged ions
are attracted by the cathode thereby the exhaust gas gets free from solids arc sent to the scrubber.

19
CHAPTER 6
MATERIAL BALANCE

20
6. MATERIAL BALANCE

Basis: 1000 kg/hr of Linear Alkyl Benzene Sulphonic Acid (LABSA)

6.1 RAW MATERIALS

Sulphur, S = 137.92 kg/hr

Air = 6855 kg/hr

Linear alkyl benzene, LAB = 765 kg/hr

Overall reactions:

S + O2 SO2

SO2 + ½ O2 SO3

SO3 + C12H25 C12H25 SO3

LAB LABSA

6.2 AIR PRECOLLER

Air in AIR Air out

6855 kg/hr PRECOOLER 6855 kg/hr

Properties of Air:

Temperature = 30°C

Relative humidity = 50%

Humidity = 0.014 kg of H2O / kg of dry air.

Dew point = 19°C

Amount of water in inlet air = 0.014 kg of H2O / kg of air

Amount of water in total air inlet = 95.97 kg/hr of water.

21
6.3 HEAT EXCHANGER

Air in HEAT Air outlet


EXCHANGER
6855kg/hr at 80°C 6835.80 kg/hr at 10°C

Water

19.20 kg/hr

Dew point of air is 19°C and so some amount of water in the gets conducted say , 20% of the water
content gets condensed here,

Amount of air gets condensed = 95.97*0.2 = 19.20 kg/hr

Amount of water in exit stream = 95.97-19.20 = 76.77 kg/hr

Air in exit stream = 6855-19.20 = 6835.80 kg/hr

Table: 5

INLET STREAM EXIT STREAM

Air = 9855 kg/hr Air = 6835.80 kg/hr

Water = 19.20 kg/hr

TOTAL = 6855.0 kg/hr

22
6.4 HYDROCYCLONE

Air in 6835.80 kg/hr Air Out 6774.38 kg/hr


HYDROCYCLONE

Water

61.42 kg/hr

Here 80% of the remaining water content of the air gets condensed.

Amount of the water condensed = 76.77*0.8 = 61.42 kg/hr

Amount of air exist stream = 6835.80-61.42 = 6774.38 kg/hr

Amount of the water in exit stream = 76.77-61.42 = 15.35 kg/hr

Table: 6

INLET STREAM EXIT STREAM

Air = 6835.80 kg/hr Air = 6774.38 kg/hr

Water = 61.42 kg/hr

TOTAL = 6835.80 kg/hr

6.5 ADSORPTION TOWER

Air in 6774.38 kg/hr ADSORBER Air Out 6759.18 kg/hr

Here 99% of the remaining water gets absorbed.

Amount of water adsorbed = 15.35*0.99 = 15.20 kg/hr

Amount of air stream = 6774.38-15.20


amount of water in exit stream = 15.35-15.20

= 0.15 kg/hr

0.15 kg/hr of water is present in 6759.18 kg/hr of dry air.

23
Table: 7

INLET STREAM EXIT STREAM

Air = 6774.38 kg/hr Air = 6759.18 kg/hr

Water = 15.20 kg/hr

TOTAL = 6774.38 kg/hr

6.6. PROCESS AIR

The amount of process air from the absorber is 6759.18 kg/hr with 0.1 kg/hr of water

We can take the process air be 6759 kg/hr excluding water content.

Amount of air actually required for dilution = 5827.4 kg/hr

For SO2 production process air subjected = 6759-5827.4

= 931.6 kg/hr

6.7 OVEN

S + O2 SO2 (92% conversion)

S = 137.92 kg/hr SO2 = 253.77 kg/hr

OVEN S = 11.03 kg/hr

Air = 931.60 kg/hr Air = 804.71 kg/hr

Amount of sulphur at sulphur at inlet = 137.92 kg/hr

Moles of sulphur = 137.92/32 = 4.31 kmoles

Moles of oxygen required = 4.31 kmoles

Assume 20% excess oxygen required = 4.31*1.2*32

= 165.50 kg/hr

24
Amount of air actually requires = 165.50*100/23 = 719.58 kg/hr

Amount of air at inlet = 931.60 kg/hr

Amount of air at inlet = 0.92*4.31*64 = 253.77 kg/hr

Amount of sulphur in exit stream = 0.08*4.31*32 = 11.03 kg/hr

Amount of oxygen reacted = 0.92*4.31*32

= 126.89 kg/hr

Amount of air in exit stream = 214.27-126.89

= 87.38 kg/hr

Amount of air in exit stream = 931.6-126.89

= 804.71 kg/hr

Table: 8

INLET STREAM EXIT STREAM

S = 137.92 kg/hr SO2 = 253.77 kg/hr

Air = 931.60 kg/hr S = 110.03 kg/hr

TOTAL = 1069.52 kg/hr Air = 804.71 kg/hr

TOTAL = 1069.52 kg/hr

6.8 FIXED BED CATALYTIC CONVERTOR

SO2 + ½ O2 SO3 (98% conversion)

FIRST BED: (75% CONVERSION)

SO2 = 253.77kg/hr SO3 = 237.90 kg/hr


FIRST BED
SO2 = 63.45 kg/hr

Air = 804.71 kg/hr Air = 757.13 kg/hr

25
Amount of air inlet = 804.71 kg/hr

Oxygen content = 87.38 kg/hr


Amount of SO2 at inlet = 253.77 kg/hr

Moles of SO2 = 253/64 = 3.965 Kmoles/hr

Amount of oxygen required = 3.965*16 = 63.44 kg/hr

Under 75% conversions

Amount of SO2 reacted = 0.75*3.965*64 = 190.32 kg/hr

Amount of oxygen reacted = 0.75*3.965*16 = 47.58 kg/hr

Amount of SO3 formed = 0.75*3.695*80 = 237.90 kg/hr

Amount of SO2 in exit = 253.77-190.30 = 63.45 kg/hr

Amount of air in exit = 804.71-47.58 = 757.13 kg/hr

Oxygen content = 87.38-47.58 = 39.80 kg/hr

Table: 9

INLET STREAM EXIT STREAM

SO2 = 253.77 kg/hr SO3 = 237.90 kg/hr

Air = 804.71 kg/hr SO2 = 63.45 kg/hr

TOTAL = 1058.48 kg/hr Air = 757.13 kg/hr

TOTAL = 1058.48 kg/hr

SECOND BED: (90% CONVERSION)

SECOND
SO2 = 63.45kg/hr SO3 = 11.89kg/hr
BED
SO2 = 53.94kg/hr

Air = 757.13kg/hr Air = 754.75kg/hr

26
Amount of air inlet = 757.13 kg/hr

Oxygen content = 39.80 kg/hr


Amount of SO2 at inlet = 63.45 kg/hr

Moles of SO2 = 63.45/64 = 0.991 Kmoles/hr

Under 90% conversions

Amount of SO2 reacted = 0.90*0.991*64 = 9.51 kg/hr

Amount of oxygen reacted = 0.90*0.991*16 = 2.38 kg/hr

Amount of SO3 formed = 0.90*0.991*80 = 11.89 kg/hr

Amount of SO2 in exit = 63.45-9.51 = 53.94 kg/hr

Amount of air in exit = 757.13-2.38 = 754.75 kg/hr

Oxygen content = 39.80-2.38 = 37.42 kg/hr

Table: 10

INLET STREAM EXIT STREAM

SO2 = 63.45 kg/hr SO3 = 11.89 kg/hr

Air = 757.13 kg/hr SO2 = 53.94 kg/hr

TOTAL = 820.53 kg/hr Air = 757.75 kg/hr

TOTAL = 820.58 kg/hr

THIRD BED: (96% CONVERSION)

SO2 = 53.94kg/hr SO3 = 4.03 kg/hr


THIRD BED
SO2 = 50.71 kg/hr

Air = 754.75 kg/hr Air = 753.95 kg/hr

Amount of air inlet = 754.75 kg/hr

27
Oxygen content = 37.42 kg/hr

Amount of SO2 at inlet = 53.94 kg/hr

Moles of SO2 at inlet = 53.94/64 = 0.84 Kmoles/hr

Under 96% conversions

Amount of SO2 reacted = 0.96*0.084*64 = 3.23 kg/hr

Amount of oxygen reacted = 0.96*0.84*16 = 0.81 kg/hr

Amount of SO3 formed = 0.96*0.84*80 = 4.03 kg/hr

Amount of SO2 in exit = 53.94 -3.23 = 50.71 kg/hr

Amount of air in exit = 754.75-0.80 = 753.95 kg/hr

Oxygen content = 37.42-0.81 = 36.61kg/hr

Table: 11

INLET STREAM EXIT STREAM

SO2 = 53.94 kg/hr SO3 = 4.03 kg/hr

Air = 754.75 kg/hr SO2 = 50.71 kg/hr

TOTAL = 808.69 kg/hr Air = 753.95 kg/hr

TOTAL = 808.69 kg/hr

FOURTH BED: (98% CONVERSION)

SO2 = 50.71kg/hr SO3 = 1.26 kg/hr

FOURTH BED SO2 = 49.70 kg/hr

Air = 753.95 kg/hr Air = 753.70 kg/hr

28
Amount of air inlet = 753.95 kg/hr

Oxygen content = 36.61kg/hr


Amount of SO2 at inlet = 50.71 kg/hr

Moles of SO2 at inlet = 50.71/64 = 0.79 Kmoles/hr

Under 98% conversions

Amount of SO2 reacted = 0.98*0.79*64 = 1.01 kg/hr

Amount of oxygen reacted = 0.98*0.79*16 = 0.25 kg/hr

Amount of SO3 formed = 0.98*0.79*80 = 1.26 kg/hr

Amount of SO2 in exit = 50.71-1.01 = 49.70 kg/hr

Amount of air in exit = 753.95-0.25 = 753.70 kg/hr

Oxygen content = 36.61-0.25 = 36.36kg/hr

Table: 12

INLET STREAM EXIT STREAM

SO2 = 50.71kg/hr SO3 = 1.26 kg/hr

Air = 753.95 kg/hr SO2 = 49.70 kg/hr

TOTAL = 804.66 kg/hr Air = 753.70 kg/hr

TOTAL = 804.66 kg/hr

Amounts of SO3 totally formed

First bed = 237.90 kg/hr

Second bed = 11.89 kg/hr

Third bed = 4.03 kg/hr

Fourth bed = 1.26 kg/hr

Total SO3 = 255.08 kg/hr

29
Amount of air in exit stream = 753.70 kg/hr

To get 45(mol %) of SO3 w.r.t. air, some amount of distillation air is added.

Dilution air = 5827.4 kg/hr

6.9 FALLING FILM SULPHONATING REACTOR

SO3 + C18H30 C18H29SO3H (79% conversion)

LAB LABSA

SO2 = 255 kg/hr LABSA = 805.80 kg/hr

SULPHONATER SO3 = 5355 kg/hr

Air = 765 kg/hr LAB = 160.65 kg/hr

Amount of air at inlet = 255 kg/hr

Moles of SO3 = 255/80 = 3.1875 kg/moles hr

Amount of SO3 reacted = 0.79*3.1875*80 = 201.45 kg/hr

Amount of LAB reacted = 0.79*3.1875*240 = 604.35 kg/hr

Amount of LABSA formed = 0.79*3.1875*320 = 805.80 kg/hr

Amount of SO3 in exit stream = 255-201.45 = 53.55 kg/hr

Amount of LAB in exit stream = 765-604.35 = 160.65 kg/hr

Table: 13

INLET STREAM EXIT STREAM

SO3 = 255 kg/hr SO3 = 5355 kg/hr

LAB = 765 kg/hr LAB = 160.65 kg/hr

TOTAL = 1020 kg/hr LABSA = 805.80 kg/hr

TOTAL = 1020.00 kg/hr

30
6.10 AGEING TANK

SO3 + LAB LABSA (91% CONVERSION)

SO3 = 53.55 kg/hr AGEING


AGEING LABSA = 194.20 kg/hr

TANK SO3 = 4.78 kg/hr

LAB = 160.65 kg/hr LAB = 14.32 kg/hr

Amount of SO3 at inlet = 53.55 kg/hr

Moles of SO3 at inlet = 5355/80 = 0.67 kmoles/hr

Amount of LAB at inlet = 160.65 kg/hr

Under 91% conversions

Amount of SO3 reacted = 0.91*0.67*80 = 48.78 kg/hr

Amount of LAB reacted = 0.91*0.67*240 = 146.33 kg/hr

Amount of LABSA formed = 0.91*0.67*320 = 194.20 kg/hr

Amount of SO3 in exit stream = 53.55-48.78 = 4.78 kg/hr

Amount of LAB in exit stream = 160.65-146.33 = 14.32 kg/hr

Table: 14

INLET STREAM EXIT STREAM

SO3 = 53.55kg/hr SO3 = 4.78 kg/hr

LAB = 160.65 kg/hr LAB = 14.32 kg/hr

TOTAL = 214.20 kg/hr LABSA = 194.20 kg/hr

Amount of Linear Alkyl Benzene Sulphonic Acid (LABSA) totally formed,

Sulphonator = 805.80 kg/hr

Ageing Vessel = 194.20 kg/hr

TOTAL LABSA = 1000.00 kg/hr.

31
Figure: 2 Material balance Flow sheet

32
CHAPTER 7
ENERGY BALANCE

33
7.1 ENERGY BALANCE

Specific heat capacity of water, CpH2O = 4.184 kJ/kgºC

Specific heat capacity of sulphur CpS = 1.07 kJ/kgºC

Specific heat capacity of sulphur dioxide CpSO2 = 0.76 kJ/kgºC

Specific heat capacity of sulphur trioxide CpSO3 = 0.550 kg/kgºC

Specific heat capacity of Air, Cp air = 10.008 kJ/kgºC

Latent heat of Vaporization of water = 2261.45 kJ/kg

Heat of formation of SO3, Hf, so3 = -4.963 kJ/kg

Heat of formation of LAB, Hf, LAB = 0.97 kJ/kg

Heat of formation of LABSA, Hf, LABSA = -0.53 kJ/kg

Heat of formation of SO2,Hf,SO2 = -4.638 kJ/kg

7.2 AIR PRECOOLER

Water 10ºC Glycol

Air in H.E Air 6855kg/hr Air out


H.E
1
6855kg/hr 27ºC 23ºC 2 6855 kg/hr

Water 18ºC Glycol

34
7.3 HEAT EXCHANGER ( 1 )

Water 32ºC

Air in 6855 Air 6855


H.E
kg/hr 80ºC kg/hr 50ºC

Water 27ºC

Amount of Air inlet Mair = 6855 kg/hr

Amount of water required Mwater = 9909 kg/hr

Heat inlet Qi = Mair Cpair Tair

= 6855 * 1.008 * (80-50)

= 207295.2 kJ/hr

Heat outlt Qo = Mwater Cpwater Twater

= Mwater (4.184) (32-27)

= 20.92 Mwater

Qi = Qo; 207295.2 = 20.92 Mwater

Mwater = 9909 kg/hr

Amount of water required = 9909 kg/hr

35
7.4 HEAT EXCHANGER (2)

Glycol 18ºC

Air 6855 Air out

kg/hr 50ºC 6855 kg/hr


H.E
10ºC

Glycol 5ºC

Amount of Air inlet Mair = 6855 kg/hr

Amount of water required Mglycol = 8921 kg/hr

Heat inlet Qi = Mair Cpair Tair

= 6855 * 1.008 * (50-10)

= 276393.6 kJ/hr

Heat outlet Qo = Mglycol Cpwater Tglycol

= Mglycol (2.36) (18-5)

= 30.68 Mglycol

Qi = Qo; 20729.52 = 30.68 Mglycol ;Mglycol = 8921 kg/hr

Amount of water required = 8921 kg/hr

7.5 HEAT EXCHANGER (3)

Steam 200ºC

SO2 + air SO2 +air


H.E
740ºC 1058.48 kg/hr 435ºC 1058.48 kg/hr

Water 45ºC

36
Amount of SO2 = 253.77 kg/hr

Amount of dry air = 804.71 kg/hr

Amount of SO2 + air = 1058.48 kg/hr

Specific heat capacity of SO2 + air Mixture,

Cp (SO2 + air) = (0.24) 0.761 + 0.76 (1.008)

= 0.95 kJ/kgºC

Heat in, Qi = MSO2+air CpSO2+air T

= 1058.48 * 0.95 * (740-435)

Qi = 306694.58 kJ/hr

Heat out Qo = Mwater Cpwater T + Mwater λ

= Mwater (4.184 (200-45) + 2261.45)

Qo = 2909.97 Mwater

Qi = Qo; 306694.58 = 2909.97 Mwater Mwater = 105.4 kg/hr

Amount of water required = 105.4 kg/hr

7.6 HEAT EXCHANGER (4)

Steam 200ºC

SO3 + air SO3 +air


H.E
440ºC 1008.69 kg/hr 239ºC 1008.69 kg/hr

Water 45ºC

Amount of SO3 = 255.00 kg/hr

Amount of dry air = 753.69 kg/hr

Amount of SO3 + air = 1008.69 kg/hr

37
Specific heat capacity of SO3 + air Mixture,

Cp (SO3 + air ) = (0.25) 3.22 + 0.75 (1.008)

= 1.56 KJ/kgºC

Heat in ,Qi = MSO3+air CpSO3+air TSO3+air

= 1008.69 * 1.56 * (440-239)

Qi = 316284.8 kJ/hr

Heat out Qo = Mwater Cpwater T + Mwater λ

= Mwater (4.184 (200-45) + 2261.45)

Qo = 2909.97 Mwater

Qi = Qo; 316284.8 = 2909.97 Mwater : Mwater = 108.7 kg/hr

Amount of water required = 108.7 kg/hr

7.7 HEAT EXCHANGER ( 5 )

Air 37ºC

SO3 + air SO3 +air


H.E
239ºC 1008.69 kg/hr 120ºC 1008.69 kg/hr

Air 10ºC

Amount of SO3 = 255.00 kg/hr

Amount of dry air = 753.69 kg/hr

Amount of SO3 + air = 1008.69 kg/hr

Amount of cooling air = 6855 kg/hr

Specific heat capacity of SO3 + air Mixture,

38
Cp (SO3 + air ) = (0.25) 3.22 + 0.75 (1.008)

= 1.56 kJ/kgºC

Heat in, Qi = MSO3+air CpSO3+air TSO3+air

= 1008.69 * 1.56 * (239-120)

Qi = 186565.7 kJ/hr

Heat Out Qo = Mair Cpair Tair

= 6855 (1.008 (17-10) )

Qo = 186565.7 kJ/hr

Therefore Qi = Qo = 186565.7 kJ/hr

7.8 HEAT EXCHANGER (6)

Air 52.5ºC

SO3 + air SO3 +air


H.E
120ºC 1008.69 kg/hr 52ºC 1008.69 kg/hr

Air 37ºC

Amount of SO3 = 255.00 kg/hr

Amount of dry air = 753.69 kg/hr

Amount of SO3 + air = 1008.69 kg/hr

Amount of cooling air = 6855 kg/hr

Specific heat capacity of SO3 + air Mixture,

Cp (SO3 + air) = (0.25) 3.22 + 0.75 (1.008)

= 1.56 kJ/kgºC

39
Heat in, Qi = MSO3+air CpSO3+air TSO3+air

= 1008.69 * 1.56 * (120-52)

Qi = 107001.8 kJ/hr

Heat Out Qo = Mair Cpair Tair

= 6855 (1.008 (52.5-37))

Qo = 107001.8 KJ/hr ; Therefore Qi = Qo = 107001.8 kJ/hr

7.9 OVEN

S + O2 SO2

S = 137.92 kg/hr OVEN

740 ºC SO2 = 255 kg/hr 740ºC

Air = 931.60 kg/hr

Amount of Sulphur at inlet Ms = 137.92 kg/hr

Amount of air at inlet Mair = 931.60kg/hr

Oxygen content MO2 = 214.27 kg/hr

Amount of SO2 formed MSO2 = 253.77 kg/hr

Heat of formation of SO2 Hf, SO2 = -4.638 kJ/kg

Heat of formation of Sulphur Hf, SO2 = 0 kJ/kg

Heat of formation of Oxygen Hf, O2 = 0 kJ/kg

Heat of reaction Hrxn = M SO2 Hf, SO2 + ( M2 Hf,s + MO2 Hf, SO2 )

= 253.77 (-4.638) – (137.92 (0) + 214.27 (0))

Heat of reaction Hrxn = -117 kJ/hr

40
7.10 FIXED BED CATALYTIC CONVERTOR

SO2 + ½ O2 SO3

SO2 = 253.77 kg/hr FIXED BED


CATALYTIC
CONVERTOR SO3 = 255 kg/hr

Air = 804.71 kg/hr

Amount of SO2 at inlet MSO2 = 253.77 kg/hr

Amount of air at inlet Mair = 804.71 kg/hr

Oxygen content MO2 = 87.38 kg/hr

Amount of SO2 formed MSO3 = 255 kg/hr

Heat of formation of SO2 Hf, SO2 = -4.936 kJ/kg

Heat of formation of Sulphur Hf, SO2 = -4.936 kJ/kg

Heat of formation of Oxygen Hf, O2 = 0 kJ/kg

Heat of reaction Hrxn = MSO2 Hf, SO2 + (MSO2 Hf,SO2 + MO2 Hf, O2 )

= 255 (-4.936) – { (253.77 (-4638) + 87.38 (0) }

Heat of reaction Hrxn = -81.68 kJ/hr

7.11 FALLING FILM SULPHONATING REACTOR

SO3 + C18H30 C18H29SO3H

LAB LABSA

SO2 = 253.77 kg/hr FALLING FILM


SULPHONATING
REACTOR SO3 = 255 kg/hr

Air = 804.71 kg/hr

Amount of SO3 at inlet MSO3 = 255 kg/hr

Amount of LAB at inlet MLAB = 765 kg/hr

41
Amount of LABSA at exit, MLABSA = 1000 kg/hr

Heat of formation of SO3, Hf, SO3 = -4.936 kJ/kg

Heat of formation of LAB, Hf, LAB = 0.97 kJ/kg

Heat of formation of LABSA, Hf, LABSA = -0.53 kJ/kg

Heat of reaction Hrxn = MLABSA Hf, SO2 + (MSO2 Hf,SO2 + MLAB Hf, LAB )

= 1000 (-0.53 ) – { (255 (-4.936) + 765 (0.97) }

Heat of reaction Hrxn = -11.9 kJ/hr

42
Figure: 3 Energy balance Flow sheet

43
CHAPTER 8
EQUIPMENT DESIGN

44
8.1 DESIGN OF FIXED BED CATALYTIC CONVERTOR

ASSUMPTION

 Vanadium Pentoxide (V2O5) Catalyst.


 Volume of Vanadium pentoxide in each bed:

First bed = 0.800 m3

Second bed = 0.600 m3

Third bed = 0.300 m3

Fourth bed = 0.300m3

 The radius of pellet = 4mm


 The length of pellet = 8mm
 Cross sectional area of the convertor = 1.54 m2
 Porosity of fixed bed = 0.44
 Space time = 1.8 sec

Calculation to find height of each bed:

First bed:

Volume of a pellet = П *r2*h

= 3.14*42*8

= 402.12 mm2.

Volume of each pellet = 4.02*10-7 m3.

Volume of the first bed= 0.8 m3

Total number of the pellets, n = 0.8/ (4.02*10-7)

= 1990050 pellets

Height of the bed = (n/2A)( П*dp3/6)(1-£)-1

= (1990050/2*1.54)(3.14*(8*10-3)3/6)(1-0.44)-1

= 0.31 m.

45
Second bed:

Volume of a pellet = П *r2*h

= 3.14*42*8

= 402.12mm2.

Volume of each pellet = 4.02*10-7 m3.

Volume of the first bed = 0.6 m3

Total number of the pellets, n= 0.6/ (4.02*10-7)

= 1492538 pellets

Height of the bed,H =(n/2A)( П*dp3/6)(1-£)-1

= (1492538/2*1.54) (3.14*(8*10-3)3/6) (1-0.44)-1

= 0.23 m.

Third bed:

Volume of a pellet = П *r2*h

= 3.14*42*8

= 402.12 mm2.

Volume of each pellet = 4.02*10-7 m3.

Volume of the first bed = 0.3 m3

Total number of the pellets, n = 0.3/ (4.02*10-7) = 746270 pellets

Height of the bed, H = (n/2A) (П*dp3/6)(1-£)-1

= (746270/2*1.54) (3.14*(8*10-3)3/6) (1-0.44)-1

= 0.12 m.

Fourth bed:

Volume of a pellet = П *r2*h

= 3.14*42*8

46
= 402.12 mm3.

Volume of each pellet = 4.02*10-7 m3.

Volume of the first bed= 0.300 m3

Total number of the pellets, n= 0.3/ (4.02*10-7)

= 746270 pellets

Height of the bed, H = (n/2A)( П*dp3/6)(1-£)-1

= (746270/2*1.54)(3.14*(8*10-3)3/6)(1-0.44)-1

= 0.12 m.

Total height required for catalyst= 0.31 + 0.23 + 0.12 + 0.12

= 0.78 m.

Calculation of volume height of the convertor required for gaseous stream:

Above First bed:

Mass flow rate of SO2-Air mixture, m = 1058.48 kg/hr.

Density of SO2-Air mixture, ρ = 0.596 kg/m3

Diameter of inlet pipe, d = 0.1524 m

Cross sectional area of pipe, A= 0.018 m2

Volumetric flow rate = m/ ρ

= 1058.48 /0.596

= 1776 m3/hr

= 0.493 m3/sec

Mass velocity of inlet stream, u = v/A

= 0.493/0.018

= 27.4 m/sec.

47
Volume required, V = v*Ʈ

= 0.493*1.8

= 0.8624 m3.

Height of the convertor required, H = V/ (П * r2)

= 0.8624/(3.14*0.352)

= 2.2 m.

Above Second bed:

Mass flow rate of SO2-Air mixture, m = 1058.48 kg/hr.

Density of SO2-Air mixture, ρ = 0.745kg/m3

Diameter of inlet pipe, d = 0.1524 m

Cross sectional area of pipe, A = 0.018 m2

Volumetric flow rate, v = m/ ρ

= 1058.48/0.745

= 1776 m3/hr

= 0.257 m3/sec

Mass velocity of inlet stream,u = v/A

= 0.257/0.018

= 14.8 m/sec.

Volume required, V = v*Ʈ

= 0.257*1.8

= 0.4626m3.

Height of the convertor required, H = V/ (П * r2)

= 0.4626/ (3.14*0.352)

= 1.2 m.

48
Above Third bed:

Mass flow rate of SO2-Air mixture, m = 820.55 kg/hr.

Density of SO2-Air mixture, ρ = 1.22 kg/m3

Diameter of inlet pipe, d = 0.1524 m

Cross sectional area of pipe, A = 0.018 m2

Volumetric flow rate, v = m/ ρ

= 820.55/1.22

= 1776 m3/hr= 0.181 m3/sec

Mass velocity of inlet stream, u = v/A

= 0.181/0.018

u = 10.1 m/sec.

Volume required, V = v*Ʈ

= 0.181*1.8

= 0.3258 m3.

Height of the convertor required, H = V/ (П * r2)

= 0.3258/ (3.14*0.352)

= 0.85 m.

Above Fourth bed:

Mass flow rate of SO2-Air mixture, m = 808.69 kg/hr.

Density of SO2-Air mixture, ρ = 2.36kg/m3

Diameter of inlet pipe, d = 0.1524 m

Cross sectional area of pipe, A = 0.018 m2

Volumetric flow rate, v = m/ ρ

= 808.69/2.36

49
= 1776m3/hr

= 0.094 m3/sec

Mass velocity of inlet stream, u = v/A

= 0.094/0.018

= 5.2 m/sec.

Volume required, V = v*Ʈ

= 0.094*1.8

= 0.1692 m3.

Height of the convertor required, H = V/ (П * r2)

= 0.1692/(3.14*0.352)

= 0.44 m.

Below fourth bed:

Mass flow rate of SO2-Air mixture, m = 804.66 kg/hr.

Density of SO2-Air mixture, ρ = 2.66kg/m3

Diameter of inlet pipe, d = 0.1524 m

Cross sectional area of pipe, A = 0.018 m2

Volumetric flow rate, v = m/ ρ

= 804.77/2.66

= 1776 m3/hr

= 0.083 m3/sec

Mass velocity of inlet stream, u = v/A

= 0.083/0.018

= 4.6 m/sec.

50
Volume required, V = v*Ʈ

= 0.083*1.8

= 0.150 m3.

Height of the convertor required, H =V/ (П * r2)

= 0.150/ (3.14*0.352)

= 0.39 m.

Sieve tray of 3 meshes is used to hold the catalyst

Area per openings = П (6.73)2/4 = 35.6 mm2

Total cross section area of the column = 1.54m2

Area of openings per square inch = 3*35.6 = 106.8mm2

Cross sectional area of the column in inches= (1.54*106)/645 = 2388 in2

Total number of openings = 3*2388 = 7164 openings

Perforated area = 7164*35.6 = 255038 mm2

Unperforated area = 1284962 mm2

Thickness of sieve tray = 0.15 m

Total height of the convertor

Height of the catalysts = 0.78 m: Height of each gaseous section

First bed = 2.2 m

Second bed = 1.2 m

Third bed = 0.85 m

Fourth bed = (0.44 + 0.39) m

Sieve trays = 0.60 m

Total height = 6.66 m

51
Thickness of the shell

Pressure inside the convertor, P = 0.7*105 kg/m2

Permissible stress, f = 2.03*105kg/m2

Inside diameter, Di = 0.7 m

Thickness of the convertor, t = PDi/ (2fj-P)

= (0.7*105*0.7)/ (2*2.03*105 – 0.7*105)

= 90 mm.

8.1.1 Design Summary of fixed bed catalytic convertor:

Cross sectional area of the convertor = 1.54 m2

Height of the convertor = 6.66 m

Pressure acting inside the convertor =0.7*105 kg/m2

Thickness of the convertor =90 mm

Radius of the catalyst pellet = 4 mm

Length of the pellets =8 mm

Pipe diameter =6 inch

52
8.2 DESIGN OF SHELL AND TUBE HEAT EXCHANGER

Shell side: (SO2)

Feed = 1058.48 kg/hr

Inlet temperature = 740 C

Outlet temperature = 435°C

Tube side: Ethylene glycol

Flow rate = 8921 kg/hr

Inlet temperature = 45 °C

Outlet temperature = 200 °C

Heat balance:

Q = mcp = 1058.48*0.64*305

= 206615.2 KW

LMTD:

= 540-390/ln (540/390)

= 465°C

Correction factor 465°C at FT = 0.8

Heat transfer area:

Q = UA

Assume U = 200 W/m2°C

206615.2 =100*A*465

A = 40.62 m2

Heat transfer area per tube = 0.3 m2

Length of the tube = 4.5 m

Number of tubes = Area/ number of tubes

53
= 40.62/0.3

= 135 tubes

Triangular pitch = 25.4 mm

Number of pitch = 300

Corrected heat transfer area = 0.3*135 = 40.5 m2

In this heat exchanger, 2 tube pass and 1 shell pass

Average properties of fluids:

Shell side:

Density = 2.93 kg/m3

Viscosity = 0.4 kg/ms

Cp = 0.81 J/kgC

K = 4.1 W/mK

Tube side:

Density = 1.1 kg/m3

Viscosity = 5.2 kg/ms

Cp = 2.2 J/kgK

K = 3.5 W/mK

Tube side velocity:

Number of pass = 2

Flow area = 3.14*D2Nt/4Np

= 0.014 m2

Vt =m/A*density

= 1.5 m/s

54
Shell side velocity:

Sm = 0.015 m2

Vs = 1058.48/2.9*0.015

= 3.1 m/s

HEAT TRANSFER COEFFICIENT

Shell side:

hiDi/K = 0.023 (Nre) 0.8 (Npr) 0.33

Di = 0.018 m

Nre = 3428.1

Npr = 0.69

hi = 3119 W/m2k

Number of baffles = L/Ls

= 4.5/0.24

= 18 baffles

Tube side:

ho*OD/K = 0.023*(Nre) 0.8(Npr)0.33

OD = 0.025 m

Nre = 138.75

Npr = 0.71

ho = 148.7 W/m2k

Clearance = Pt – OD

= 25.4 – 25

= 0.45 mm

Equivalent diameter = 3.29 mm (which is triangular pitch )

55
De = 8/3.14*D[ [0.5 P*0.86 P] – [0.5*3.14*P2]]

Baffle spacing = Eq.wt * Pitch/Shell ID * clearance

= 7.4 mm

PRESSURE DROP

Shell side:

f * Gs2 * Ds * Nb/2000000 * s * De *

De = 3.29 mm

Aa = DCB/Pt= 3.2 m2

Gs = m/As

= 0.11/3.22

= 0.03 kg/sm2

Nre = De * Gs/viscosity

= 2467

F = 1.87 + Nre-0.2

= 2.07

∆ = 0.66
Tube side:

In this, f = 0.079(Nre)-0.2

f = 0.011

V = Gt/ density

= 795/1110

= 0.71 m/s

f * Gt2 * Ds * Nb/2000000 * s * De *

1.2 kPa

56
8.2.1 Design Summary:

Shell side: SO2

Tube side: Ethylene glycol

Q = 206615.2 KW

LMTD = 465 °C

HT Area = 40.62 m2

Length of tube = 4.5 m

HT Area per tube = 0.32 m2 , No. of tubes = 135tubes

Velocity:

Shell side = 2.5 m/s

Tube side = 2.6 m/s

Heat transfer coefficient:

Shell side = 3119.6 W/m2k

Tube side = 148.7 W/m2k

Pressure drop:

Shell side = 0.66 kPa

Tube side = 1.2 kPa

Clearance = 0.45 mm

Baffle spacing = 7.4 mm

57
CHAPTER 9
COST ESTIMATION

58
9. COST ESTIMATION
9.1 ESTIMATION OF PURCHASED EQUIPMENT COST
PURCHASED EQUIPMENT COST

1. DIRECT COST = MATERIAL AND LABOUR INVOLVED IN ACTUAL


INSTALLATION
A. Equipment + installation + instrumentation + piping + electrical + insulation + painting
B. Buildings, process and auxiliary
C. Service facilities and yard improvements
D. Land
2. Indirect costs = expenses which are not directly involved with material and labor of actual
installation of complete facility
A. Engineering and supervision
B. Construction expense and contractor’s fee
C. Contingency
3. Fixed-capital investment = direct costs + indirect costs
4. Working capital
5. Total capital investment = fixed-capital investment + working capital
6. Manufacturing cost = direct production costs + fixed charges + plant overhead costs
A. Direct production costs
1. Raw materials
2. Operating labor
3. Direct supervisory and clerical labor
4. Utilities
5. Maintenance and repairs
6. Operating supplies
7. Laboratory charges
8. Patents and royalties

B. Fixed charges
1. Depreciation
2. Local taxes
3. Insurance
7. Rent (8-12% of value of rented land and buildings)

59
8. General expenses = administrative costs + distribution and selling costs + research and
Development costs
A. Administrative costs
B. Distribution and selling costs
C. Research and development
D. Financing

9. Total product cost = manufacturing cost + general expenses

10. Gross earnings cost = total income - total product cost

60
9.2 Equipment cost:

Table: 15
Equipment cost Cost in rupees Number of items Total cost in Rupees
Compressor 13,00,000 1 13,00,000
Chiller 5,00,000 2 10,00,000
Cyclone Separator 60,000 2 1,20,000
Packed Bed Dryer 5,00,000 2 10,00,000
Steam Boilers 10,00,000 1 10,00,000
Shell and Tube Heat
1,50,000 9 13,50,000
Exchanger
Pump 50,000 2 1,00,000
Sulphur Melter 10,00,000 1 10,00,000
Burner 15,00,000 1 15,00,000
Catalyst Bed
25,00,000 1 25,00,000
Converter
Falling Film Reactor 25,00,000 1 25,00,000
Electrostatic
6,00,000 1 6,00,000
Precipitator
Scrubber 7,00,000 1 7,00,000
Demoisturizer 4,50,000 1 4,50,000
Storage Tank 1,50,000 10 15,00,000
Total 1,66,20,000

61
9.3 CATALYST

Activated alumina per kg 500 INR.

For 400 kg=2,00,000 INR.

Vanadium pentoxide 5,500 INR

For 400 kg= 22,00, 000 INR.

Total cost of catalyst=24, 00,000 INR

9.4 DIRECT COST


INSTRUMENTATION AND CONTROL
25% OF THE PURCHASED EQUIPMENT
=16620000*0.25
=41,55,000(Rs).

PIPING
35% OF THE PURCHASED EQUIPMENT
=16620000 x 0.35
=58,17,000(Rs).

BUILDING, PROCESS AND AUXILLARY


40% OF THE PURCHASED EQUIPMENT
=16620000 x 0.40
=66,48,000(Rs).

SERVICE FACILITIES AND YARD IMPROVEMENT


60% OF THE PURCHASED EQUIPMENT
= 16620000 x 0.60
=99,72,000(Rs).

LAND
6% OF THE PURCHASED EQUIPMENT
= 16620000x 0.06
=9,97,200(Rs).

62
DIRECT COST
=41,55,000+58,17,000+66,48,000+99,72,000+9,97,200

=2,75,89,200(INR).

9.5 INDIRECT COST


ENGINEERING COST
15% OF THE DIRECT COST
= 27589200 x 0.15
= 41,38,380(INR).

CONSTRUCTION, EXPENSE AND CONTRACT


20% OF THE DIRECT COST
=27589200x 0.20
= 55,17,840(INR).

FIXED CAPITAL INVESTMENT


= DIRECT COST + INDIRECT COST
= 27589200+4138380+5517840
= 3,72,45,420(INR).

CONTINGENCE
10% OF THE FIXED CAPITAL INVESTMENT
=37245420x 0.10
= 37,24,542 (INR).

WORKING CAPITAL COST


10-20% OF THE TOTAL CAPITAL INVESTMENT
=37245420 x 0.15
= 55,86,813(INR).

9.6 TOTAL CAPITAL COST


= FIXED CAPITAL INVESTMENT + WORKING COST + CATALYST COST
= 37245420+5586813+2400000
=4,52,32,233(INR).

63
9.7 TOTAL PRODUCT COST

LABSA

TOTAL LABSA PRODUCED =1,000 kg/hr

=24,000 kg/day.

=87,60,000 kg/year.

PRICE OF LABSA = 135 (INR)/kg.

TOTAL COST OF LABSA =1,18,26,00,000 (INR)

TOTAL PRODUCTION COST


RAW MATERIAL
20% OF THE TOTAL PRODUCT COST
=1182600000 x 0.20
= 23,65,20,000(INR)

OPERATING LABOR
10% OF THE TOTAL PRODUCT COST
=1182600000 x 0.10
= 11,82,60,000(INR).

DIRECT SUPERVISORY AND CLERICAL LABOR


15% OF THE TOTAL PRODUCT COST
=1182600000 x 0.15
= 17,73,90,000 (INR)

UTILITIES
10% OF THE TOTAL PRODUCT COST
=1182600000 x 0.10
= 11,82,60,000(INR).
MAINTAINANCE AND REPAIR
6% OF THE TOTAL PRODUCT COST
=1182600000 x 0.06
= 7,09,56,000(INR).

64
OPERATING SUPPLIES
6% OF THE TOTAL PRODUCT COST
=1182600000 x 0.06
= 7,09,56,000(INR).

LABORATORY CHARGE
10% OF THE TOTAL PRODUCT COST
=1182600000 x 0.10
= 11,82,60,000(INR).
DEPRICIATION
10% OF THE FIXED CAPITAL INVESTMENT + 2% BUILDING COST
= (3,72,45,420 x 0.10) + (66,48,000x 0.02)
= 38,57,502(INR).
LOCAL TAXES
3 % OF THE FIXED CAPITAL INVESTMENT
=37245420 x 0.03
= 11,17,362.6 (INR).

INSURANCE

1 % OF THE FIXED CAPITAL INVESTMENT


=37245420 x 0.01
= 3,72,454.2(INR).

PLANT OVER HEAD COST


7% OF THE TOTAL PRODUCT COST
=1182600000 x 0.07
= 8,27,82,000(INR).

ADMINISTRATIVE COST
3% OF THE TOTAL PRODUCT COST
=1182600000 x 0.03
= 3,54,78,000(INR).

65
DISTRIBUTION AND SELLING COST
5% OF THE TOTAL PRODUCT COST
=1182600000 x 0.05
= 5,91,30,000(INR).
RESEARCH AND DEVELOPMENT
5% OF THE TOTAL PRODUCT COST
=1182600000 x 0.05
= 5,91,30,000(INR).

ELECTRICITY
It is calculated and it comes out to be 350kWhr
Take 1kWhr = Rs.8
For a day = 350*24
= 8400kWhr.
Annual cost = 8400*365*8
=2,45,28,000(INR)
9.8 TOTAL COST FOR THE PRODUCTION PER YEAR

THE PRODUCTION PER YEAR = RAW MATERIAL + OPERATING LABOR +


DIRECT SUPERVISORY AND CLERICAL LABOR + UTILITIES + MAINTAINANCE
AND REPAIR + OPERATING SUPPLIES + LABORATORY CHARGE + DEPRICIATION
+ LOCAL TAXES + INSURANCE + PLANT OVERHEAD COST + ADMINISTRATIVE
COST + DISTRIBUTION AND SELLING COST + RESEARCH AND
DEVELOPMENT+ELECTRICITY.

TOTAL COST FOR THE PRODUCTION PER YEAR


= 23,65,20,000+11,82,60,000+17,73,90,000+11,82,60,000+7,09,56,000+7,09,56,000+
11,82,60,000+38,57,502+11,17,362+3,72,454+8,27,82,000+3,54,78,000+11,17,362+
3,72,454+8,27,82,000+3,54,78,000+5,91,30,000+5,91,30,000+2,45,28,000

TOTAL COST FOR THE PRODUCTION PER YEAR=1,12,37,80,282 (INR).

66
9.9 GROSS EARNINGS = TOTAL INCOME - TOTAL PRODUCTION COST
= 1,18,26,00,000-1,12,37,80,282
= 5,88,19,718(INR).

9.10 TAX RATE


USUALLY COMMON TAX IS 40-50%
NET PROFIT PER ANNUM = 0.40 x 58819718
= 2,35,27,888(INR)
NET PROFIT PER ANNUM = 58819718(INR) – 23527888(INR)
= 3,52,91,830(INR)

9.11 PAYBACK PERIOD


PAYBACK PERIOD = TOTAL CAPITAL COST / GROSS EARNING
= 4,52,32,233 (INR) / 3,52,91,830 (INR)
= 1.28YEARS.

67
CHAPTER 10
PLANT LOCATION AND LAYOUT

68
10.1 PLANT LOCATION
The location of the plant can have a crucial effect on the overall profitability of a project, and the
scope for future expansion. Many factors must be considered when selecting a suitable plant site. The
principle factors are:
1. Location, with respect to the marketing area.
2. Raw material supply.
3. Transport facilities.
4. Availability of labor.
5. Availability of suitable land.
6. Environmental impact and effluent disposal.
7. Local community consideration.
8. Climate.
9. Political and strategic consideration.
PLANT LAYOUT
The economic construction and operation of a process unit will depend on how well the Plant
equipment specified on the process flow sheet and laid out. The principle factors to be considered:
Economic consideration: construction and operation cost.
1. The process requirement.
2. Convenience of operation.
3. Safety.
4. Future expansion.
5. Modular construction.
10.2 COST
The cost of construction can be maintained by adopting a layout that gives shortest run of connecting
pipes between equipment, and adopting the least amount of structural steel work.However, this will
not necessarily be the best arrangement for operation and maintenance.
10.3 PROCESS ECONOMICS
Economics plays an important role in any industry. The very purpose of an investor is to put his capital
into some venture so that he can earn a lot. Hence an economic analysis plays of any project I s
inevitable. In most consideration, in the selection of the alternative between equipment or process or
anything, final decision is made by making an economics. The process that has no commercial
feasibility has no significance and hence chemical engineers should have a thorough knowledge of
fundamental economics. Since the cost of the equipment is not accurately known, it is usually
estimated by various methods from the available data like the use of the cost indicates and also the
Williamson 6/10th factor by which the cost of equipment can be related to its size or capacity.

69
Since the exact determined of cost of equipment and various expenditures are difficult and never
perfect, we must use of the various pervious data available. In this project we have made an effort to
take care of various principles and steps involved in the economics analysis of a chemical plant. The
land costs, electrical costs, instrumentation costs, building costs, piping costs, steel structure, service,
building, construction expense, contact fee contingency etc., were calculated from the empirical
relations given in terms of Purchased Equipment Cost (PEC), given in Peter and Timmerhaus.
10.4 PROCESS REQUIREMENT
All the required equipment’s have to be placed properly within process. Even the installation of the
auxiliaries should be done in such a way that it’ll occupy the least space. The plant has to be closely
located to the raw material resources.
10.5 OPERATION
As the plant handles toxic and inflammable materials the operation should be carried out with full
safety precautions. Equipment that needs to have frequent operation should be located convenient to
the control room. Valves, sample points, and instruments should be located at convenient position and
height. Sufficient working space and headroom must be provided to allow easy access to equipment.
10.6 MAINTENANCE
Heat exchangers need to be sited so that the tubes bundles can be easily withdrawn for cleaning and
tube replacement. Vessels that require frequent replacement of catalysts or packing should be located
on the outside of buildings. Equipment that requires dismantling for maintenance, such as compressors
and large pumps, should be under cover.
10.7 RAW MATERIAL SUPPLY
The location of the raw materials of an industry contributes more towards the choice of plant site than
any other factor. This is especially noticeable in those industries in which the raw materials is
inexpensive and bulky and is made more compact and obtains a high bulk value.
10.8 MARKETS AND TRANSPORTATION
The existence of transportation facilities has given rise to many of the greatest trade centres of the
world. A location should be chosen, if possible which has several competition will help to maintain
low rates and given better services.
10.9 POWER AND FUEL SUPPLY
The fuel best plan is to locate near larger coal field if coal is the primary fuel or to tie up by long term
contracts sufficient gas/oil to ensure the continuity of operation over a long term.

70
10.10 WATER SUPPLY
Water for industrial purposes can be obtained from two general sources, the plants own sources or
principle supply if the demand s for water are large. It is more economical for the industry to supply its
own water such a supply may be obtained from drilled rivers, lakes, damned streams before a
company enters up on any project, it must ensure itself of as insufficient supply of water for all
industrial. Sanitary and fire demands both present and future. Water nature quality is as diverse as the
sites and regions from which it is. Water temperature and chemical characteristic such as organic and
inorganic contaminants, the relative prices are of greatest economic importance in determining the
value of water to the chemical industry. The relative importance of each of these depends upon the
service for which the water is wanted.

10.11 LABOR
Before locating any particular location a careful study of the supply of available labor must be made.
Factors to be considered in labour studies are supply. Kind , diversity, intelligence, wage scale,
regulations, efficiency and costs. The layout will bed one by the (unit areas) concept method which is
particularly well adopted to large plant layout. Unite areas are often delineated by means of distant
process phase and operational producers by reasons of contamination and by satisfy consideration
requirement. Thus the delineation of the shape and extent of a unite area and of interrelation ships of
each area in a master plot plan is one of the first take of layout planning.

71
10.12 PLANT LAYOUT DIAGRAM

Figure: 4 Plant layout diagram

72
CHAPTER 11
PROCESS SAFETY MEASURES

73
11. PROCESS SAFETY MEASURES

11.1 HAZARD IDENTIFICATION

The major constituents that are considered as hazardous in Linear Alkyl Benzene Sulphonic Acid plant
are,

1. Sulphur

2. Sulphur dioxide

3. Sulphur trioxide

4. Vanadium pentoxide

SULPHUR

Elemental sulphur dust is an irritant to eyes mucous membrane and skin .It is called as “NUISANCE
DUST”. Sulphur when stored in bulk piles of doors ,a wind may disseminate sufficient dust to cause
complaints of irritation .The use of dust tight eye protection and dust respiration guards may be used
to overcome this hazard.

SULPHUR DIOXIDE

It is colourless having characteristic odour and it has strong irritant effect on eyes , throat and upper
respiratory tract. Low concentration of SO2 cause eye irritation and coughing, high concentrations are
so irrition that voluntary exposure would not be endured. In normal operation falling film sulphonation
plant, only small SO2 escapes to atmosphere through waste gas from the plant. But this quantity will be
during start up and abnormal operating condition. Except leak in dust, SO2 is not defected in the plant
SO2 emission during the start up condition increases and proper operating and maintaining procedures
can effectively control it.

SULPHUR TRIOXIDE

Hazardous effect association with this are of two types respectively local effect on the skin and eyes
and irritation of respiratory tracts.

VANADIUM PENTOXIDE

It is used as a catalyst in contact process for the conversion of SO2 to SO3 .Dust containing V2O5 is
toxic and must not be inhaled. Exposure to vanadium pent oxide dust also produces irritation to the
eyes and respiratory tract . personnel handling the catalyst are therefore exposed to severe hazards.

74
Catalyst cleaning is a serious problem and the catalyst is removed and screened externally. Respiratory
and safety glass must be won during catalyst cleaning.

11.2 FIRST AID MEASURES


EYES
Irrigate eyes with a heavy stream of water for at least 15 -20 minutes.
SKIN
Wash immediately with plenty of soap and water. Remove all contained clothes and footwear
immediately unless stuck to skin.
INHALATION
Remove causality from exposure ensuring one’s own safety whilst doing so, seek medical attention. If
symptoms persist.
INGESTION
Do not induce vomiting .Wash out mouth with water .If conscious ,give half a litter of water to drink
immediately. If gastro – intestinal symptoms develop, consult medical Personnel.(Never give anything
by mouth to an unconscious person).

11.3 FIRE FIGHTING MEASURES


EXTINGUISHING MEDIA
Appropriate extinguishing media Dry chemical powder, alcohol resistant foam,halon(may not be
permission in some counter),CO2,water spray(fog) Unsuitable extinguishing media Water stream may
splash the burning liquid and spread fire.

SPECIAL HAZARDS ARISING FROM THE SUBSTANCE OR MIXTURE


In combustion emits toxic fumes of carbon dioxide /carbon monoxide. Biodiesel soaked rags or spill
absorbents (i.e. oil dry, propylene socks, sand, etc )can cause spontaneous combustion if stored near
combustibles and not handled properly.
ADVICE FOR FIRE FIGHTERS
Fire -fighters should use self -contained breathing apparatus to avoid exposure to smoke and vapour.
Wear protective clothing to prevent contact with skin and eyes.
Protective equipment
Fire -resistant clothing, self – contained breathing apparatus.
11.4 ACCIDENTAL RELEASE MEASURES
Personnel precautions, protective equipment and emergency procedures
For non -emergency personnel
Prevent contamination of clothes and shoes;avoid contact with the skin and eyes.

75
Eliminate all sources of ignition. If outside do not approach from downwind.Evcuate all personnel
who do not take part in the cleaning/emergency procedure. Mark out the contaminated area with signs
and prevent access to unauthorized personnel.
For emergency responders
Wear self – contained breathing apparatus. Wear protective clothing to prevent contact with skin and
eyes.
11.5 ENVIRONMENTAL PRECAUTIONS
Prevent any leakage .Do not discharge into communal sewerage, drains or waters.

METHODS AND MATERIAL FOR CONTAINENT AND CLEANING UP


Spill containment Contain any spillage using bounding
Spill clean-up
Pick up small spills with absorbent materials and dispose of properly to avoid spontaneous
combustion. Disposal must be carried out according to valid legislation on wastes and residues.
Recover large spills for appropriate treatment and reutilization or for disposal according to legislation.
Wash hard surfaces with safety solvent or detergent to remove remaining oil film. Greasy nature will
result in a slippery surface.
HANDLING AND STORAGE
Precautions for safe handling
Recommendations for safe handling
For safe handling is recommended to avoid direct contact with the substance.
Occupational hygiene advice
Do not eat, drink or smoke in work areas; wash hands after use; and remove Contaminated clothing
and protective equipment before entering eating areas.
CONDITIONS FOR SAFE STORAGE, INCLUDING ANY INCOMPATIBILITIES
Safe storage conditions
Store in cool, well ventilated area. Keep away from sources of ignition, excessive heat and oxidizing
agents. Keep container tightly closed. Storage life, ~2 years. Protect from frost. Protect against static
electricity. Store at +15°C to +25°C.
SPECIFIC END USES
The product is designed especially for use as fuel for diesel engines.
11.6 PERSONAL PROTECTIVE EQUIPMENT
Eye Protection: Wear safety glasses with side-shields. Wear chemical safety goggles with a face
shield to protect against skin and eye contact when appropriate. Provide an emergency eye wash
fountain and quick drench shower in the immediate work area. Goggles Face shield.

76
Skin and Body Protection: Wear appropriate chemical resistant clothing. When responding to
accidental release of unknown concentrations, wear one-piece, total encapsulating suit of Butyl coated
nylon or equivalent.
Hand Protection: Wear chemical resistant, insulated gloves such as Perfect Fit NL-56(TM) or Best
6781R(TM). Consult a glove supplier for assistance in selecting an appropriate chemical resistant
glove.
Respiratory Protection:
Where vapour concentration exceeds or is likely to exceed applicable exposure limits, a NIOSH
approved respirator is required. When an air-purifying respirator is not adequate or for spills and/or
emergencies of unknown concentrations, a NIOSH approved self contained breathing apparatus or
airline respirator with full-face piece is required. A respiratory protection program that meets 29 CFR
1910.134 must be followed whenever workplace conditions warrant use of a respirator.

77
Figure: 5 Personal protective equipments

78
CHAPTER 12
INSTRUMENTATION AND CONTROL

79
12. INSTRUMENTATION AND CONTROL

INTRODUCTION
The primary objectives of designer when specifying instrumentation and process control are
 Safe plant operation
 To keep the process variable within known safe operating limits
 To detect the dangerous situation as they develop and to provide alarms and automatic
 shutdown systems
 To provide interlocks and alarms to prevent dangerous operating procedures.
 Production rate. To achieve the decide product output.
 Production quality
 Cost
Processes may be controlled more precisely to view more uniform and higher quality products by the
application of automatic control often leading to higher profits. Automatic control is also Beneficial in
certain remote, hazardous operations .For manual control and operated periodically measures to give
uniform the pressure for example, below the desired value to operator increase the flow rate by
opening the value slightly. For automatic control, a pressure sensitive-device is used to produce
signal (electrical, pneumatic, etc.) proportional to the measured pressure. This is fed to a controller,
which compares it with a pre-set decide value are set point. If a difference exists, the controller
changes the opening of product control valve to control/throttle the pressure.

Good operating particles and the control system are essential for the reactor. After heat exchanges and
the distillation column to ensure high product purity, and energy efficiency, and to achieve the desired
production rate. The reactor control system is required to regulate the normal operation and provide
adequate production system against the runaway reaction caused by high operating temperature. The
control system on the recovery units are require to maintain the outlet temperature within a narrow
operating range for optimum product recovery. Other units in the plant need less sophisticated control
schemes but must guarantee safely and other operated stability. Piping throughout the plant was sized
from correlation for the economical pipe diameter based on the typical follow rate for the different
sections of plant.

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CONTROL AND INSTRUMENTATION
Three levels of control and instrumentation are required.
1. An alarm and warning system to ensure a safety of all processing units, but especially those
where there is a significant risk (example. Reaction runs away in the reactor).
2. A regularly control system for all processing unit which is used to maintain steady operation
of the process.
3. An optimizing control system which utilized advanced control techniques to maximize
profitability of the key units (E.g., the reactor after heat exchanger, distillation column and
storage tanks).
Production system need to be installed to handle emergency situation. A pressure release valve could
be installed on the reactor and would be capable of quickly reducing reactor temperature and pressure
in the event of runway. However, this would allow large quantities of hydrocarbon to enter the
atmosphere creating the secondary and possible more serious. Hazards therefore, a vent could only be
used as final emergency action and other control system must be incorporate into a design. During
normal operation, the temperature profile in the reactor should be continuously monitor and optimize
in the other to control to heat composition of the product and regulate the energy flow. High
temperature reduces the selectivity for the hydration reaction (forming ethanol) and increase the
fraction of feed that is not fully converted.

The larger reactor volume suggest that some type of feed forward control would be effective. The feed
rate temperature and composition are critical variables that will need to incorporate into the control
system. Outlet temperature from the recovery equipment is critical to the overall plant performance. A
compromise must be found between quantity (the amount of product condensed) and quality(the
amount of impurities condensed with the product).

After condensed product is ethanol along with unreacted ethylene and water. Then condensed product
must be separated from the unreacted compounds. so there sent through the pressure separators. First
is the high-pressure separator operating at 500kpa. The outlet from the condenser must be throttled to
500kpa before sending it to the high-pressure separator. A pressure controller is placed in the high-
pressure separator that sense the pressure inside the separator. And helps in sending the signal the
control the valve if any unusual condition occurs. Similarly bottom outlet from the high-pressure
separator is send to the low-pressure separator operating at 250kpa. The bottom from the low pressure
must be throttled to 250kpa. Similar pressure controller is kept in the low-pressure separator the helps
in adjusting the control valve. Consequently, there is a very narrow range of operating temperature,
and an effective control system for the after-heat exchanger is essential. Similarly, in the distillation
columns, if the temperature is too low, impurity co-condense with the product ethanol and quality is

81
reduced. However, if the outlet temperature is too high, then an excessive amount of ethanol will
escape with the effluent gas. Both recovery units need a right temperature control which may be
enhanced by using appropriate advanced control strategies. Product composition should be in regular
throughout the process. One or more process analyzers could reduce the level of sampling and testing
required and provides continuous process data.

However, significant and specialized maintenance will be required that the analyzers are calibrated
and operating accurately. Otherwise they are of little or no value to the operator. Daily sample should
be taken from the reactor inlet (to check variation in the composition which might requires process
adjustment), reactor outlet (to monitor reactor operation), the after heat exchanger products, the
ethanol product storage vessels, stripping column bottom and final product). The laboratory
turnaround should be typically less than four hours so that appropriate operating adjustments can be
made in a timely manner. Adequate control and instrumentation and good operating techniques are
essential to the overall profitability of the process. Safety should always the first objective of the
control system followed by the operability and profitability.
CONTROLLER
The control hardware required for controlling the temperature of the steam leaving at heat exchanger.
The hardware available from manufacture of such equipment consists of following component listed
here along with their respective conversions.
Transducers - Temperature to current
Controller – recorder - Current to current
Converter - Current to pressure
Control valve - Pressure to flow rate
Thermocouple is used to measure the temperature. The signal from the thermocouple is send to the
transducers which produces an input in the range of 4-20 mA, which is the linear function of input.
The output of the transducers enters the controller where it is compared to the setpoint to produce the
error signal.

The controller converts the error to an output in the range 4-20 mA according to the control law stored
in the memory of the computer. The only control we have consider for has been proportional. The
output of the controller enters the converter, which produces and output range 3-15 psig, which is the
linear function of the input. Finally, the output of the converter is send to the top of the control valve,
which adjust the flow of cooling water to the heat exchanger. The value is assumed to be linear and the
pressure is to open type. Electricity is needed for transducer, controller and converter. A source of 20
psig air is needed for the converter.

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CHAPTER 13
CONCLUSION

83
13. CONCLUSION

The general treating methods are discussed and suitable process was selected for profitable
manufacturing of Alpha Olefin Sulphonate. The process of manufacture of Alpha Olefin
Sulphonate is discussed with detailed process description. The important parameter of in the
production was explained. The required material and energy balance for the production is also
given. One packed bed converted and a pump in the manufacture of Alpha Olefin Sulphonate unit
is designed. The process layout and material safety data sheet were also explained. The
applications of the Alpha Olefin Sulphonate are analyzed and the safety limits are studied.

84
CHAPTER 14
REFERENCES

85
14. REFERENCES

COMPANY
Ultramarine and Pigments Limited, Ranipet – Vellore.

BOOKS:
1. Perry’s “Chemical Engineering Handbook” 6th Edition By Robert H. Perry & Don Green.
2. “Process Equipment Design” By M.V. Joshi, 2nd Edition.
3. “Plant Design &Economics For Chemical Engineers” 3rd Edition By Max Peters
&Timmerhaus.
4. “Heat Transfer” By M. NecatiOzisik 3rd Edition
5. “Encyclopedia Of Chemical Technologies” By Kirk –Othmer (Vol 3).
6. “Riegel’ Handbook Of Industrial Chemistry”

WEBSITES:
1. www.cpchem.com
2. en.wikipedia.org/wiki/alpha _olefins.com
3. www.infotherm.com
4. www.NIST.com
5. www.chemeo.com
6. www.upl.com

86
RESEARCH PROJECT

87
Abstract

Here the researchers conducted on waste plastic pyrolysis as an alternative method from other plastic
pyrolysis method. Plastics (HDPE, LDPE & PP) were pyrolyzed in a batch reactor laboratory
condition to produce useful fuel products. HDPE, LDPE & PP plastic wastes were completely
pyrolyzed at 240-290°C for 45 mins to obtain solid residue on bottom, liquid fuel oil, and flammable
gaseous hydrocarbon products on top. Comparison of the fuel properties to the petrodiesel fuel
standards revealed that the synthetic product was within all specifications. Notably, the fuel properties
of flash and fire point, density, GC-FID test and calorific value represented significant enhancements
over those of conventional petroleum diesel fuel.

Figure: 6 Types of plastics with codes

1. Introduction

These 7 types of Plastics have become an indispensable part in today’s world, due to their
lightweight, durability, and energy efficiency, coupled with a faster rate of production and design
flexibility; these plastics are employed in entire gamut of industrial and domestic areas; hence, plastics
have become essential materials and their applications in the industrial field are continually increasing.
At the same time, waste plastics have created a very serious environmental challenge because of their
huge quantities and their disposal problems. Waste plastic pyrolysis in liquid fuel (gasoline, diesel oil,
etc.) can effectively solve the problem of white pollution and also can alleviate the energy shortage to
a certain extent.

The plastics include polystyrene [1, 2], poly (vinyl chloride) [2, 3], polypropylene [2-4], PE
terephthalate [3], acrylonitrile-butadiene-styrene [3], and PE [1–3]. In some cases, plastics were
copyrolyzed with other materials such as waste motor oil [3]. With regard to fast pyrolysis of PE,
pyrolysis of LDPE [1], HDPE [5, 6], and various mixtures [2] was reported.

88
The pyrolysis thermally degrades the plastic component to produce an oil and gas product. This oil
may be used as a liquid fuel or returned for refining [7, 8].

Under pressure and heat, the long chain polymers of hydrogen, oxygen, and carbon decompose into
short-chain petroleum hydrocarbons with a ceiling length of around 18 carbons. Hydrocarbon
molecules from the basic materials are split under the impact of the catalytic (carbon material)
convertor inside the reactor at 70–240 0C [9].

Objective of this study was the research for production, characterization, and evaluation of alternative
pyrolysed plastic fuel from HDPE, LDPE and PP waste plastics. Comparison of our pyrolyzed oil with
conventional petroleum-derived fuels was a further objective, along with a comparison to petrodiesel
standards. Waste plastic pyrolysis oil (WPPO) were prepared and the resultant fuel properties were
measured. It is anticipated that these results will further the understanding of the applicability and
limitations of HDPE, LDPE and PP as a feedstock for the production of alternative fuel.

2. Materials and Experimental setup

Materials and Process Description

The plastic used in this study was used waste plastic covers (HDPE, LDPE) and plastic glasses (PP)
for domestic purposes. Waste plastics were washed out, waste plastics then were dried and cut into
small pieces by using scissor.

Pyrolysis process
The pyrolysis process is an advanced conversion technology that has the ability to produce a clean,
high-calorific value fuel from a wide variety of biomass and waste streams. It is the thermo-chemical
decomposition of organic material at elevated temperatures in the absence of oxygen. The pyrolysis
provides various operational, environmental and economical advantages. Under pressure and heat, the
long chain polymers of hydrogen, oxygen, and carbon decompose into short-chain petroleum
hydrocarbons with a ceiling length of around 18 carbons. Hydrocarbon molecules from the basic
materials are split under the impact of the catalytic (carbon material) convertor inside the reactor at
70–240 0C. The reduction of process temperature takes place from 500–600 0C (1atm) to 240 0C
(under pressure).

89
Distillation
The distillation is a method of separating mixtures based on differences in their volatilities. The
collected oil from pyrolysis process was found to contain various percentages of gases and various
densities of oil. The presence of the catalyst has enhanced the medium to reflux and then distilled to
obtain three fractions viz. gas, light oil, and heavy oil.

Figure: 7 Simple distillation apparatus

Experimental Setup

The shredded plastic was feed into the reactor as mixed plastics or separately. Then the reactor placed
in the electric heater. Then reactor connected with condenser. Then connect the condenser to the
distillate collecting tank, other tube connects to the immersed water tank. After the Setup were
finished then start the process. Maintain heat in the reactor by suitable insulation. The reactor is
maintained in suitable conditions.

When the process starts the plastics were get heated. Due to the boiling range and volatility of plastics
starts to condense as plastic pyrolysed oil and lube oil remains in the reactor.

The process is maintained in 270- 290 0Celsius.

After the completion of plastic conversion, the char with catalyst from the reactor are retreated,
regenerated and reused.

3. Results and discussion

The overall conversion and residue, along with the various types of liquid hydrocarbon products were
received from catalytic and non-catalytic cracking methods. The catalyst has influenced the yield and
the composition of the liquid yield. The activity of charcoal has influenced the yield up. Use of high
reduction catalyst gives higher influence to yield up.

90
PHYSICAL PROPERTIES OF OIL

Specific gravity and density


Hydrocarbons of low specific gravity can be calculated with the help of the ratio of maximum thermal
energy to the volume of oil. The formula used for finding the specific gravity is given as:
Specific gravity = density of sample/density of water
A 10 ml specific gravity bottle was used to determine the specific gravity of the samples. 10 mL of the
sample was pipette out into a pre-weighed bottle up to its brim. Thisgives the weight of the sample
which when divided by 10 gives the specific gravity and hence the density of the sample can be found
out. It was found to be having a specific gravity of 0.811 and a density of 811.7 kg/m3

Flash point
The flash point of a volatile material is the lowest temperature at which it can vaporize to form an
ignitable mixture in air. The flash point is used to determine the (1) volatility of liquid fuels, (2)
amount of low boiling fraction present in the liquid fuel, and (3) explosion hazards. The flash point of
the sample was determined using Pensky Martens closed cup flash point test. About 30 mL of the
sample was heated and stirred for every 1-degree C rise in temperature. An ignition source is directed
into the cup at regular intervals with intermittent stirring until a flash that spreads throughout the
inside of the cup is seen. The corresponding temperature is known as the flash point and was found to
be 65-degree C.

Fire point
It is the temperature at which the fuel will continue to burn for about 5 s after ignition by an open
flame source. It is the temperature at which the vapour is produced to sustain a flame. The fire point
was determined using the Pensky Martens open cup apparatus. About 30 ml of sample was heated and
stirred continuously for every 1 0C rise in temperature. An ignition source was introduced into the cup
at regular intervals until a flame sustains for at least 5 Sec. The fire point of the light fraction oil
sample was about 110 0C.

Flame characteristics
The flame characteristics of the light fraction oil were studied and this was compared with kerosene
and petrol. It was observed that there were no carbon settlements on the tiles. This suggests that the oil
from pyrolysis process has similar characteristics of petrol. Henceforth, the chemical properties of the
light fraction oil were checked by the GC-FID TPH analysis. Gas chromatography (GC-FID TPH
analysis) Gas chromatography (GC) is the group of analytical separation techniques used to analyse
volatile substances in the gas phase. Flame ionization detector (FID) is one of the most widely used

91
detectors for GC. It has a wide field of application. For instance, the fuel for air planes, kerosene, is
carefully analysed with GC-FID as a routine control. The overall complexity of the problem and of the
spectrum of hydrocarbons is likely to be encountered. It is inevitable to view TPH as a single entity.
This also relates to the sampling methodology employed. The approach consists of subdividing the
hydrocarbon into the most volatile fraction (referred as gasoline range organics or GRO) and the less
volatile less fraction. The GC-FID (TPH) for the petrol/diesel/motor oil and commercial petrol is
shown in Figs. 4a, respectively. The GC-FID (TPH) report for the oil, obtained as a result of pyrolysis,
is shown in Fig. 4b. When the GC-FID(TPH) report of the obtained oil was compared with that of the
commercial petrol, it was clearly evident that the prepared oil mainly consists of petrol components.

4. Conclusion

The current research process is technologically and economically viable for industrial scale. There is
no scarcity of feedstock as plastic waste generation has already become a habit of the modern society.
A simple catalytic and non-catalytic process for depolymerising the waste plastics (individual and
mixed plastics) to synthetic crude oil has been developed and further refined using a scale distillation
followed by condensation process. The physical and chemical properties of the light fraction oil were
done with the standard methods. The comparison of physical properties, chemical properties and gas
chromatograms suggests that the oil can be further fractionated and used as appropriate gasoline or
aviation fuel. The characterization studies by GC-FID indicate that the depolymerisation product is
essentially all straight chain hydrocarbons when linear thermoplastic polymers are used as feed. GC-
FID analysis indicates that the prepared oil includes hydrocarbons ranging from C4 to C12, a range
that includes commercial gasoline. GC-FID analysis further indicates that the pyrolysed oil has higher
percentage of petrol. The residue obtained from the distillation process can be recover and reuse t in
process.

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