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DESIGN FOR PRODUCTION OF N- BUTYL ACRYLATE FROM

PROPENE

A PROJECT REPORT

Submitted by

ARAVIIND S (2018303008)

VARSHINI KO (2018303558)

in partial fulfillment for the award of the degree

of

BACHELOR OF TECHNOLOGY

IN

CHEMICAL ENGINEERING

AC COLLEGE OF TECHNOLOGY
ANNA UNIVERSITY: CHENNAI 600 025
JUNE 2022

i
BONAFIDE CERTIFICATE

Certified that this project report “PRODUCTION OF N-BUTYL


ACRYLATE FROM PROPENE” is the bonafide work of “ARAVIIND
S(2018303008), VARSHINI KO(2018303558)” who carried out the project
work under my supervision.

SIGNATURE SIGNATURE

Dr. LIMA ROSE MIRANDA, Dr. A. BRINDA LAKSHMI,


HEAD OF THE DEPARMENT ASSOCIATE PROFESSOR
SUPERVISOR
DEPT. OF CHEMICAL ENGINEERING DEPT. OF CHEMICAL ENGINEERING
ALAGAPPA COLLEGE ALAGAPPA COLLEGE
OF TECHNOLOGY OF TECHNOLOGY
ANNA UNIVERSITY ANNA UNIVERSITY
CHENNAI – 25. CHENNAI – 25.

ii
ACKNOWLEDGEMENT
We thank our parents, friends and almighty the God for giving us the
opportunity to pursue and complete this work successfully.

We take this opportunity to thank our Head of the Department Dr. Lima
Rose Miranda, Professor and to our Dean, Dr. R. Jayavel, Professor,
Alagappa College of Technology, Anna University for permitting us to use all
the necessary facilities in the institution.

We record our special thanks to our project coordinator Dr. T. Santhosini


Priya, Assistant Professor, Department of Chemical Engineering for her constant
encouragement, guidance, and unremitting help throughout the period of study.
We are also thankful to all the other Chemical Engineering faculty members for
their kind cooperation and help.
We express our sincere and heartfelt thanks to our project guide
Dr. A. Brinda Lakshmi, Associate Professor, Department of Chemical
Engineering, Alagappa College of technology, Anna University, Chennai for
providing us the facilities, encouragement, support and who extended
maximum help to complete this piece of our work. We would like to express
our heartfelt gratitude to the entire faculty and our department staff members
who have been kind enough to render their inputs despite their busy schedule.

iii
ABSTRACT

Butyl Acrylate is one of the most important acrylic monomers presenting great
potential for several industrial applications mainly in the surface coating field. A
suitable process was selected involving heterogeneous catalysis. A plant design
simulated with the help of Aspen Plus is drafted using propene as primary
reactant. Conventional esterification methodology is replaced with Reactive
distillation.

iv
TABLE OF CONTENTS

CHAPTER TITLE PAGE


NUMBER NUMBER

ABSTRACT iv
LIST OF FIGURES viii
LIST OF TABLES x

1. INTRODUCTION 1
1.1 INTRODUCTION 1
1.2 PHYSICAL & CHEMICAL PROPERTIES 4
1.3 CHEMICAL REACTIVITY 4
1.4 MARKET DEMAND 5
1.5 APPLICATIONS 5

2. METHODS OF PRODUCTION 7
2.1 LITERATURE REVIEW 8
2.1.1 PROCESS ALTERNATES 8
2.1.2 CATALYSTS 10
2.2 PROCESS DESCRIPTION 12
2.2.1 PROPYLENE OXIDATION PROCESS 13
2.2.2 ACRYLIC ACID ESTERIFICATION PROCESS 14
2.3 JUSTIFICATION FOR THE CHOICE OF PROCESS 14
3. MATERIAL BALANCE 15
3.1 BASIS CALCULATION 16
3.2 MIXER 17
3.3 REACTOR 1 17
3.4 REACTOR 2 19
3.5 ABSORBER 21
3.6 DISTILLATION COLUMN 23
v
3.7 REACTIVE DISTILLATION COLUMN 25
4. ENERGY BALANCE 29
4.1 PREHEATER 30
4.2 REACTOR 1 32
4.3 REACTOR 2 34
4.4 HEAT EXCHANGER 35
4.5 ABSORBER 36
4.6 DISTILLATION COLUMN 38
4.7 COOLER 41
4.8 REACTIVE DISTILLATION COLUMN 42
5. EQUIPMENT DESIGN 46
5.1 DISTILLATION COLUMN 47
5.1.1 PROCESS DESIGN 47
5.1.2 MECHANICAL DESIGN 52
5.2 SHELL AND TUBE HEAT EXCHANGER 67
5.2.1 PROCESS DESIGN 67
5.2.2 MECHANICAL DESIGN 72
5.3 ABSOPRTION COLUMN 83
5.4 STORAGE VESSEL 92
5.5 PUMP 98
6. ECONOMIC ANALYSIS 105
6.1 TOTAL EQUIPMENT COST 106
6.2 TOTAL DIRECT COST 107
6.3 TOTAL INDIRECT COST 108
6.4 RAW MATERIAL COST 109
6.5 OPERATING LABOUR COST 109
6.6 TOTAL UTILITY COST 110
6.7 REVENUE FROM SALES 110
6.8 EXPENSES 111

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6.9 PROFITABILITY STUDY 111
7. PIPING AND INSTRUMENTATION DIAGRAM 113
8. SAFETY ANALYSIS 119
8.1 HAZOP ANALYSIS 120
8.1.1 INTRODUCTION 120
8.1.2 OBJECTIVES 120
8.1.3 HAZOP STUDY ON PACKED BED REACTOR 123
8.1.4 HAZOP STUDY ON HEAT EXCHANGER 125
8.1.5 HAZOP STUDY ON ABSORBER 128
8.1.6 HAZOP STUDY ON CENTRIFUGAL PUMP 130
8.1.7 HAZOP STUDY ON DISTILLATION COLUMN 132
8.2 FAULT TREE ANALYSIS 134
8.2.1 FAULT TREE ANALYSIS ON PACKED BED REACTOR 135
8.2.2 FAULT TREE ANALYSIS ON HEAT EXCHANGER 136
8.2.3 FAULT TREE ANALYSIS ON STORAGE TANK 137
8.2.4 FAULT TREE ANALYSIS ON CENTRIGUGAL PUMP 138
8.2.5 FAULT TREE ANALYSIS ON DISTILLATION COLUMN 139
9. PROCESS SIMULATION 140
10. PLANT LAYOUT 149
11. MATERIAL SAFETY DATA SHEET- N-BUTYL ACRYLATE 155
12. REFERENCES 156

vii
LIST OF FIGURES
Figure No. Name
1 MANUFACTURERS OF N-BUTYL ACRYLATE IN ABROAD AND IN INDIA

2 N-BUTYL ACRYLATE MARKET SHARE

3 PROCESS FLOW DIAGRAM FOR N-BUTYL ACRYLATE PRODUCTION

4 MASS BALANCE BLOCK DIAGRAM FOR MIXER (MIX)

5 MASS BALANCE BLOCK DIAGRAM FOR REACTOR 1 (R1)

6 MASS BALANCE BLOCK DIAGRAM FOR REACTOR 2 (R2)

7 MASS BALANCE BLOCK DIAGRAM FOR ABSORBER (ABS)

8 MASS BALANCE BLOCK DIAGRAM FOR DISTILLATION COLUMN (D1)

9 MASS BALANCE BLOCK DIAGRAM FOR REACTIVE DISTILLATION(RD)

10 OVERALL MASS BALANCE FOR N-BUTYL ACRYLATE SYNTHESIS

11 ENERGY BALANCE BLOCK DIAGRAM FOR PREHEATER (H1)

12 ENERGY BALANCE BLOCK DIAGRAM FOR REACTOR 1 (R1)

13 ENERGY BALANCE BLOCK DIAGRAM FOR REACTOR 2 (R2)

14 ENERGY BALANCE BLOCK DIAGRAM FOR HEAT EXCHANGER (HX)

15 ENERGY BALANCE BLOCK DIAGRAM FOR ABSORBER (ABS)

16 ENERGY BALANCE BLOCK DIAGRAM FOR DISTILLATION COLUMN(D1)

17 ENERGY BALANCE BLOCK DIAGRAM FOR COOLER (C1)

18 ENERGY BALANCE BLOCK DIAGRAM FOR REACTIVE DISTILLATION(RD)

19 OVERALL ENERGY BALANCE FOR N-BUTYL ACRYLATE SYNTHESIS

20 MC-CABE THIELE PLOT FOR THE SYSTEM

21 EQUIPMENT DESIGN FOR DISTILLATION COLUMN

22 EQUIPMENT DESIGN FOR SHELL AND TUBE HEAT EXCHANGER

23 EQUIPMENT DESIGN FOR STORAGE TANK

24 ILLUSTRATION OF CONNECTIONS INVOLVED FOR PUMP DESIGN

25 PUMP PERFORMANCE CURVE FOR A RANGE OF PUMPS

26 EXTENDED PUMP PERFORMANCE CURVE FOR SELECTED PUMP

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27 P&ID FOR N – BUTYL ACRYLATE SYNTHESIS

28 FAULT TREE ANALYSIS OF PACKED BED REACTOR

29 FAULT TREE ANALYSIS OF SHELL AND TUBE HEAT EXCHANGER

30 FAULT TREE ANALYSIS OF STORAGE TANK

31 FAULT TREE ANALYSIS OF CENTRIFUGAL PUMP

32 FAULT TREE ANALYSIS OF DISTILLATION COLUMN

33 COMPONENTS AND SELECTED MODEL FOR THE PROCESS

34 RAW MATERIALS STREAMS

35 HEATER H1 STREAM RESULTS

36 REACTORS STREAM RESULTS

37 ABSORBER STREAM RESULTS

38 DISTILLATION STREAM RESULTS

39 REACTIVE DISTILLATION STREAM RESULTS

40 PLANT LAYOUT FOR N – BUTYL ACRYLATE SYNTHESIS

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LIST OF TABLES
Table No. Name
1 N-BUTYL ACRYLATE MANUFACTURERS IN INDIA
2 N-BUTYL ACRYLATE MANUFACTURERS ABROAD
3 PROCESS ALTERNATES FOR ACRYLIC ACID PRODUCTION
4 MOLECULAR WEIGHTS OF COMPOUNDS INVOLVED
5 MASS BALANCE SPREADSHEET FOR MIXER (MIX)
6 MASS BALANCE SPREADSHEET FOR REACTOR 1 (R1)
7 MASS BALANCE SPREADSHEET FOR REACTOR 2 (R2)
8 MASS BALANCE SPREADSHEET FOR ABSORBER (ABS)
9 MASS BALANCE SPREADSHEET FOR DISTILLATION COLUMN (D1)
10 MASS BALANCE SPREADSHEET FOR REACTIVE DISTILLATION (RD)
11 STANDARD HEATS OF FORMATION OF COMPOUNDS INVOLVED
12 ENERGY BALANCE SPREADSHEET FOR PREHEATER (H1)
13 ENERGY BALANCE SPREADSHEET FOR REACTOR 1 (R1)
14 ENERGY BALANCE SPREADSHEET FOR REACTOR 2 (R2)
15 ENERGY BALANCE SPREADSHEET FOR ABSORBER (ABS)
16 ENERGY BALANCE SPREADSHEET FOR DISTILLATION COLUMN (D1)
17 ENERGY BALANCE SPREADSHEET FOR REACTIVE DISTILATION(RD)
18 VAPOUR LIQUID EQUILIBRIUM DATA FOR THE SYSTEM
19 ESTIMATED SURFACE TENSION VALUES
20 PROPERTIES OF COMPOUNDS FLOWING IN SHELL AND TUBE SIDE
21 PARAMETERS INVOLVED IN ABSORPTION COLUMN
22 MECHANICAL FACTORS FOR ABSORPTION COLUMN DESIGN
23 PUMP HEAD VALUES
24 PUMP MINOR LOSSES
25 TOTAL EQUIPMENT COST ESTIMATION
26 TOTAL DIRECT COST ESTIMATION
27 TOTAL INDIRECT COST ESTIMATION
28 RAW MATERIAL COST ESTIMATION
29 OPERATING LABOUR COST ESTIMATION
30 GUIDE WORDS FOR HAZOP ANALYSIS

x
31 GUIDE WORD WITH ASSOCIATED PARAMETERS
32 HAZOP ANALYSIS OF PBR – NODE 1
33 HAZOP ANALYSIS OF PBR – NODE 2
34 HAZOP ANALYSIS OF SHELL AND TUBE HEAT EXCHANGER
35 HAZOP ANALYSIS OF ABSORBER
36 HAZOP ANALYSIS OF CENTRIFUGAL PUMP
37 HAZOP ANALYSIS OF DISTILLATION COLUMN
38 LIST OF SYMBOLS USED IN FAULT TREE ANALYSIS

xi
CHAPTER - 1
INTRODUCTION

1
1.1 INTRODUCTION:

Butyl Acrylate is an important intermediate organic compound with the


formula C4H9O2CCH=CH2. An acrylate ester obtained by the formal
condensation of the hydroxyl group of butan-1-ol with the carboxyl group of
acrylic acid with water as byproduct. Butyl acrylate is a colorless liquid with a
sharp odor. It is readily miscible with most organic solvents. It is commercially
used in large scale as precursor in paints, sealants, coatings, adhesives, fuel,
textiles and plastics. At commercial scale, n-BA is produced in a multi-stage
process using two reactors. The most common strong acidic homogeneous
catalyst used is sulfuric acid.

Preferred IUPAC name is Butyl prop-2-enoate. Some other names are n-


Butyl Acrylate, Butyl ester of acrylic acid, Butyl-2-propenoate.

Fig.1 - MANUFACTURERS OF N-BUTYL ACRYLATE IN ABROAD AND IN INDIA:

2
Table. 1 – N-Butyl Acrylate Manufacturers in India

S No Manufacturer Phase Location

1 Hwatsi Chemical Pvt Ltd Liquid Gujarat

2 Nutrichem Products Liquid Mumbai

3 Alpha Chemika Liquid Mumbai

4 National Analytical corporation - Liquid Mumbai


chemical division

5 Moonex technology Liquid Haryana

6 Maheswari Organochem Liquid Tamil Nadu

7 Chemex Liquid Mumbai

Table. 2 – N-Butyl Acrylate Manufacturers abroad

S No Manufacturer Location

1 Technichem, Inc. USA

2 ICC Industries B.V Netherlands

3 Luyunjia Chemistry Xiamen Ltd China

4 Sancai Industry Co.,Ltd. China

5 Simagchem Corporation China

6 Hangzhou J&H Chemical Co., Ltd. China

3
1.2 PHYSICAL & CHEMICAL PROPERTIES:

 Physical State at 15° C and 1 atm: Liquid


 Molecular Weight: 128.17
 Boiling Point at 1 atm: 299.8°F = 148.8°C = 422.0°K
 Freezing Point: –83°F = –64°C = 209°K
 Critical Temperature: 620.6°F = 327°C = 600.2°K
 Critical Pressure: 426 psia = 29 atm = 2.9 MN/m2
 Specific Gravity: 0.899 at 20°C (liquid)
 Liquid Surface Tension: (est.) 20 dynes/cm = 0.020 N/m at 27°C 9.
 Liquid Water Interfacial Tension: (est.) 60 dynes/cm = 0.060 N/m at 27°C
 Vapor (Gas) Specific Gravity: Not pertinent
 Ratio of Specific Heats of Vapor (Gas): 1.080 12.
 Latent Heat of Vaporization: 120 Btu/lb = 66.4 cal/g = 2.78 X 105 J/kg
 Heat of Combustion: –13,860 Btu/lb = –7700 cal/g = –322.4 X 105 J/kg
 Heat of Decomposition: Not pertinent
 Heat of Solution: Not pertinent
 Heat of Polymerization: –25.9 Btu/lb = –144 cal/g = –6.03 X 105 J/kg
 Heat of Fusion: Currently not available
 Reid Vapor Pressure: 0.2 psia

1.3 CHEMICAL REACTIVITY:

 Reactivity with Water: No reaction


 Reactivity with Common Materials: No reaction
 Stability During Transport: Stable
 Neutralizing Agents for Acids and Caustics: Not pertinent
 Polymerization: Will polymerize on application of heat; uncontrolled bulk
polymerization can be explosive.

4
 Inhibitor of Polymerization: Methyl ether of hydroquinone: 15-100 ppm.
Store in contact with air.
1.4 MARKET DEMAND AND APPLICATION:
Butyl acrylate demand is anticipated to increase in the next ten years with
a CAGR of 4.91% and influenced by GDP. GDP rises rapidly in developing
countries and so demand will also have a similar trend.
Oil-based paints release more hazardous VOC than water-based (acrylic)
paints. Since butyl acrylate is a constituent of the latter, its market has scope.Butyl
acrylate is extensively used in adhesives like pressure-sensitive adhesives,
automobile coating, varnishes and finishes for paper, textiles and leather.The high
purity segment is expected to expand at a significant growth rate during the
forecast period. Based on application, the global butyl acrylate market has been
classified into paints & coatings, adhesives & sealants, chemical synthesis, plastic
additives, textiles, and others. The other segment includes pulp & paper
applications and leather processing. Butyl acrylate is utilized extensively in the
production of plastic compounds. Butyl acrylate is also used in the production of
industrial textile materials and apparel.

1.5 APPLICATIONS:
Fig.2

5
 Paint And Surface Coatings:

High quality and durable acrylic emulsions have revolutionized the paint
industry. Acrylics now account for over 25 percent of the global paint and
coatings market, with ongoing displacement of solvent-borne acrylics and alkyds.
Polymeric binders based on butyl acrylate exhibit lower water absorption, higher
resistance to hydrolysis, and good wet scrub resistance. All acrylic systems based
on BA are preferred for outdoor use, particularly paints and coatings that have a
low pigment content, such as varnishes, wood stains and high gloss paints.

 Co-Polymer Design:

n-BA combination with other polymerization monomers often results in the


design of numerous other co-polymers.BA co-polymer formulations often
contain four or more different co-monomers. Butyl acrylate is the principle
acrylic ester monomer polymerized with methyl methacrylate, styrene, and vinyl
acetate monomer to obtain the requisite degrees of hardness, flexibility, and
toughness in a copolymer system.

 Adhesives And Sealants:

The adhesive properties of acrylic copolymers can be widely varied and are
defined by both the adhesive strength and cohesive strength. For pressure-
sensitive adhesives, tack is the other dominant property, most associated with low
co-polymer Tgs. Variations in BA co-monomer composition can change both the
surface (adhesive) and bulk (cohesive properties). The “soft,”, lower -Tg
monomers like BA contribute to the adhesive properties

 Textile Industry:

Textile industry products which contain butyl acrylate are fibers, warp sizing ,
thickener, and back coat formulations.

6
CHAPTER – 2
METHODS OF PRODUCTION

7
2.1 LITERATURE REVIEW:
2.1.1 Process Alternates:
Process Reactants Catalysts and Operating Issues involved
conditions

Propylene Propene Acid -


Oxidation

Reppe process Acetylene Acid + Nickel Carbonyl Toxic and


40ºC corrosive
14 MPa catalyst

Ketene process Acetic Acid - Carcinogenic


(or) intermediates
Acetone

Propene Acrylonitrile - Lower yield.


ammoxidation NH4HSO4
waste disposal.

Ethylene Ethylene oxide + H2SO4 HCN and


Cyanohydrin HCN NH4HSO4
process waste disposal.

Thermal Polypropiolactone Heat Economic cost


Depolymerization (from ethylene 220ºC rise
oxide)

Table. 3 – Process alternates for Acrylic Acid

Ethylene Cyanohydrin Method: This process involves the acidic hydrolysis


and dehydration of ethylene cyanohydrin (from ethylene oxide and hydrogen

8
cyanide) and the removal of the product from the reaction mixture by distillation.
Like all other preparation of polymerizable monomers, care must be exercised
to remove the product from the reaction mixture and either inhibit or
appropriately cool it before uncontrolled polymerization can ensue.

Propiolactone Method: This commercial method is based on the


polymerization of propiolactone and the destructive distillation of this polymer
to form acrylic acid.

Carbonyl Reaction: Basic raw materials in the preparation of acrylic acid by


the carbonyl reaction are acetylene carbon monoxide (supplied as such or in the
form of nickel carbonyl), and water.

Stoichiometric Carbonyl Reaction: The reaction is very rapid at atmospheric


pressure and at mild temperature. The hydrogen shown in the accompanying
equation does not appear in gaseous form but is consumed by side reactions.

Catalytic Carbonyl reaction: The catalytic reaction requires elevated


temperature and super atmospheric pressures. Nickle salts or complexes thereof
are used as catalysts.

Propylene Method: This recently developed process involves the oxidation of


propylene to hydroxy propionic acid: oxides of nitrogen or nitric acid act as
catalyst for the reaction. Subsequent dehydration yields acrylic acid. An
alternative route is the catalytic oxidation to acrolein, CH2CHCHO , and then
to acrylic acid with oxygen and certain metallic catalyst such as Mo, Co, or Ce.

Acrylic Ester Method: This method is hampered by the ready polymerizable


of the starting material, and the low boiling points of the most available esters
and the formed alcohols as compared with that of the product, acrylic acid. It is

9
generally preferable to saponify the ester to form the corresponding salt.
Neutralizing the calcium salt with sulphuric acid, removing precipitated calcium
sulfate by a difficult filtration procedure, and obtaining the formed acrylic acid
in aqueous concentrate. Treating an aqueous solution of sodium salt with ion-
exchange resin to remove sodium ions, removing the resin by filtration, and
obtaining an aqueous concentrate of acrylic acid.

Vinyl Grignard Method: This interesting synthesis involves the use of the
well-known carboxylation of a Grignard reagent to form the acid.

2.1.2 Catalysts:
 Amberlyst 15:
This is non-toxic, heterogenous making it easy for separation. It
is macro-porous with high H+ exchange capacity (4.7 mequiv /g) and
surface area (42 m2/g). Since it is thermally unstable above 120 oC and
hence unsuitable for usage in reactive distillation unit.
 p-TSA: (para-Toluene sulfonic acid)
It has high activity and acidity of 5.8 mmol/g. It is preferred for
homogeneous aqueous phase reactions. Hence separation of
catalysts poses problems.
 Nafion:
It has acidity of 0.8 mmol/g and surface area of 0.02 m2/g. But it
is costly.
 Amberlyst 131:
It has excellent strength with lower pressure drop, longer catalyst
life, exchange capacity of 1.8 meq/ml. Since the chemical activity and
thermal stability are high, it is preferred over other catalysts.

10
11
LEGENDS:
D1 - Distillation Column
H1 - Preheater
R1 - Reactor 1
RD - Reactive Distillation
R2 - Reactor 2
C2 - Coolers

Fig. 3 - Process Flow Diagram for n-Butyl Acrylate Synthesis from Propene
HX - Shell And Tube Heat Exchanger

HFIN/HFOUT – Hot Fluid In/Out (Water)


CFIN/CFOUT - Cold Water In/Out (Water)
2.2 PROCESS DESCRIPTION:
2.2.1 Propylene oxidation process:

The usual mechanism for producing AA utilizes a two-step process in


which propylene is first oxidized to acrolein and then further oxidized to AA.
Each reaction step usually takes place over a separate catalyst and at different
operating conditions. The reaction stoichiometry and side reactions are given
below:

C3H6 +O2 C3H4O + H2O (Acrolein)

C3 H4 +1/2O2 C3 H4 O2 (Acrylic Acid)


C 3H 4O + 7/2O2 3 CO2 + 2H2 O

C 3H4 O +3/2 O2 C2 H4 O2 + CO2 (Acetic Acid)


C3 H6 + 9/2O2 3 CO2 + 3 H2 O

Therefore, the typical process set-up consists of a two-reactor system with


each reactor containing a separate catalyst and operating at conditions to
maximize the production of AA. The first reactor typically operates at a higher
temperature than the second unit. The catalyst used here are molten salts,
Bi2Mo3O12 in reactor 1 and VMo3O11 in reactor 2.

The oxidation process flow sheet shows equipment and typical operating
conditions. The reactors are of the fixed-bed shell-and-tube type (about 3-5m
long and 2.5cm in diameter) with a molten salt coolant on the shell side. The
tubes are packed with catalyst, a small amount of inert material at the top serving
as a preheater section for the feed gases. Vaporized propylene is mixed with
steam and air and fed to the first stage reactor. The preheated gases react
exothermically over the first-stage catalyst with the peak temperature in the
range of 330-430 C, depending on conditions and catalyst selectivity. At the end
of the catalyst bed, the temperature of the mixture drops toward that of the
12
molten salt coolant. The acrolein rich gaseous mixture containing some acrylic
acid is then passed to the second stage reactor, which is like the first stage reactor
but packed with catalyst designed for selective conversion of acrolein to acrylic
acid. Here the temperature peaks in the range of 280- 360 c depending on
condition. The temperature of the effluent from the second stage reactor again
approximates that of the salt coolant. The heat of reaction is recovered as steam
in external waste heat boiler. The process is operated at the lowest
temperature consistent with high conversion. Conversion increases with
temperature: the selectivity generally decreases only with large increase in
temperature.

The first unit product stream enters is the absorption tower, which
quickly lowers the temperature of entering stream from about 220 c to 80 c.
The purpose is to put the acrylic acid into a cool, liquid state that will not readily
dimerize. Also, this separates out the gaseous material in the product stream
such as nitrogen, carbon dioxide, oxygen, and propylene. These components exit
out the top along with some fugitive acrylic and acetic acid that is still in the
vapor phase. The gases entering the gas absorber are absorbed using deionized
water. The water absorbs the acrylic and acetic acids and allows the other gases
to continue to an incinerator to be burned. The aqueous effluent from the bottom
of the absorber is 20 - 30 % acrylic acid which is sent to the recovery column.
The overall yield of acrylic acid in the oxidation reaction steps is in the range of
73 - 83 % depending on the catalysts and condition employed. It is fed into the
acid tower. The acid tower is a distillation column that again operates in vacuum
conditions. The acetic acid leaves the top, while the acrylic acid leaves in the
bottoms. Both the acrylic and acetic acids are warmed and compressed to normal
pressure levels. Both now meet the given requirements. Namely, that acrylic
acid must be 99% pure and that acetic acid must be 95% pure. The top stream is
sent to wastewater treatment.
2.2.2 Acrylic acid esterification process:

13
Now, acrylic acid joins with n-Butanol to give butyl ester our desired
product n-Butyl acrylate. This reaction takes place in REACTIVE
DISTILLATION UNIT. The top product of the RD UNIT will be mixture of n-
Butanol and water. The bottom product will be n-Butyl acrylate with purity of
90-93%.
The equilibrium esterification reaction between n-Butanol and Acrylic Acid
with formation of water and n-BA is described below. Due to operation at
relatively low temperatures and low residence times, it is considered that this is
the only reaction that takes place in the system. Catalyst used here is
AMBERLYST 131.
𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 + 𝑛𝑛 − 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 − −→ 𝑛𝑛 − 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 + 𝐻𝐻2𝑂𝑂
2.3 JUSTIFICATION FOR THE CHOICE OF PROCESS:
Propene oxidation process is economically feasible because propylene is
one of the conventional reactants. Its cost is relatively lower than the reactants
used for alternate processes, like acetylene and acrylonitrile. Also, disposal issues
are minimal, and the catalyst is innocuous in this process.
Acrylic acid can be easily transported as a poly propiolactone. This
polymer is produced from ethylene oxide and acrylic acid is produced by thermal
depolymerization. This process is rejected since ethylene oxide is highly unstable
with severe health hazards in comparison to propene. Also, acrylic acid is not the
final product, its transport is not necessary.
The current production of butyl acrylate through conventional processes
involves lots of challenges, are very cost intensive, are complex in
thermodynamic behavior and has a high risk of polymerization. The Reactive
distillation simplifies and integrates reaction and separation under one unit. The
RD-AD (azeotropic distillation) Process is an efficient process intensification
strategy and has key advantages like reduced Total Annual Cost, improved
separation efficiency, significant energy savings and improved selectivity.

14
CHAPTER 3
MATERIAL BALANCE

15
3.1 BASIS CALCULATION:

Product (Butyl acrylate) production rate = 185 tons/day

= 60 kmol/hr

From literature, Propylene: Air (22% O2): Steam = 1:8.75: 1.09

Reactant yield with respect to propene to be 52.4 %

Reactant (Propene) required = 60/0.524 = 114.37 kmol/hr

O2 required = 8.75*114.37*0.22 = 230 kmol/hr

Steam required = 1.09*114.37 = 124.66 kmol/hr


Table. 4 – Molecular weight of compounds involved

S.NO Compound Molecular weight (g/gmol)

1. Propene 42.08

2. O2 32

3. Steam/water 18

4. Acrolein 56.06

5. Acrylic Acid 72.06

6. Di isopropyl ether 102.18

7. CO2 44

8. Acetic Acid 60

9. N2 14

10. n-Butanol 74.121

11. n-Butyl acrylate 128.17

16
3.2 Mixer-MIX:

Propene 114.37 kmol/hr


Propene 114.37 kmol/hr
Steam 124.66 kmol/hr
Steam 124.66 kmol/hr O2 230 kmol/hr
N2 700.22 kmol/hr
O2 230 kmol/hr
N2 700.22 kmol/hr

Fig. 4 – Mass Balance Block Diagram for Mixer (MIX)

Table. 5 – Mass Balance Spreadsheet for Mixer

Streams MASS IN MASS OUT

kg/hr kmol/hr kg/hr kmol/hr

Propene 4812.76 114.37 4812.76 114.37

O2 7359.724 230 7359.724 230

N2 19615.6 700.2199999 19615.6 700.2199999

Steam 2245.7 124.66 2245.7 124.66

TOTAL (kg/hr) 34027.7 34027.7

3.3 REACTOR1-R1:

Reactions in reactor 1 are:

𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂 + 𝐻𝐻2 𝑂𝑂 (PDT: Acrolein) ---selectivity-70%


3
𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂2 + 𝐻𝐻2 𝑂𝑂 (PDT: Acrylic acid) ---selectivity-11%
2

5
𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 𝐶𝐶2 𝐻𝐻4 𝑂𝑂2 + 𝐻𝐻2 𝑂𝑂 + 𝐶𝐶𝑂𝑂2 (PDT: Acetic acid) ---selectivity-9.5%
2

9
𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 3𝐻𝐻2 𝑂𝑂 + 3𝐶𝐶𝑂𝑂2 (PDT: CO2) --- selectivity-9.5%
2

Catalyst used: Bi2Mo3O12

17
114.37 kmol propene/hr 56.1576 kmol O2/hr
230 kmol O2/hr 700.21 kmol N2/hr
700.21 kmol N2/hr 80.059 kmol Acrolein/hr
124.66 kmol Steam/hr 12.5807 kmol acrylic acid/hr
42.3169 kmol CO2/hr
11.437 kmol acetic acid/hr
134.957 kmol H2O/hr

Fig. 5 – Mass Balance Block Diagram for Reactor 1 (R1)

Equations : (Total = 6)

Acrolein , Acrylic acid, Acetic acid and CO2 are represented by 1, 2, 3 and 4
respectively.

F represents molar flow rate.

(Fout)1 = (Fin)prop * X * S1

(Fout)2 = (Fin)prop * X * S2

(Fout)3 = (Fin)prop * X * S3

(Fout)4 = (Fin)prop * X * S4

(Fout)H20 = (Fout)1 +(Fout)2 + (Fout)4

(Fout)O2 = (Fin)O2 –[(Fout)1 +(Fout)2 *1.5 + (Fout)3 *2.5]+ [(Fout)4 -(Fout)3 ]*4.5/3

Known variables – X, S1, S2, S3, S4, (Fin)prop, (Fin)O2 (Total = 7)

Propene conversion, X=1

Acrolein Selectivity, S1=0.7

Acrylic acid selectivity, S2=0.11

Acetic acid selectivity, S3=0.095

CO2 selectivity, S4=0.095

(Fin)prop = 114.37 kmol/hr

18
(Fin)O2 = 230 kmol/hr

Unknown variables - X, S1, S2, S3, S4, (Fin)prop, (Fin)O2, (Fout)1, (Fout)2, (Fout)4, (Fout)3,
(Fin)prop, (Fout)H20 [Total = 13]

DOF = Unknown variables – Equations – Known variables = 13-6-7 = 0


Table. 6 – Mass Balance Spreadsheet for Reactor 1 (R1)

Streams MASS IN MASS OUT

kg/hr kmol/hr kg/hr kmol/hr

Propene 4812.76 114.37 0 0

O2 7359.724 230 1796.98 56.1576

N2 19609.6 700.2199999 19609.6 700.2199999

Steam 2245.7 124.66 2245.7 124.66

Acrolein 0 0 4488.44 80.059

Acrylic acid 0 0 906.61 12.5807

CO2 0 0 1862.36 42.3169

Acetic acid 0 0 686.821 11.437

H2O 0 0 2431.28 134.957

TOTAL (kg/hr) 34027.7 34027.7

3.4 REACTOR 2-R2:

Reactions in reactor 2 are:


1
𝐶𝐶3 𝐻𝐻4 𝑂𝑂 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂2 (PDT: Acrylic acid) ---conversion-98%
2

3
𝐶𝐶3 𝐻𝐻4 𝑂𝑂 + 𝑂𝑂2 → 𝐶𝐶2 𝐻𝐻4 𝑂𝑂2 + 𝐶𝐶𝑂𝑂2 (PDT: Acetic acid+CO2) ---conversion-2%
2

Catalyst used: VMO3O11

19
56.1576 kmol O2/hr 14.526 kmol O2/hr
700.21 kmol N2/hr 700.21 kmol N2/hr
80.059 kmol Acrolein/hr 91.0385 kmol acrylic acid/hr
12.5807 kmol acrylic acid/hr 43.918 kmol CO2/hr
42.3169 kmol CO2/hr 13.038 kmol acetic acid/hr
11.437 kmol acetic acid/hr 134.957 kmol H2O/hr
134.957 kmol H2O/hr

Fig. 6 – Mass Balance Block Diagram for Reactor 2 (R2)

Acrylic acid and Acetic acid are represented by 1 and 2 respectively.

F deontes molar flow rate

Equations : (Total = 5 )

(Fout)1 = (Fin)Acrol * X * S1 +(Fin)1

(Fout)2 = (Fin)Acrol * X * S2+(Fin)2

(Fout)CO2 =(Fout)2 + (Fin)CO2

(Fout)H20 = (Fin)H2O

(Fout)O2 = (Fin)O2 –[(Fout)1 *0.5+(Fout)2 *1.5]

Known variables - X, S1, S2, (Fin)Acrol, (Fin)O2, (Fin)H2O, (Fin)CO2, (Fin)1, (Fin)2 (Total
= 9)

Acrolein conversion, X=1

Acrylic acid selectivity, S1=0.98

Acetic acid selectivity, S2=0.02

(Fin)Acrol = 80.059 kmol/hr

(Fin)O2 = 56.1576 kmol/hr

(Fin)H2O = 134.957 kmol/hr

20
(Fin)CO2 = 42.3169 kmol/hr

(Fin)1 = 12.5807 kmol/hr

(Fin)2 = 11.437 kmol/hr

Unknown variables - X, S1, S2, (Fin)Acrol, (Fin)O2, (Fin)H2O, (Fin)CO2, (Fin)1, (Fin)2 ,
(Fout)O2, (Fout)1, (Fout)2, (Fout)H20, (Fout)CO2 [Total = 14]

DOF = Unknown variables – Equations – Known variables = 14-9-5 = 0


Table. 7 – Mass Balance Spreadsheet for Reactor 2 (R2)

Streams MASS IN MASS OUT

kg/hr kmol/hr kg/hr kmol/hr

Propene 0 0 0 0

O2 1796.98 56.1576 464.844 14.52692

N2 19609.6 700.2199999 19609.6 700.2199999

Steam 2245.7 124.66 2245.7 124.66

Acrolein 4488.44 80.059 0 0

Acrylic acid 906.61 12.5807 6560.56 91.0385

CO2 1862.36 42.3169 1932.825 43.91808

Acetic acid 686.821 11.437 782.976 13.03818

H2O 2431.28 134.957 2431.28 134.957

TOTAL 34027.7 34027.7


(kg/hr)

3.5 Absorber-ABS:

Equations : (Total = 3 )

L1 + G1 = L2 + G2

21
x1 L1 + y1,A G1 = x2,A L2 + y2,A G2

x1 L1 + y1,B G1 = x2,B L2 + y2,B G2

where, A is Acrylic acid

B is Acetic acid

1 and 2 are top and bottom respectively.


14.485 kmol O2/hr
699.214 kmol N2/hr
0.0048 kmol acrylic acid/hr
43.532 kmol CO2/hr
0.2441 kmol acetic acid/hr
79.2681 kmol H2O/hr
140.991 kmol H2O/hr

14.526 kmol O2/hr


700.21 kmol N2/hr 91.0336 kmol acrylic acid/hr
91.0385 kmol acrylic acid/hr 12.794 kmol acetic acid/hr
43.918 kmol CO2/hr 196.68 kmol H2O/hr
13.038 kmol acetic acid/hr 0.04346 kmol O2/hr
134.957 kmol H2O/hr 0.3858 kmol CO2/hr
0.78647 kmol N2/hr

Fig. 7 – Mass Balance Block Diagram for Absorber (ABS)

Known variables - x1, G2, y1,A, y1,B, x2,A, x2,B, G1, L2 [ Total – 8]

x1 = 0 ( pure water)

G2 = 1192.3 kmol/hr

y1,A = 0

y1,B = 0

x2,A= 0.215

x2,B = 0.028

G1 = 837.72 kmol/hr

22
L2 = 421.6 kmol/hr

Unknown variables - x1, G2, y1,A, y1,B, x2,A, x2,B, G1, L2, L1, y2,A, y2,B (Total = 11)

DOF = Unknown variables – Equations – Known variables = 11-8-3= 0


Table. 8 – Mass Balance Spreadsheet for Absorber (ABS)

Streams MASS IN MASS OUT

9 VENTGAS(TOP) ABS-BOTTOM

kg/hr kmol/hr kg/hr kmol/hr kg/hr kmol/hr

O2 464.844 14.52692 463.453 14.4835 1.39088 0.04346

N2 19609.6 700.219 19587.4 699.214 22.0318 0.78647

Steam 2245.7 124.66 0.00605 0.000336 2245.7 124.66

Acrylic acid 6560.56 91.0385 0.3518 0.00488 6560.21 91.0336

CO2 1932.825 43.91808 1915.84 43.5322 16.9187 0.3858

Acetic acid 782.976 13.03818 14.6604 0.24412 768.316 12.7941

H2O 2431.28 134.9 + 1428.04 79.2681 3543.24 196.68


+ 2540 140.9 =

= 4971 275.948

Total (kg/hr) 34027.7+2540 = 23409.8+13158 = 36567.7


36567.7

3.6 DISTILLATION COLUMN -D1:

Equations : (Total = 4)

F=D+B

xF,1 F = xD,1 D + xB,1 B

23
xF,2 F = xD,2 D + xB,2 B

xF,3 F = xD,3 D + xB,3 B

where 1, 2 and 3 are acrylic acid, acetic acid and solvent respectively
0.04346 kmol O2/hr
0.3858 kmol CO2/hr
0.78647 kmol N2/hr
6.04229 kmol acrylic acid/hr
12.509 kmol acetic acid/hr
196.68 kmol H2O/hr

91.0336 kmol acrylic acid/hr


12.794 kmol acetic acid/hr 84.9913 kmol acrylic acid/hr
196.68 kmol H2O/hr 0.2846 kmol acetic acid/hr
0.04346 kmol O2/hr
0.3858 kmol CO2/hr
0.78647 kmol N2/hr

Fig. 8 – Mass Balance Block Diagram for Distillation Column (D1)

Table. 9 – Mass Balance Spreadsheet for Distillation Column (D1)

STREAMS MASS IN MASS OUT

ABS-BOTTOM D1 DIST D1 BOTTOM

kg/hr kmol/hr kg/hr kmol/hr kg/hr kmol/hr

O2 1.39088 0.04346 1.39088 0.04346 0 0

N2 22.0318 0.78647 22.0318 0.78647 0 0

Steam 2245.7 124.66 2245.7 124.66 0 0

Acrylic acid 6560.21 91.0336 435.429 6.04229 6124.78 84.9913

CO2 16.9187 0.3858 16.9187 0.3858 0 0

Acetic acid 768.316 12.7941 751.221 12.5094 17.0944 0.28465

24
H2O 3543.24 196.68 3543.24 196.68 0 0

Total (kg/hr) 13158 7016.07+6141.88 = 13158

Known Variables – F, XF,1, XF,2, XF,3, XB,1, XB,2, XB,3, B [ Total – 8 ]

F = 422 kmol/hr

XF,1 = 0.21

XF,2 = 0.028

XF,3 = 0.0023

XB,1 = 0.257

XB,2 = 0.026

XB,3 = 0

B = 343.437 kmol/hr

Unknown variables – F, XF,1, XF,2, XF,3, XB,1, XB,2, XB,3, B, D, XD,1, XD,2, XD,3
(Total = 12)

DOF = Unknown variables – Equations – Known variables= 12-8-4 = 0

3.7 REACTIVE DISTILLATION:


84.9913 kmol n-Butanol/hr

0.28465 kmol acetic acid/hr


6.9156 kmol acrylic acid/hr
5.8377 kmol n-Butanol/hr
11.912 kmol n-BA/hr
78.075 kmol H2O/hr
84.9913 kmol acrylic acid/hr
0.2846 kmol acetic acid/hr
0.0001 kmol acrylic acid/hr
1.077 kmol n-Butanol/hr
66.163 kmol n-BA/hr
Fig. 9 – Mass Balance Block Diagram for Reactive Distillation (RD)

25
Equations : (Total = 4)

Here mass basis is considered

F+ Gen=D+B+Con

xF,1 F +(Gen)1 = xD,1 D + xB,1 B+ (Con)1

xF,2 F +(Gen)2 = xD,2 D + xB,2 B+ (Con)2

xF,3 F +(Gen)3 = xD,3 D + xB,3 B+ (Con)3

where 1 and 2 are Acrylic acid, Butanol and Butyl acrylate respectively

Known Variables - F, XF,1, XF,2, XF,3, Gen, (Gen)1, (Gen)2, (Gen)3, XD,1, XD,2, XD,3,
B, XB,1, XB,2, XB,3, Con, (Con)1, (Con)2, (Con)3 [ Total = 16 ]

F = 2923.74 kg/hr

XF,1 = 0.5

XF,2 = 0.5

XF,3 = 0

Gen=(Gen)1+(Gen)2+(Gen)3

(Gen)1 =(Gen)2= 0

XD,1 = 0.112

XD,2 = 0.004

XD,3 = 0.3018

B =8046 kg/hr

XB,1 = 0.0107

XB,2 = 0.0388

XB,3 = 0.9504

26
Con=(Con)1+(Con)2+(Con)3

(Con)3=0

Variables - F, XF,1, XF,2, XF,3, Gen, (Gen)1, (Gen)2, (Gen)3, D, XD,1, XD,2, XD,3, B,
XB,1, XB,2, XB,3, Con, (Con)1, (Con)2, (Con)3, (Total = 20)

DOF = Unknown variables – Equations – Known variables = 20-20 = 0


Table. 10 – Mass Balance Spreadsheet for Reactive Distillation (RD)

STREAMS MASS IN MASS OUT

AA n-Butanol H2O(TOP) NBA (Bottom)

kg/hr kmol/ kg/hr kmol/ kg/hr kmol/ kg/hr kmol/


hr hr hr hr

Acetic acid 17.09 0.2846 - - 17.09 0.2846 - -

Acrylic 6124 84.991 - - 498.3 6.9156 0.0073 0.0001


acid

n-Butanol - - 6299 84.991 432.7 5.8377 79.900 1.07794

n-Butyl - - - - 1526 11.912 8480.2 66.1634

Acrylate

Water - - - - 1406 78.07 - -

Total 12441.66 3881.53+8560.13 = 12441.66


kg/hr

27
28
SYNTHESIS
LEGENDS:
D1 - Distillation Column
H1 - Preheater
R1 - Reactor 1
RD - Reactive Distillation
R2 - Reactor 2
C2 - Coolers
HX - Shell And Tube Heat Exchanger

Fig. 10 - OVERALL MASS BALANCE FOR N-BUTYL ACRYLATE


HFIN/HFOUT – Hot Fluid In/Out (Water)
CFIN/CFOUT - Cold Water In/Out (Water)
CHAPTER 4
ENERGY BALANCE

29
Table. 11- Standard Heats of Formation of compounds involved

COMPOUND ∆ (H)formation (KJ/Kmol)


Propene 20600

Oxygen 0

Acrolein -120000

Water -285830

Acrylic acid -324700

Carbondioxide -393520

Acetic acid -435400

n-Butanol -275600

n-Butyl Acrylate -428400

4.1 PREHEATER :
Feed is entering at 38.492℃ and preheated to 270℃. The reference temperature is
25℃.

Enthalpy in

=(114.37*74.992*13.4922)+(230*29.600*13.4922)+(700*29.600*13.4922)+(124.
66*39.234*13.4922) = 550286.328 kJ/hr

Enthalpy out

=(114.37*100.45*245)+(230*31.577*245)+(700*29.83*245)+(124.66*36.125*24
5) =10814077.2 kJ/hr

Heat supplied ∆𝐻𝐻 =Enthalpy out – Enthalpy in = 10263790.88 kJ/hr

Assume steam is entering at 300℃ and leaves at 80℃

Mass of steam required will be,


30
10263790.88 = (m*Cp*∆𝑇𝑇) + 𝑚𝑚𝑚𝑚, 𝜆𝜆 = 2676 𝑘𝑘𝑘𝑘/𝑘𝑘𝑘𝑘

m = 3323.868 kmol/hr
Fig. 11 – Energy Balance block Diagram for Preheater

Table. 12 – Energy Balance block Spreadsheet for Preheater

INPUT OUTPUT
S. No
Components Enthalpy(kJ/hr) Components Enthalpy (kJ/hr)

1 Propene 115721.3438 Propene 2814879.755

2 O2 91857.88385 O2 1779414.896
3 N2 276717.0669 N2 5116440.43

4 Steam as feed 65990.03377 Steam as feed 1103342.131

5 Preheater steam 10263790.88 Preheater steam -

Total 10814077.2 Total 10814077.2

31
4.2 REACTOR 1:
Feed Temperature = 270 ºC
Reference Temperature = 25 ºC
Reactions : 1 - 𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂 + 𝐻𝐻2 𝑂𝑂
3
2 - 𝐶𝐶3 𝐻𝐻6 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂2 + 𝐻𝐻2 𝑂𝑂
2

Enthalpy in (Q in )

=(114.37*100.45*245)+(230*31.577*245)+(700*29.83*245)+(124.66*36.125*24
5) =10814077.2 kJ/hr

Enthalpy out (Q out)

=(56.1576*31.577*245)+(700*29.83*245)+(124.66*36.125*245)+(42.3169*46.00
94*245)+(11.437*100.46*245)+(80.059*118.4232*245)+(12.5807*118.423*245+
(134.956*36.125*245)= 11083677.78 kJ/hr

Heat of reaction-1 = ΔHr = (ΔHf, products) - (ΔHf, reactants) × ξ

=(-12*10^4-(-285830))-(20600) × 80.059

ΔHr = -34139559 KJ/hr

Heat of reaction-2 = ΔHr = (ΔHf, products) - (ΔHf, reactants) × ξ

=(-324700-(-285830))-(20600) × 12.5807

ΔHr = -7940057.19 KJ/hr

Total ΔHr = -42079616 KJ/hr

Heat removed = Q out – Q in + ΔHr = -41810016 KJ/hr

Thus reaction is EXOTHERMIC

Mass of water required:

Q = m cp ΔT

-41810016= m × 74.539× (25-90)


32
Mass of cooling water required = 8629.45 kmol/hr
Fig. 12 – Energy Balance Block Diagram for Reactor 1 (R1)

Table. 13 - Energy Balance Spreadsheet for Reactor-1 (R1)

INPUT OUTPUT
S. No
Components Enthalpy (kJ/hr) Components Enthalpy (kJ/hr)
1 Propene 2814879.755 Propene -
2 O2 1779414.896 O2 434468.1302
3 N2 5116440.43 N2 5116440.43
4 Steam 1103342.131 Steam 1103342.131
5 CO2 CO2 477009.2229
6 CH3COOH CH3COOH 281521.4093

7 Acrolein Acrolein 2111408.492

8 Acrylic acid Acrylic acid 365012.5663


9 Water-By pdt Water-by pdt 1194475.394
10 Cooling water 41810016 Heat of reaction 42079616
Total 52624093.21 Total 52624093.21

33
4.3 REACTOR 2:
Fig. 13 – Energy Balance Block diagram for Reactor 2 (R2)

1
Reaction : 𝐶𝐶3 𝐻𝐻4 𝑂𝑂 + 𝑂𝑂2 → 𝐶𝐶3 𝐻𝐻4 𝑂𝑂2
2

Feed Temperature = 270 ºC


Reference Temperature = 25 ºC
Operating temperature = 300 ºC
Enthalpy in(Q in)

=(56.1576*31.577*245)+(700*29.83*245)+(124.66*36.125*245)+(42.3169*46.00
94*245)+(11.437*100.46*245)+(80.059*118.4232*245)+(12.5807*118.423*245)
+(134.956*36.125*245)

= 11083677.78 kJ/hr

Enthalpy out(Q out)

=(56.1576*31.87*275)+(700*29.99*275)+(124.66*36.405*275)+(43.918*46.709*
275)+(13.038*103.97*275)+(91.0385*121.82*275)+(134.956*36.405*275)

34
= 12851399 kJ/hr

Heat of reaction-1 = ΔHr = (ΔHf, products) - (ΔHf, reactants) × ξ

=(-324700-(-120000)) × 91.0385

ΔHr = -18635585 KJ/hr

Heat removed = Q out – Q in + ΔHr = -16867864 KJ/hr ( Exothermic reaction )

Mass of water required:

Q = m cp ΔT

-16867864= m × 74.539× (25-100)

Mass of cooling water required = 9051.8326 kmol/hr


Table. 14 – Energy Balance Spreadsheet for Reactor 2 (R2)
S. No INPUT OUTPUT
Components Enthalpy in Components Enthalpy in
kJ/hr kJ/hr
1 O2 434468.1302 O2 492258.3905
2 N2 5116440.43 N2 5773119.988
3 Steam 1103342.131 Steam 1248022.024
4 CO2 477009.2229 CO2 564136.6953
5 CH3COOH 281521.4093 CH3COOH 372787.6205

6 Acrolein 2111408.492 Acrolein -

7 Acrylic acid 365012.5663 Acrylic acid 3049968.77


8 Water-By pdt 1194475.394 Water-by pdt 1351105
9 Cooling water 16867864 Heat of 18635585
reaction
Total 26848199.65 Total 26848199.65
4.4 HEAT EXCHANGER (HX) :

Enthalpy in = Enthalpy out of reactor 2 = 12851399 kJ/hr

35
Process stream ΔT =300-70 =230 ºC

Cold stream ΔT = 60-25 = 35 ºC

Mass of coolant required = Q/Cp* ΔT = 12851399/74.539*35 = 4926.04 kmol/hr


Fig. 14 – Energy Balance Block Diagram for Heat Exchanger (HX)

4.5 ABSORBER (ABS) :

Mass of solvent(water)=140.991 kmol/hr

Cp=74.00771 kJ/kmol-K

ΔT =(310-298) =12 K

Heat in through the solvent = Q=125321.113 kJ/hr

Total enthalpy in = 2102956.2+125321.113 = 2228277.308 kJ/hr

36
Fig. 15 – Energy Balance Block Diagram for Absorber (ABS)

Table. 15.a – Energy Balance Spreadsheet for Absorber (ABS)

Enthalpy in through process stream

STREAMS m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
O2 56.1576 31.87512485 45 80551.373
N2 700 29.99023371 45 944692.362
STEAM 124.66 36.40511716 45 204221.786
CO2 43.91808 46.7098326 45 92313.2774
CH3COOH 13.03818 103.9709029 45 61001.6106
ACRYL-01 91.03852 121.8253058 45 499085.799
WATER 134.9566 36.40511716 45 221089.988
TOTAL 2102956.2 kJ/hr

Enthalpy out with Absorber Bottom

STREAMS m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
O2 0.043466726 29.46248 21.9341 28.08964
N2 0.786472801 29.13978 21.9341 502.6779

37
STEAM 124.66 75.51897 21.9341 206491.9
CO2 0.385862406 38.33703 21.9341 324.4672
CH3COOH 12.7940531 79.22206 21.9341 22231.77
ACRYL-01 91.03363778 77.70418 21.9341 155155.1
WATER 196.6799058 75.51897 21.9341 325788.6
TOTAL 710522.6 kJ/hr
Table. 15.b – Energy Balance Spreadsheet for Absorber (ABS)
Enthalpy out with Vent
STREAMS m Cp ΔT Q =m*Cp*ΔT
kmol/hr kJ/kmol-K K kJ/hr
O2 14.48345327 29.49502 19.9346 8515.856
N2 699.2135272 29.17766 19.9346 406694
STEAM 0.000336004 34.0437 19.9346 0.228029
CO2 43.53221759 38.40594 19.9346 33328.57
CH3COOH 0.2441269 68.15279 19.9346 331.6705
ACRYL-01 0.004882221 82.75495 19.9346 8.054136
WATER 79.26811922 34.0437 19.9346 53795.12
TOTAL 502673.5 kJ/hr
Table. 15.c – Energy Balance Spreadsheet for Absorber (ABS)

Total enthalpy out =502673.5+710522.6 = 1213196.104 kJ/hr

Enthalpy in = Q absorbed + Enthalpy out

Therefore, Qabsorbed = 2228277.308-1213196.104 = 1015081.205 kJ/hr

4.6 DISTILLATION COLUMN (D1) :

Temperature of feed = 46.934 ºC

Temperature of distillate = 56.658 ºC

Temperature of residue = 88.0825 ºC

Reboiler Load + Feed Heat = Distillate Heat + Residue Heat + Condenser duty
FEED ENTHALPY
m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
O2 0.04346673 29.4624835 21.934 28.0895072

38
N2 0.7864728 29.13978055 21.934 502.675622
CO2 0.38586241 38.33703447 21.934 324.465722
CH3COOH 12.7940531 79.2220574 21.934 22231.6709
ACRYL-01 91.0336378 77.70418026 21.934 155154.409
WATER 196.679906 75.51897255 21.934 325787.115
STEAM 124.659664 75.51897255 21.934 206490.399
TOTAL 710522.6 kJ/hr
Table 16.a – Energy Balance Spreadsheet for Distillation Column (D1)

DISTILLATE ENTHALPY
m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
O2 0.043466726 2.16947459 34.658 3.268247914
N2 0.786472801 29.1067554 34.658 793.3795493
CO2 0.385862406 81.5474039 34.658 1090.551314
CH3COOH 12.5093958 69.2805684 34.658 30036.63474
ACRYL-01 6.042292931 65.6884176 34.658 13756.06039
WATER 196.679664 72.7627329 34.658 495988.8999
STEAM 124.6595107 72.7627329 34.658 314367.6999
TOTAL 856036.494 kJ/hr
Table 16.b – Energy Balance Spreadsheet for Distillation Column (D1)

BOTTOM DISTILLATE
m cp delT Q
kmol/hr kJ/kmol-K K kJ/hr
CH3COOH 0.284657 78.93403 63.0825 1417.410071
ACRYL-01 84.99134 82.60041 63.0825 442859.3491
TOTAL 444276.7591 kJ/hr
Table 16.c – Energy Balance Spreadsheet for Distillation Column (D1)

Condenser duty

Reflux Ratio = 0.956

D = 341.10 kmol/hr

39
L = R x D = 326.09 kmol/hr

V = D + L = 667.19 kmol/hr

Condenser Duty = V x λ

= 667.19 x 41352.4

= 27589893.5 kJ/hr

Cooling water requirement:

Cooling Water Inlet Temperature = 298 K = 25 C

Cooling Water Outlet Temperature = 368 K = 95C

Cooling water required = Heat removed / (Cp(water) x ΔT)

= 27589893.5 / (74.539 x 70)

= 5287.71 kmol/hr

Reboiler duty

Reboiler Load = Distillate Heat + Residue Heat + Condenser duty – Feed Heat

Reboiler load = 28179687.91 kJ/hr

Cooling Water Inlet Temperature = 450 C

Cooling Water Outlet Temperature = 150 C

Amount of steam required = = 28179687.91 / (1.8123 x 300)+2676 = 8752.29


kmol/hr

40
Fig. 16 – Energy Balance Block Diagram for Distillation Column (D1)

4.7 COOLER (C1) :


Fig. 17 – Energy Balance Block Diagram for Cooler (C1)

Enthalpy in = Enthalpy out of distillation = 444276.7591 kJ/hr

Process stream ΔT =88.0825-25 =63.0825 ºC

Cold stream ΔT = 60-25 = 35 ºC


41
Mass of coolant required = Q/Cp* ΔT = 444276.7591/74.539*35 = 170.29 kmol/hr

4.8 REACTIVE DISTILLATION (RD) :

Temperature of feed = 25ºC

Reference temperature = 25ºC. Therefore, Enthalpy in =0

Temperature of distillate = 45.20 ºC

Temperature of residue = 83.27ºC

Reboiler Load = Distillate Heat + Residue Heat + Condenser duty-Heat of reaction


Reaction : 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 + 𝑛𝑛 − 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 − −→ 𝑛𝑛 − 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 + 𝐻𝐻2𝑂𝑂

Heat of reaction = ΔHr = (ΔHf, products) - (ΔHf, reactants) × ξ

=(-428400-285830)-(-324700-275600) × 66.163

ΔHr = 7537991.2 kJ/hr


Table. 17.a – Energy Balance Spreadsheet for Reactive Distillation (RD)

DISTILLATE ENTHALPY
m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
CH3COOH 0.284625567 79.3133099 20.203 456.0745592
ACRYL-01 6.915649484 77.5783485 20.203 10839.00377
N-BUTANOL 5.837764313 220.237652 20.203 25974.90625
N-BUTYL ACRYLATE 11.91223574 273.109636 20.203 65727.35656
WATER 78.07583487 75.3954623 20.203 118926.2458
TOTAL 221923.5869 kJ/hr

42
Table. 17.b – Energy Balance Spreadsheet for Reactive Distillation (RD)

BOTTOM ENTHALPY
m Cp ΔT Q=m*Cp* ΔT
kmol/hr kJ/kmol-K K kJ/hr
ACRYL-01 0.00010233 81.8599807 58.275 0.488156395
N-BUTANOL 1.077942652 238.541842 58.275 14984.61154
N-BUTYL ACRYLATE 66.16335729 289.824057 58.275 1117473.49
TOTAL 1132458.59 kJ/hr
Condenser duty :

Reflux Ratio = 1.73

D = 103.026 kmol/hr

L = R x D = 175.144 kmol/hr

V = D + L = 278.17 kmol/hr

Condenser Duty = V x λ

= 278.17 x 40151.7

= 11169017 kJ/hr

Cooling water requirement:

Cooling Water Inlet Temperature = 298 K = 25 C

Cooling Water Outlet Temperature = 368 K = 95C

Cooling water required = Heat removed / (Cp(water) x ΔT)

= 11169017/ (74.539 x 70)

= 2140.7 Kmol/hr

Reboiler duty :

Reboiler Load = Distillate Heat + Residue Heat + Condenser duty - Heat of


reaction

43
Reboiler load = 20061390 kJ/hr

Amount of steam required = 20061390 / (1.8123 x200)+2676 =6602.4 kmol/hr

Fig. 18 – Energy Balance Block Diagram for Reactive Distillation (RD)

44
45
LEGENDS:
D1 - Distillation Column
H1 - Preheater
R1 - Reactor 1
RD - Reactive Distillation
R2 - Reactor 2
C2 - Coolers
HX - Shell And Tube Heat Exchanger

HFIN/HFOUT – Hot Fluid In/Out (Water)


CFIN/CFOUT - Cold Water In/Out (Water)

Fig. 19 – Overall Energy Balance for n-Butyl Acrylate synthesis


CHAPTER 5
EQUIPMENT DESIGN

46
5.1 DISTILLATION COLUMN
5.1.1 Process Design:
Feed flow rate = 426.38 kmol/hr

Distillate rate = 341.10 kmol/hr

Bottom rate = 85.275 kmol/hr


Mole fraction of Acetic acid (Liquid) (X) Mole fraction of Acetic acid (Vapour) (Y)

0 0
0.1 0.200997
0.2 0.358702
0.3 0.485248
0.4 0.589133
0.5 0.676476
0.6 0.751853
0.7 0.818865
0.8 0.880575
0.9 0.939889
1 1
Table. 18 – Vapor Liquid Equilibrium data for the system

Plotting XY graph using ‘Mc-Cabbe Thiele’ method

From graph given below, Number of theoretical stages = 13

Assuming efficiency as 60%

Number of Actual stages = (13-1)/0.6 =20 stages

Slope of enriching section = 0.956

V= 667.19 kmol/hr, L= 326.09 kmol/hr

Slope of stripping section = 5.01

V’= 341.1kmol/hr, L’= 426.375 kmol/hr

47
MOLE FRACTION VAPOUR, Y

MOLE FRACTION OF LIQUID, X

Fig. 20 – McCabe Thiele plot for the system

Surface tension :
Using Sugden (1924), equation 8.23 (Coulson and Richardson’s, volume 6, page
335)

σ = (𝑃𝑃𝑃𝑃h(𝜌𝜌𝜌𝜌− 𝜌𝜌𝜌𝜌)) 4

where σ = surface tension, N/m

Pch = Sugden’s parachor

ρv = Vapor density, kmol/m3

ρL = Liquid density, kmol/m3

Pch(bottom) =158.9 (from perry)

Pch(top) = 129.82(from perry)


Table. 19 – Estimated Surface Tension values

48
Table. 19 – Estimated Surface Tension values

Bottom VALUES UNIT


T 141 deg. Cel.
ρV (from perry) 2.77 Kg/m3
ρL (from perry) 973.55 Kg/m3
σ 0.028 N/m

Top
T 118 deg. Cel.
ρV (from perry) 1.89 Kg/m3
ρL (from perry) 1071.81 Kg/m3
σ 0.026 N/m
Enriching Section :
FLV =𝐿𝐿/𝑉𝑉�(ρV/ρL) = 0.956*�(1.89/1071.81)= 0.0401
To find flooding velocity,
K1= 0.09, Corrected K1= K1(σ/0.02)0.2 = 0.09(0.026/0.02)0.2 = 0.0948
Flooding velocity, Uf = K1�(ρl − ρv/ρv) = 2.256 m/s
Design for 85% of Uf, Uv = 0.85*2.256 = 1.918 m/s
Maximum Vapour Flow rate, V= (V*MW/3600* ρv) =2.0160 m3/s
Net area required A= V/ Uv = 2.0160/1.918 = 1.0509 m2
Downcomer = 12% of total area
Therefore, Actual area = 1.0509/0.88 = 1.194 m2
Column diameter = DC = �1.194 ∗ 4/π = 1.233 m
Stripping Section :
FLV =𝐿𝐿/𝑉𝑉�(ρV/ρL) = 5.01*�(2.77/973.55)= 0.266
To find flooding velocity,
K1= 0.087, Corrected K1= K1(σ/0.02)0.2 = 0.087(0.028/0.02)0.2 = 0.0930
Flooding velocity, Uf = K1�(ρl − ρv/ρv) = 1.7420 m/s

49
Design for 85% of Uf, Uv = 0.85*1.7420 = 1.480 m/s
Maximum Vapour Flow rate, V= (V*MW/3600* ρv) =2.4648 m3/s
Net area required A= V/ Uv = 2.4648/1.480 = 1.6645 m2
Downcomer = 12% of total area
Therefore, Actual area = 1.6645/0.88 = 1.891 m2
Column diameter = DC = �1.891 ∗ 4/π = 1.230 m
Largest Diamter is taken as the column diamter. DC = 1.233 m
From standard BS 1600 DO = 1241 mm, Di = 1233 mm, Thickness = 8mm.
Tray Design :
π
Column area, AC = * Di2 = 1.193 m2
4

Downcomer area AD = 0.12*1.193 = 0.1432 m2


Net area, AN = AC – AD = 1.0502 m2
Active area, Aa = AC –2*AD = 0.9070 m2
Hole area, Ah = 0.1* Aa = 0.0907 m2
Referring to Figure 11.31 from Coulson and Richardson’s, Chemical Engineering,
Volume 6, page 572, with (Ad/Ac) x 100 is 12 percent, thus, Iw/Dc is 0.50
Length of the weir, lw = 0.61 m
Assumptions:
Height of the weir, hw = 50mm
Hole diameter = 5mm
Plate thickness = 5 mm
Plate spacing = 0.5 m
Weeping verification :
Mass flowrate of liquid MMAX= 6.527 kg/s
Minimum Flow rate of liquid at 70% turndown MMIN = 0.7*6.527= 4.5689 kg/s
Height of crest over weir:

50
Maximum how = 750*( MMAX/lW* ρL) = 34.77 mm
Minimum how = 750*( MMIN/lW* ρL) = 27.413 mm
At minimum rate, how+ hw = 77.413mm
From Figure 11.30, in Coulson and Richardson’s, Chemical Engineering, Volume
6, page 571, weep point correlation K2= 30.5
Minimum design vapour velocity = K2 -0.9(25.4-hole dia)/(ρv)0.5 = 4.593 m/s
Actual minimum vapour velocity = 0.7*V/Ah = 19.02 m/s
Since Actual minimum vapour velocity > Minimum design Vapour velocity
WEEPING DOES NOT OCCUR.
Plate Pressure Drop:
Maximum vapour velocity through holes = V(TOP)/Hole area = 22.22 m/s
Assume plate thickness = hole diameter
From Figure 11.34 in Coulson and Richardson’s, Chemical Engineering, Volume
6, page 576, for discharge coefficient for sieve plate, = CO = 0.84
Dry plate drop, hd = 51(22.22/0.74)2 * (1.89/1071.81) = 62.967 mm liquid
Residual Head hr = (12.3*103/1071.81) = 11.662 mm liquid
Total head ht = how+ hw+ hd + hr = 152.044 mm liquid
100 mm was assumed, calculated value is within limit hence acceptable.
Downcomer:
Height of the apron = 40 mm
Area under apron = 0.61*40*10-3 = 0.0244 m2
Head loss in downcomer hdc = 166*(6.527/0.0244*1071.81)2 = 10.338 mm
Backup in downcomer hh = ht + how+ hw+hdc = 0.239 m
Since hh < 0.5 m, plate spacing is accpetable.

51
5.1.2 Mechanical Design :
Several factors need to be considered in the mechanical design of distillation
column such as
1. Design pressure
2. Design temperature
3. Material of construction
4. Design stress
5. Wall thickness
6. Welded joint efficiency
7. Analysis of stresses
a. Dead weight load
b. Wind load
c. Pressure stress
d. Bending stress
8. Vessel support
9. Insulation
Column Design Specification:
Design pressure = 0.15 N/mm2
Design temperature = 88.082°C
Take as 10% above operating temperature
Operating temperature = 88.082 x 1.1= 96.89°C
Material of Constructions
Selection of suitable material must be taking onto account the suitability of
material for fabrication (particularly welding) as well as the compatibility of the
material with the process environment. In this case, the material used in the
construction of the distillation column is carbon steel as the material as it is the

52
most used material in industry. For this material, the design stress at 150°C is
obtained from Table 13.2 for the typical design stresses for plate.
Design stress, f = 95 N/mm2
Join factor = 1
Diameter vessel, D = 1233 mm
Operating pressure = 0.15 N/mm2
Insulation,
mineral wool = 75 mm thick
Vessel Thickness :
T = pDi/(2fJ-P) = (0.15*1233)/(2*95*1-0.15) = 4.146 mm
For sake of rigidity Take vessel thickness = 8mm
Head And Closure :
Hemispherical, ellipsoidal and torispherical heads are collectively referred to
as domed heads. They are formed by pressing or spinning, large diameters are
fabricated from formed sections. Torispherical are often referred to as dished ends.
After comparing the thickness of all heads, torispherical head had been chosen
because of operating pressure for this below 10 bars and suitable for liquid vapor
phase process in inconsistent high pressure. The thickness of torispherical head can
be calculated below
th = (P*Rc*Cs)/(2Jf+p(Cs-0.2))
Cs = 0.25(3+sqrt(Rc/Rk)
Rc=crown radius = Dc = 1233mm, Rk =knuckkle radius =0.06*Rc=73.98 mm
Cs= 1.7706
th= 5.0247 mm
Take head thickness same as that of vessel thickness, th= 8mm
Weight Loads :

53
The major sources of the dead weight loads are:
1. The vessel shell
2. The vessel fittings: manhole, nozzles
3. Internal fitting: plates, heating cooling coils
4. External fittings: ladders, platforms, piping
5. Auxiliary equipment which is not self supported, condensers
6. Insulation
Dead Weight Of Vessel :
Dead weight of vessel can be calculated by using equation below:
Wv = 240 x Cv x Dm x (Hv + 0.8 Dm)t x 10-3 kN
where, Wv= total weight of shell, excluding internal fitting such as plates
Cv= a factor to account for the weight of nozzles, man ways and internal
supports. (In this distillation column, take Cv as 1.15)
Dm= mean diameter of vessel = (Dc + t) m= (1.233 + 0.008)= 1.241 m
Hv= height or length between tangent lines = 11m
t= wall thickness, m
Wv = 240 x 1.15 x 1.241(11.0 + 0.8(1.241)) x 0.008= 32.86 kN
Weight of plates :
From Nelson Guide, page 833 Chemical Engineering Volume 6; take
contacting plates, 1.2 kN/m2 (for typical liquid loading). The total of weight of
plate determine by multiply the value with number of plate design.
π
Plate area = = * Di2 = 1.1941 m2
4

Weight of plate = Typical standard loading*plate area = 0.12*1.1941= 1.4330 kN


For 20 stages, Wp = 20*1.4330 = 28.6604 kN
Weight of Insulation :

54
The mineral wool was chosen as insulation material. By referring to
Coulson & Richardson, Chemical Engineering Design, Volume 6, page 833,
Density of mineral wool, ρ = 130 kg/m3
Thickness = 75 mm = 0.075 m
Volume of insulation, Vi= π x Di x Hv x thickness of insulation
= (3.142)(1.233)(11)(0.075) = 3.1961 m3
Weight of insulation, Wi = Volume of insulation x ρ x g
= 3.1961 x 130 x 9.81= 4076.01 N
= 4.076 kN
Weight of fittings= 2*weight of insulation = 2*4.076 = 8.1520 kN
Total Weight :
The total weight is the summation of dead weight of vessel, weight of
accessories and weight of insulation:
Total weight = Wv + W ρ + Wi = 32.86 + 28.660 + 8.152 = 69.6743 kN
Wind Load :
A wind loading must be designed to withstand the highest wind speed that is
likely to encounter at the site during the life of the plant. From the British Standard
Code of Practice BS CP 3: 1972 “Basic Data for the Design of Buildings, Chapter
V Loading: Part 2 Winds Load”, (Sinnott, 1999), a wind speed of 160 km/h (100
mph) can be used for preliminary design. For cylindrical column, semi-empirical
equation can be used to estimate the wind pressure:
Pw = 0.05 x u2
where, Pw= wind pressure, N/m2
u= wind speed, km/h
Pw = 0.05 (160)2 = 1280 N/m2
Mean diameter, including insulation = Di + 2(t + tins)

55
= 1230 + 2(8 + 75)
= 1399 mm
= 1.399 m
Loading (per linear meter), Fw = Pw*Deff = 1280 x 1.5 = 1920 N/m
𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚, 𝑀𝑀𝑀𝑀 =𝐹𝐹𝐹𝐹 𝐻𝐻𝐻𝐻2/2 =1920 × 112/2 = 116160 Nm = 116.16 kN m
Analysing Stresses on Vessel:
 Pressure Stresses:
1. Longitudinal Stress is given by,
𝜎𝜎𝐿𝐿 = 𝑃𝑃𝑃𝑃 ∗ 𝐷𝐷𝐷𝐷/4 ∗ 𝑡𝑡 = 0.15*1233/4*8 = 5.7796 N/mm2
2. Circumferential Stress is given by,
𝜎𝜎ℎ = 𝑃𝑃𝑃𝑃 ∗ 𝐷𝐷𝐷𝐷/2 ∗ 𝑡𝑡 = 0.15*1233/2*8 = 11.5593 N/mm2
 Dead Weight Stress:
Dead weight stresses are significant for tall columns. This stress can
be tensile for points below the column support or compressive for points
above the support. Dead weight stresses are given by:
𝜎𝜎𝑤𝑤 = 𝑊𝑊/(3.14(𝐷𝐷𝐷𝐷 + 𝑡𝑡)𝑡𝑡= 69.6743/3.14(1233+8) *8 = 2.2335 N/mm2
 Bending Stress:
The bending stress will be compressive or tensile, depending on
location and are given by:
𝑀𝑀𝑀𝑀 𝐷𝐷𝐷𝐷
𝜎𝜎𝑏𝑏 = ± � � � + 𝑡𝑡� 𝑤𝑤ℎ𝑒𝑒𝑒𝑒𝑒𝑒, 𝑀𝑀𝑀𝑀 − 𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇 𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚
𝐼𝐼𝐼𝐼 2
𝜋𝜋
𝐼𝐼𝑣𝑣 = � � (𝐷𝐷𝑂𝑂4 − 𝐷𝐷𝑖𝑖4 )
64
𝜋𝜋
𝐼𝐼𝐼𝐼 = 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 = � � (12414 − 12334 )
64
= 2971756987 mm4
𝜎𝜎𝑏𝑏 = ± 0.02441 𝑁𝑁/𝑚𝑚𝑚𝑚2

56
Resultant Longitudinal Stress:
The resultant of longitudinal stress is the summation of longitudinal stresses, dead
weight stresses and bending stress.
𝜎𝜎𝜎𝜎 = 𝜎𝜎𝜎𝜎 + 𝜎𝜎𝜎𝜎 ± 𝜎𝜎𝜎𝜎
For upwind,
𝜎𝜎𝜎𝜎 = 5.7796+ (−2.2335) + 0.02441 = 3.5705 N/mm2
For downwind,
𝜎𝜎𝜎𝜎 = 5.7796+ (−2.2335) – 0.02441 = 3.5216 N/mm2
Therefore, the greatest difference between the principle stresses,
𝜎𝜎𝜎𝜎 = 𝜎𝜎h − 𝜎𝜎𝜎𝜎 (up𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤) = 11.5593 – 3.5216 = 7.988 N/mm2
The value obtained is well below the maximum allowable design stress which is 95
N/mm2
Vessel Support Design:
The method used to support a vessel will depend on the size, shape, and
weight of the vessel; the design temperature and pressure, the vessel location and
arrangement; and the internal and external fittings and attachment. Since the
distillation column is a vertical vessel, skirt support is used in this design.
A skirt support consists of a cylindrical or conical shell welded to the base of
the vessel. A flange at the bottom of the skirt transmits the load to the foundations.
The skirt may be welded to the bottom, level of the vessel. Skirt supports are
recommended for vertical vessels as they do not impose concentrated loads on the
vessel shells; they are particularly suitable for use with tall columns subject to
wind loading.

57
Type of support = Straight cylindrical skirt
𝜃𝜃 = 90°
Material of construction = Carbon Steel
Design stress, f = 95 N/mm2
Young’s modulus = 200,000 N/mm2
Skirt height, hs =4m
Skirt thickness, ts = 8 mm
Joint factor = 0.85
Weight of the Skirt:
Approximate weight, Wapprox = (π/4 x Di2 x Hv) x ρL x 9.81
= (π/4 x 1.2332 x 11) x 973.55 x 9.81 = 45620.45 N = 45.620 kN
Weight of vessel, W = 69.6743 kN
Total weight = 45.620 kN + 69.6743 kN = 115.294 kN

Analysis of Stresses of Skirt:


 Bending moment of base skirt (Ms)
Ms = 0.5 x Fw(Hv + Hs)2 = 0.5 x 1.92(11 + 4)2 = 216 kNm
 Bending stress of skirt (σbs)
𝜎𝜎𝜎𝜎𝜎𝜎 = 4 𝑀𝑀𝑀𝑀 / 𝜋𝜋 (𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡) × 𝐷𝐷𝐷𝐷 x 𝑡𝑡𝑡𝑡
= 4 × 116.16 × 103 × 103/ 𝜋𝜋 (1233 + 8) × 1233 × 8 = 22.4737 N/mm2
 Dead weight stress in skirt (σws)
𝜎𝜎𝜎𝜎𝜎𝜎 (𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡) = 𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊 /𝜋𝜋 𝑡𝑡𝑡𝑡(𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡)
=45620.45/𝜋𝜋 × 8(1233 + 8) = 1.4634 N/mm2
𝜎𝜎𝜎𝜎𝜎𝜎 (𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜) = 𝑊𝑊/𝜋𝜋𝜋𝜋𝜋𝜋(𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡)
= 69674.32/𝜋𝜋 × 8(1233 + 8) = 2.2335 N/mm2
 Resultant Stress In Skirt (σs)

58
Maximum σs (tensile) = σbs + σws test = 22.4737 + 1.4634 = 23.9271
N/mm2
Maximum σs (compressive) = σbs - σws operating = 22.4737 – 2.2335
= 20.2301 N/mm2
 Criteria for Design
Take the joint factor, J as 0.85 Where θs = 90°
σs (tensile) < fs J sin θs
23.9271 N/mm2 < 95 x 0.85 sin 90°
23.9271 N/mm2 < 80.75 N/mm2
σs (compressive) < 0.125 E(ts/Ds) sin θs
20.2301 N/mm2 < 0.125 x 200000(9/1233) sin 90°
20.2301 N/mm2 < 169.17 N/mm2.
Both the criteria are satisfied.
Flange Design :
Flange material : IS 2004-1962 Class 2 Carbon Steel
Bolting steel : 5% Chromium, Molybdenum Steel
Gasket Material : Asbestos
Shell OD = 1.241 m
Shell Thickness = 0.008 m (g)
Shell ID = 1.233 m
Allowable stress for flange material = 100 N/mm2
Allowable stress of bolting material = 138 N/mm2
Determination Of Gasket Width :
Minimum design yield seating stress, Ya = 52.386 N/mm2
Gasket factor, m = 3.75
Gasket Size:

59
Outer Diameter = 1286 mm
Inner Diameter = 1256 mm
Mean Gasket Diameter, G = 1271 mm
Minimum gasket width, N = 30 mm.
Basic gasket seating width, bo = 30/2 = 15 mm
Effective Gasket Seating Width, b = 2.5 x [bo]0.5= 9.7 mm
Estimation Of Bolt Loads:
Under atmospheric conditions, the bolt load due to gasket reaction is given
by
Wm1 = π b G y
= π x 9.7 x 1271 x 52.386
= 2029.26 KN
Load due to design pressure
Wm2 = πG2P/4 + πG(2b)*m*p
= 233.91KN
The controlling load is Wm1 because Wm1 > Wm2
Calculation Of Minimum Bolting Area :
Am = Ao = W / S
S = allowable stress for bolting material
Am1 = Ao= 2029.26 x 103/138 = 14704.78 mm2
Calculation Of Optimum Bolt Size :
Bolts are of 5% Cr Mo Steel
Number of bolts = G / [bo x 2.5]
= 1271 / [15 x 2.5]
= 34 bolts
Diameter of bolts = [(Am1 / Number of bolts) x (4 / π) ]1/2 = 24mm
60
Flange Thickness :
Thickness of flange, tf = [G√(p/K*f)] + C

where, C is the Corrosion allowance


hG is radial distance from gasket load reaction to bolt
circle Hydrostatic end force,
H = (π /4) G2 p
= 190.339KN
K =1/ [0.3 + {(1.5 Wm hG) / (H x G)}]
hG = (B – G)/2
B = Outside diameter of gasket + 2*Diameter of bolt + 12mm
= 1286+(2*24) +12
= 1346 mm
hG = (1346-1271)/2 = 37.5 mm
K = 1.295
tf = [G√(p/K*f)] + C
= 43.24 + 3
tf = 47 mm
Nozzle Design :
Nozzle diameter at head = 200 mm
Nozzle diameter at shell = 300 mm
 Nozzle (in the head)-Top product
tn= pDi / (2fJ – p)= (0.15*200)/(2*95*0.85)-0.15) = 0.1859 mm
For sake of rigidity, nozzle thickness is taken as 3 mm which is standard size.
Maximum nozzle distance = 2*d = 2*200 = 400 mm
Maximum vertical distance for compensation provided outside vessel
= 2.5* th = 2.5*8 =20 mm

61
Area for compensation required A = d*th = 200*2.0247 = 404.94mm2
Area available for compensation is as follows:
• Portion on head having excess thickness
As = d*(ts – ts’ – c) = 200*(8-2.0427) = 1195.2mm2
ts - actual thickness of head
ts’- theoretical thickness of head
• Portion of nozzle external to vessel
Ao = 2*2.5* ts (tn – tn’ – c) = 2*2.5*8(3-0.1859) = 112.56 mm2
• Portion of nozzle inside the head is zero
Therefore, area available for compensation = 1195.2 + 112.56 = 1307.7 mm2
(AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
 Nozzle (in the head)-Bottom product:
tn= pDi / (2fJ – p) = (0.15*200)/ (2*95*0.85)-0.15) = 0.1859 mm.
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*200 = 400 mm
Maximum vertical distance for compensation provided outside vessel = 2.5*ts
= 2.5*4 =20 mm
Area for compensation required A = d*th = 200*2.0247 = 404.94 mm2
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 200*(8-2.0247) = 1195.2 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5*ts (tn – tn’ – c) = 2*2.5*8(3-0.1859) = 112.562 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 1195.2 + 112.56 = 1307.7 mm2
AS+AO)>A, THIS IS SATISFACTORY.

62
Nozzle reinforcement not required.
 Nozzle-Vent:
tn= p*Di / (2fJ – p) = (0.15*100)/(2*95*0.85)-0.15) = 0.0929 mm
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*100 = 200mm
Maximum vertical distance for compensation provided outside vessel = 2.5*th
= 2.5*8= 20 mm
Area for compensation required A = d*th = 100*2.0247 = 202.47 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 100*(8-2.0247) = 597.6 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*8(3-0.0929) = 116.28 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 597.6+116.28 = 713.88 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
Nozzle-Shell-Reflux :
tn= p*Di / (2fJ – p) = (0.15*200)/(2*95*0.85)-0.15) = 0.1859 mm
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*200 = 400mm
Maximum vertical distance for compensation provided outside vessel = 2.5*th
= 2.5*8= 20 mm
Area for compensation required A = d*th = 200*4.146 = 202.47 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 200*(8-4.146) = 770.8 mm2

63
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*8(3-0.1858) = 112.56 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 770.8+112.56 = 883.36 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
 Nozzle-Shell-Feed :
tn= p*Di / (2fJ – p) = (0.15*100)/(2*95*0.85)-0.15) = 0.0929 mm
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*100 = 200mm
Maximum vertical distance for compensation provided outside vessel = 2.5*th
= 2.5*8= 20 mm
Area for compensation required A = d*th = 100*4.146 = 414.6 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 100*(8-4.146) = 385.4mm2
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*8(3-0.0929) = 116.28 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 385.4+116.28 = 501.68 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
 Nozzle-Shell-Reboiler Inlet :
tn= p*Di / (2fJ – p) = (0.15*200)/(2*95*0.85)-0.15) = 0.1859 mm
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*200 = 400mm
Maximum vertical distance for compensation provided outside vessel = 2.5*th

64
= 2.5*8= 20 mm
Area for compensation required A = d*th = 200*4.146 = 829.2 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 200*(8-4.146) = 770.8 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*8(3-0.1859) = 112.562 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 770.8+112.56 = 883.36 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
 Nozzle-Shell-Manhole :
tn= p*Di / (2fJ – p) = (0.15*400)/(2*95*0.85)-0.15) = 0.3718 mm
Considering rigidity, nozzle thickness of standard size is taken as 4 mm.
Maximum nozzle distance = 2*d = 2*400 = 800mm
Maximum vertical distance for compensation provided outside vessel = 2.5*th
= 2.5*8= 20 mm
Area for compensation required A = d*th = 400*4.146 = 1658.4 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 400*(8-4.146) = 1541.6 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*8(4-0.3718) = 145.12 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 1541.6+145.12 = 1686.72 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.

65
Fig. 21 - EQUIPMENT DESIGN FOR DISTILLATION COLUMN (D1)

66
5.2 SHELL AND TUBE HEAT EXCHANGER (HX) :
5.2.1 Process Design :
Table. 20 – Properties of compounds flowing through shell and tube side

SHELL SIDE PARAMETERS TUBE SIDE PARAMETERS

(PROCESS STREAM-HOT FLUID) (COOLING WATER-COLD FLUID)

Inlet 573.15 K Inlet 298.15 K


temperature(T1) temperature(t1)

Outlet 343.15 K Outlet 333.15 K


temperature(T2) temperature(t2)

Mean temperature 458.15 K Mean temperature 315.65 K

Mass flow rate 9.4521 kg/s Mass flow rate 24.63 kg/s

Average Density 2.84357 kg/m3 Density 995.97 Kg/m3

Specific heat 1.3312 kJ/kg K Specific heat 4.2 kJ/kg K


capacity capacity

Thermal 0.04097 W/mK Thermal 0.6063 W/mK


conductivity conductivity

Viscosity 2.659*10-5 Pa s Viscosity 0.0009125 Pa.s

Passes 1 Passes 2

Logarithmic Mean Temperature Difference (ΔTLMTD)


= [(T1 - t2) – (T2 – t1)] / ln [(T1 – t2) / (T2 – t1)]
=103.57°C
R = (T1 – T2) / (t2 – t1)
= 6.8571

67
S = (t2 – t1) / (T1 – t2)
= 0.1272
Correction factor (Ft) = 0.97 (from fig.18 Kern Book)
Corrected ΔTLMTD = ΔTLMTD * Ft
= 100.46°C
Assume U = 600 W/m2°C
Area (A) = Q / U*ΔTLMTD
= 48.01m2
Standard Values :
Tube outer diameter(do) = 20 mm

Tube inner diameter(di) = 16 mm

Tube length(l) = 4.83m

HT Area of one tube = π*do*L

= 0.3035 m2

No. of tubes = A / Area of one tube

= 158

Bundle diameter (Db) = do*(Nt / k1) (1/n1)

For triangular pitch, k1 = 0.175, n1 = 2.285

Db = 532.42 mm

Tube pitch (Pt) = 1.25 * do = 0.025 mm

Clearance (C) = 58 mm (for split ring floating head)

Shell diameter (Ds) = Db + C = 590 mm

68
Tube side heat transfer coefficient :

Cross-sectional area (at) = (π/4)*di 2 = 200.9 mm2

Tubes per pass = Nt / passes = 39 tubes

Total flow area (At) = at * (Nt / passes)

= 0.007935 m2

Mass velocity (Gt) = m / At

= 3103.75 kg/m2s

Reynold’s Number (Re) = Gt*di / μ

= 54421.99

Prandtl’s Number (Pr) = Cp * μ / K

= 5.5418

JH factor = 0.0037 (from fig.24 Kern Book)

hi = K / di * JH * Re * Pr0.33

= 6712.68 W/m2°C

hio = hi * di/ do

= 5370.144 W/m2°C

Shell side heat transfer coefficient :

Baffle spacing (B) = 0.2 * Ds

= 118 mm

Flow area (As) = (Pt-d0) * Ds *B/ Pt)

69
= 0.0139 m2

Mass velocity (Gs) = M / As

= 678.8 kg/m2s

Equivalent diameter (De) = (1.1 / do) *(Pt2–0.917*do2)

= 14.20 mm

Reynold’s Number (Re) = Gs * De / μavg

= 362528.72

Prandtl’s Number (Pr) = Cpmix * μavg / Kavg

= 26.11

JH factor = 0.0028 (from fig.28 Kern Book)

ho = K / di * JH * Re * Pr0.33

Heat transfer coefficient (ho) = 8594.5 W/m2 °C

Overall heat transfer coefficient :

Carbon steel is used, therefore thermal conductivity K = 51 W/m °C

1/U = (1/hs) + (1/hod) + [do/(di*hid)] + (do/di*hi) + (do * ln(do/di) / 2K)

U = 641.2138 W/m2 °C

U(assumed) = 600 W/m2 °C (error is less than 30% and within acceptable limit)

Shell side pressure drop :

Ds = 590 mm

De = 14.2 mm

70
L = 4.83 m

B = 118 mm

jf = 2.8*10-2(from kern book)

Pressure drop (ΔPs) = 8*jf*(Ds/De) *(L/B) *(pu2/2)

= 30.87 kpa

= 4.477 psi

Tube side pressure drop :

jf = 0.0033 (from Kern Book)

L = 4.83 m

Di = 16 mm

u = 3.119 m/s

ΔPt = n*(8*f(L/Di) +2.5) * (pu2)/2

= 3.6259 psi

As this value of Pressure Drop on the shell side is less than the 70 KPa, the
design is acceptable from the Pressure Drop Point of View.
Thus, the design is acceptable from process design consideration.
Summary Of Process Design For Heat Exchanger :
Mass flow rate of acid = 9.4521 Kg/s

Mass flow rate of water = 24.73 Kg/s

Shell outer diameter = 590 mm


Number of tubes = 158

71
Tube OD = 20mm
Pitch (Triangular) = 0.025m
Tube length = 4.83 m
Shell side pressure drop = 30.87
Kpa
Tube side pressure drop = 25 KPa
Heat Exchanger type = TEMA S type 1-4 Heat Exchanger.

5.2.2 Mechanical Design Of Heat Exchanger :


Working pressure = 0.101325 N/mm2
Design pressure = 0.114575 N/mm2
Inlet temperature = 300°C
Shell Diameter = 590 mm
Number of tubes = 158
Material chosen: IS 2825-1969 Grade I plain Carbon Steel
Permissible stress(f) = 95 N/mm2
Joint factor(J) = 0.85
Shell thickness :
ts = PD / (2fJ - P) + C

P = 0.114575 N/mm2

f = 95 N/mm2

D = 590 mm

J = 0.85

ts = 3.418 mm
For the sake of rigidity thickness is taken as 7mm
72
ts = 7 mm
Nozzles :
Take inlet and outlet nozzles as 100mm diameter.
Vent nozzle = 25mm diameter
Drain nozzle = 25mm diameter
Relief Valve = 50 mm diameter.
Nozzle thickness = (P x Di) / (2 f J – P)
tn = (0.114575*100)/ (2*95*0.85-0.114575)
tn = 3.074 mm
For the sake of rigidity thickness is taken as 7mm
Head Thickness :
Torispherical heads are taken for both ends.
Rc (Crown radius) = 590 mm
Rnk (knuckle radius) = 59 mm

Head thickness ( th )
= [ P x Rc x W] / {2 f J}
where ,
W = (1/4) x [ 3 + (Rc / Rnk)0.5]
= 1.7706

Head thickness ( th ) = [ P x Rc x W] / {2 f J}
Head thickness = 3.7411 mm

For sake of rigidity take Head Thickness as that of the Shell Thickness = 7mm

Transverse Baffles :
Baffle thickness = 6mm (standard)
Baffle cut = 25%
Baffle spacing = 118mm

73
Number of baffles = (Length of Hx / Baffle cut)-1 = (4.83/0.1475)-1
= 32 baffles
Tie Rods and Spacers:
Diameter of tie rods = 10mm
Diameter of Spacers = 8mm
Flange Design:
Flange is ring type with plain face.
Flange material: IS 2004-1962 Class 2 Carbon Steel
Bolting steel: 5% Chromium, Molybdenum Steel
Gasket Material: Asbestos
Shell OD = 0.590 m
Shell Thickness =0.008 m (g)
Shell ID = 0.583 m
Allowable stress for flange material = 100 N/mm2
Allowable stress of bolting material = 138 N/mm2
Determination Of Gasket Width:
Minimum design yield seating stress, Ya = 52.386 N/mm2
Gasket factor, m = 3.75
Gasket Size:
Outer Diameter = 635 mm
Inner Diameter = 605 mm
Mean Gasket Diameter, G = 620 mm
Minimum gasket width, N = 30 mm.
Basic gasket seating width, bo = 30/2 = 15 mm
Effective Gasket Seating Width, b = 2.5 x [bo]0.5= 9.7 mm

74
Estimation Of Bolt Loads:
Under atmospheric conditions, the bolt load due to gasket reaction is given
by
Wm1 = π b G y
= 989.88 KN
Load due to design pressure
Wm2 = πG2P/4 + πG(2b)*m*p
= 473.86 KN
Wm1 > Wm2 Hence, the controlling load is Wm1
Calculation Of Minimum Bolting Area:
Am = Ao = W / S
S = allowable stress for bolting material
Am1 = Ao= 989.88 x 103/138 = 7173.08 mm2
Calculation Of Optimum Bolt Size:
Bolts are of 5% Cr Mo Steel
Number of bolts = G / [bo x 2.5]
= 620 / [15 x 2.5]
= 18 bolts
Diameter of bolts = [(Am1 / Number of bolts) x ( 4 / π) ]1/2 = 23mm
Flange Thickness:
Thickness of flange, tf = [G√(p/K*f)] + C

Where, C is the Corrosion allowance


hG is radial distance from gasket load reaction to bolt
circle Hydrostatic end force,
H = (π /4) G2 p
= 33.654 KN
75
K =1/ [0.3 + {(1.5 Wm hG) / (H x G)}]
hG = (B – G)/2
B = Outside diameter of gasket + 2*Diameter of bolt + 12mm
= 635+(2*23) +12
= 693 mm
hG = (693-620)/2 = 36.5 mm
K = 0.3449
tf = [G√(p/K*f)] + C
= 36.16 + 3
tf = 39 mm
Tube Side :
Material used: Stainless steel
Thickness of tube = tf = {P x Do} / (2 f J + P)
Were, Do = 20mm, Di = 16mm
Design pressure, P = 0.111457 N/mm2
Permissible Stress, f= 100.6 N/mm2
Joint Efficiency, J = 1
Thickness of tube= 4mm
Tube Sheet :
Thickness of Tube Sheet, tts = FG√[(0.25 P)/f]
where, F= 1.25
Thickness of tube sheet = 144 mm
Channel And Channel Cover :
Material : Carbon Steel
Permissible stress, f = 95 N/mm2
For Ring type gasket K = 0.3

76
Thickness of channel, th =G √[( (K x P) /f ] = 130.36 mm

Gasket Size :
Gasket material: Steel Jacketed Asbestos
Minimum design yield seating stress, Ya = 126.6 N/mm2
Gasket factor, m = 5.5
Mean Gasket Diameter, G = 620 mm
Minimum gasket width, N = 30 mm.
Basic gasket seating width, bo = 30/4 = 7.5mm
Effective Gasket Seating Width, b = 2.5 x [bo]0.5= 6.846 mm
Estimation Of Bolt Loads :
Under atmospheric conditions, the bolt load due to gasket reaction is given
by
Wm1 = π b G y
= π x 6.846 x 620 x 126.6
= 1688.5 KN
Load due to design pressure
Wm2 = π/4 G2P+ πG(2b)*m*p
= 6281.03KN
The controlling load is Wm2 because Wm2 > Wm1
Calculation Of Minimum Bolting Area :
Am = Ao = W / S
S = allowable stress for bolting material
Am1 = Ao= 6281.03x 103/138 = 44673.07 mm2
Calculation Of Optimum Bolt Size :
Bolts are of 5% Cr Mo Steel
77
Number of bolts = G / [bo x 2.5]
= 620 / [7.5 x 2.5]
= 34 bolts
Diameter of bolts = [(Am1 / Number of bolts ) x ( 4 / π) ]1/2 = 40.9mm
Thickness Of Nozzle :
Considering inlet and outlet diameter to be 100mm, then thickness of the nozzle is
given by,
Thickness of nozzle, tn = (P x Dn) / [2 x f J – P]
Permissible stress, f = 95 N/ mm2
Joint Efficiency, J = 0.85
Then, Thickness of nozzles =10 mm
Flange Thickness :
Thickness of flange, tf = [G√(p/K*f)] + C

where, C is the Corrosion allowance


hG is radial distance from gasket load reaction to bolt
circle Hydrostatic end force,
H = (π /4) G2 p
= 4227.2 KN
K =1/ [0.3 + {(1.5 Wm hG) / (H x G)}]
hG = (B – G)/2
B = Outside diameter of gasket + 2*Diameter of bolt + 12mm
= 635+(2*40.9) +12
= 728.8 mm
hG = (728.8-620)/2 = 54.4 mm
K = 2.0179
tf = [G√(p/K*f)] + C

78
= 36.16 + 3
tf = 166 mm

Hence the thickness of flange = 166 mm

Support For Shell And Tube Heat Exchanger :


Length of the heat exchanger, L = 4830 mm
Inner Diameter of Shell, Di = 583 mm
Outer diameter of Shell, Do = 590 mm
Thickness of Shell, ts = 8 mm
Outer diameter of tube, do = 20mm
Number of tubes, Nt = 158
Density of Steel, 𝜌𝜌𝑠𝑠 = 7850 Kg /m3
Density of Water in tubes = 995 Kg /m3

Volume of Shell body, V = (π / 4) (Do2 – Di2) x L = 0.0311 m3


Weight of Shell body, Ws = V x 𝜌𝜌s =
244.54 Kgs

Volume of Tubes, Vt = (π / 4 ) ( do 2 – di2 ) x L x Nt = 0.0863 m3


Total Weight of Tubes, Wt = Vt x 𝜌𝜌s
= 677.61 Kgs
Volume of Head, Vh = 0.087 D 3
= 0.0172 m3
Weight of Head, Wh = Vh x 𝜌𝜌s
= 135 Kgs

Weight of Liquid, Wl = ( π / 4) (d 2) x L x N x 995

= 152.69 Kgs
Total Weight, W = Ws+ Wt + Wh + Wl = 1220.84 kgs =12.20KN
79
Depth of head, H = 250 mm

Q = (W/2) = 6.1042KN
Now, we calculate,
Distance of saddle center line from shell end,
A = 0.4 x Ri
= 0.4 x (590/2)
= 118 mm
Longitudinal Bending Moments :
Radius, R = 0.295 m
Depth of head, H = 0.250 m
The bending moment at the supports is
M1= QA [ 1 – {(A/L)+ (R2 - H2) / 2 AL}/{1 + 4H/3L}]
= 48.464 N-m
The bending moment at the center of the span is given by
M2 = (Q L / 4)[{1+ 2 ( R2 - H2 ) / L2 }/{1+ 4H / 3L} - ( 4A / L) ]
= 6189.17 N-m
Stress In Shell At The Saddle :
For 𝜃𝜃 =120
k1 = 0.107
k2 = 0.192
Thickness of shell, t = 8 mm
f1 = M1/( k1πR2 t)
= 207.059 x 103 N/m2
f2 = M1/( k2πR2 t)
= 115.39 x 103 N/m2

80
Stress In The Shell At Mid- Span :
The stress at the mid span is f3, which is either tensile or compressive
depending on the position of the fiber. The resultant tensile stresses (including the
axial stress due to internal pressure) should not exceed the permissible stress, and
the resultant compressive stress should not exceed the permissible compressive
stress
f3 = M2 / (πR2 t) =2.82 x 106 N/m2

Axial Stress in Shell due to internal pressure


fp= (P x Di )/ (4 t) = 2.0306 x 106 N/m2
All combined stresses ( fp + f1 ) , ( fp + f2 ) , and ( fp + f3 ) are well within
allowable limits. Hence, the given parameters can be considered for design.
Thus, a shell and tube Heat Exchanger with the above specifications is designed.

81
Fig. 22 - EQUIPMENT DESIGN FOR SHELL AND TUBE HEAT EXCHANGER (HX)

TYPE : TEMA – ‘S’ TYPE (1 – SHELL PASS; 4 – TUBE PASS )


TUBE SIDE HEAT TRANSFER COEFFICIENT (hio) = 5370.14 W/m2.⁰C
SHELL SIDE HEAT TRANSFER COEFFICIENT (ho) = 8594.5 W/m2.⁰C
NUMBER OF TUBES = 158
TUBE OD = 20 mm
TUBE ID = 16 mm
PITCH = 0.025 m
∆PSHELL = 30.87 kPa
∆PTUBE = 25 kPa
NOZZLE DIAMETER = 100 mm
BAFFLES : TRANSVERSE SEGMENTAL BAFFLE
MATERIAL OF CONSTRUCTION: CARBON STEEL ( SHELL )
STAINLESS STEEL ( TUBE )

82
5.3 ABSORPTION COLUMN (ABS) :
Table. 21 – Parameters involved in Absorption Column
Ls 140.991 kmol/hr
Solvent (WATER) Density (𝜌𝜌𝜌𝜌) 993.95 kg/m3
Molecular weight 18.01 kg/kmol
Gs 1122.1383 kmol/hr
Feed Density (𝜌𝜌𝜌𝜌) 2.8435 kg/m3
Average Mol. Weight 30.24 Kg/kmol
Flv = (Ls/Gs) *(𝜌𝜌𝜌𝜌/𝜌𝜌𝜌𝜌)^0.5 = 2.34909
From Coulson and Richardson’s, Chemical Engineering, Volume 6
K4 = 0.15
Flooding velocity Uv= K4*�(𝜌𝜌𝜌𝜌 − 𝜌𝜌𝜌𝜌)/𝜌𝜌𝜌𝜌 = 2.800 m/s
Design at 85%, Uf = 0.85*2.800 = 2.380 m/s
V=(Gs*Mw)/(3600* 𝜌𝜌𝜌𝜌) = 3.3149 m3/s
Area required =3.3149/2.380 =1.392 m2
D =�(1.392 ∗ 4)/𝜋𝜋 = 1.3315 m
Therefore, from nearest BS Standard Di = 1330 mm and DO =
1337 m
Number of stages =20
Tray spacing = 0.5m
Therefore, Height of the column = Number of stages * tray spacing
=20*0.5 +(2*0.5) =11m
Table. 22 – Mechanical factors for Absorption Column design

Operating pressure 4 Bar


Design pressure 0.4 N/mm2
DESIGN STRESS (f) 95 N/mm2
TENSILE STRENGTH 360 N/mm2
JOINT FACTOR 0.85

83
Di 1330 mm
Vessel Thickness :
T = pDi/(2fJ-P) = (0.4*1330)/(2*95*1-0.4) = 6.302 mm
For sake of rigidity Take vessel thickness = 7mm
Head And Closure :
Torispherical are often referred to as dished ends. After comparing the
thickness of all heads, torispherical head had been chosen because of
operating pressure for this below 10 bars and suitable for liquid vapor phase
process in inconsistent high pressure. The thickness of torispherical head can
be calculated below
th = (P*Rc*Cs)/(2Jf+p(Cs-0.2))
where, Cs = 0.25(3+sqrt(Rc/Rk)
Rc=crown radius = Dc = 1330mm
Rk =knuckkle radius =0.06*Rc=79.8 mm
Cs= 1.7706
th= 5.810 mm
Take head thickness same as that of vessel thickness, th= 7mm
Weight Loads :
The major sources of the dead weight loads are:
1.The vessel shell
2.The vessel fittings: manhole, nozzles
3.Internal fitting: plates, heating cooling coils
4.External fittings: ladders, platforms, piping
5.Insulation
• Dead Weight Of Vessel:

84
Dead weight of vessel can be calculated by using equation below:
Wv = 240 x Cv x Dm x (Hv + 0.8 Dm)t x 10-3 kN
where, Wv= total weight of shell, excluding internal fitting such as
plates
Cv= a factor to account for the weight of nozzles, man ways
and internal supports. (For absorbtion column, take Cv as 1.15)
Dm= mean diameter of vessel= (Dc + t) m= (1.330 +
0.007)=1.337 m
Hv= height or length between tangent lines = 11m
t= wall thickness, m
Wv = 240 x 1.15 x 1.337(11.0 + 0.8(1.337)) x 0.007= 31.176 kN
• Weight Of Plates:
From Nelson Guide, page 833 Chemical Engineering Volume 6; take
contacting plates, 1.2 kN/m2 (for typical liquid loading). The total of
weight of plate determine by multiply the value with number of plate
design.
π
Plate area = = 4 * Di2 = 1.3894 m2
Weight of plate = Typical standard loading*plate area = 0.12*1.3894=
1.6673 kN
For 20 stages, Wp = 20*1.6673 = 33.34 kN
• Weight of Insulation :
The mineral wool was chosen as insulation material. By referring to Coulson
& Richardson, Chemical Engineering Design, Volume 6, page 833,
Density of mineral wool, ρ = 130 kg/m3
Thickness = 75 mm = 0.075 m

85
Volume of insulation, Vi= π x Di x Hv x thickness of insulation
= (3.142)(1.330)(11)(0.075) = 3.447 m3
Weight of insulation, Wi = Volume of insulation x ρ x g
= 3.447 x 130 x 9.81= 4396.67 N = 4.396 kN
Weight of fittings= 2*weight of insulation = 2*4.396 = 8.793 kN

Total Weight :
The total weight is the summation of dead weight of vessel, weight of accessories
and weight of insulation:
Total weight = Wv + W ρ + Wi = 31.176+33.347+8.793 = 73.3174 kN
Wind Load :
A wind loading must be designed to withstand the highest wind speed that is
likely to encounter at the site during the life of the plant. From the British Standard
Code of Practice BS CP 3: 1972 “Basic Data for the Design of Buildings, Chapter
V Loading: Part 2 Winds Load”, (Sinnott, 1999), a wind speed of 160 km/h (100
mph) can be used for preliminary design. For cylindrical column, semi-empirical
equation can be used to estimate the wind pressure:
Pw = 0.05 x u2
where, Pw= wind pressure, N/m2
u= wind speed, km/h
Pw = 0.05 (160)2 = 1280 N/m2
Mean diameter, including insulation = Di + 2(t + tins)
= 1330 + 2(7 + 75)
= 1494 mm
= 1.494 m

86
Loading (per linear meter), Fw = Pw*Deff = 1280 x 1.5 = 1920 N/m
𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚, 𝑀𝑀𝑀𝑀 =𝐹𝐹𝐹𝐹 𝐻𝐻𝐻𝐻2/2 =1920 × 112/2 = 116160 Nm = 116.16 kN m
Analysing Stresses On Vessel:
• Pressure Stresses :
1. Longitudinal Stress is given by,
𝜎𝜎𝐿𝐿 = 𝑃𝑃𝑃𝑃 ∗ 𝐷𝐷𝐷𝐷/4 ∗ 𝑡𝑡 = 0.4*1330/4*7 = 19 N/mm2
2. Circumferential Stress is given by,
𝜎𝜎ℎ = 𝑃𝑃𝑃𝑃 ∗ 𝐷𝐷𝐷𝐷/2 ∗ 𝑡𝑡 = 0.4*1330/2*8 = 38 N/mm2
• Dead Weight Stress :
Dead weight stresses are significant for tall columns. This stress can be
tensile for points below the column support or compressive for points above
the support. Dead weight stresses are given by:
𝜎𝜎𝑤𝑤 = 𝑊𝑊/(3.14(𝐷𝐷𝐷𝐷 + 𝑡𝑡)𝑡𝑡= 73.3174/3.14(1330+7) *7 = 2.4932 N/mm2
• Bending Stress :
The bending stress will be compressive or tensile, depending on
location and are given by:
𝑀𝑀𝑀𝑀 𝐷𝐷𝐷𝐷
𝜎𝜎𝑏𝑏 = ± � � � + 𝑡𝑡� 𝑤𝑤ℎ𝑒𝑒𝑒𝑒𝑒𝑒, 𝑀𝑀𝑀𝑀 − 𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇𝑇 𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏𝑏 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚
𝐼𝐼𝐼𝐼 2
𝜋𝜋
𝐼𝐼𝑣𝑣 = � � (𝐷𝐷𝑂𝑂4 − 𝐷𝐷𝑖𝑖4 )
64
𝜋𝜋
𝐼𝐼𝐼𝐼 − 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 = � � (1338_^4 − 1330_^4 )
64

= 3257540001 mm4
𝜎𝜎𝑏𝑏 = ± 0.02396 𝑁𝑁/𝑚𝑚𝑚𝑚2

• The Resultant Longitudinal Stress :


The resultant of longitudinal stress is the summation of longitudinal
stresses, dead weight stresses and bending stress.

87
𝜎𝜎𝜎𝜎 = 𝜎𝜎𝜎𝜎 + 𝜎𝜎𝜎𝜎 ± 𝜎𝜎𝜎𝜎
For upwind,
𝜎𝜎𝜎𝜎 = 19+ (−2.4932) + 0.02396 = 16.530 N/mm2
For downwind,
𝜎𝜎𝜎𝜎 = 19+ (−2.4932) – 0.02396 = 16.48 N/mm2
Therefore, the greatest difference between the principle stresses,
𝜎𝜎𝜎𝜎 = 𝜎𝜎h − 𝜎𝜎𝜎𝜎 (up𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤) = 38 – 16.53 = 21.469 N/mm2
The value obtained is well below the maximum allowable design stress
which is 95 N/mm2
Vessel Support Design :
The method used to support a vessel will depend on the size, shape, and
weight of the vessel; the design temperature and pressure, the vessel location and
arrangement; and the internal and external fittings and attachment. Since the
Absorption column is a vertical vessel, skirt support is used in this design.
A skirt support consists of a cylindrical or conical shell welded to the base of
the vessel. A flange at the bottom of the skirt transmits the load to the foundations.
The skirt may be welded to the bottom, level of the vessel. Skirt supports are
recommended for vertical vessels as they do not impose concentrated loads on the
vessel shells; they are particularly suitable for use with tall columns subject to
wind loading.

Type of support = Straight cylindrical skirt


𝜃𝜃 = 90°
Material of construction = Carbon Steel
Design stress, f = 95 N/mm2
Young’s modulus = 200,000 N/mm2

88
Skirt height, hs =4m
Skirt thickness, ts = 8 mm
Joint factor = 0.85
Weight of the Skirt :
Approximate weight, Wapprox = (π/4 x Di2 x Hv) x ρL x 9.81
= (π/4 x 1.3302 x 11) x 986.221 x 9.81 = 53771.56 N = 53.771 kN
Weight of vessel, W = 73.314 kN
Total weight = 53.771 kN + 73.314 kN = 127.089 kN

Analysis of Stresses of Skirt :


• Bending moment of skirt, Ms
Ms = 0.5 x Fw (Hv + Hs)2 = 0.5 x 1.92(11 + 4)2 = 216 kNm
• Bending stress of skirt, σbs
𝜎𝜎𝜎𝜎𝜎𝜎 = 4 𝑀𝑀𝑀𝑀 / 𝜋𝜋 (𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡) × 𝐷𝐷𝐷𝐷 x 𝑡𝑡𝑡𝑡
= 4 × 116.16 × 103 × 103/ 𝜋𝜋 (1330 + 8) × 1330 × 8 = 19.315 N/mm2
• Dead weight stress in skirt, σws
𝜎𝜎𝜎𝜎𝜎𝜎 (𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡) = 𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊𝑊 /𝜋𝜋 𝑡𝑡𝑡𝑡(𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡)
=53771.56/𝜋𝜋 × 8(1330 + 8) = 1.599 N/mm2
𝜎𝜎𝜎𝜎𝜎𝜎 (𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜) = 𝑊𝑊/𝜋𝜋𝜋𝜋𝜋𝜋(𝐷𝐷𝐷𝐷 + 𝑡𝑡𝑡𝑡)
= 73.3174/𝜋𝜋 × 8(1330 + 8) = 2.1799 N/mm2
• Resultant stress in skirt, σs
Maximum σs (tensile) = σbs + σws test = 19.315 + 2.1799 = 20.91755
N/mm2
Maximum σs(compressive) =σbs- σws operating=19.315 – 2.1799
=17.135N/mm2
• Criteria for Design
89
Take the joint factor, J as 0.85 Where θs = 90°
σs (tensile) < fs J sin θs
20.9155 N/mm2 < 95 x 0.85 sin 90°
20.9155 N/mm2 < 80.75 N/mm2
σs (compressive) < 0.125 E(ts/Ds) sin θs
17.135 N/mm2 < 0.125 x 200000(8/1330) sin 90°
17.135 N/mm2 < 150.37 N/mm2. Both the criteria are satisfied.
Nozzle Reinforcement :
Area for area method is used to provide reinforcement. The below nozzles
are in the channel cover (dished). The design pressure is same as that of tube.
• Nozzle diameter: 75mm (Exhaust gas in and out)
t s = p Di / (2fJ – p) +c = 0.186 mm
4 mm standard nozzle thickness is used for safety and rigidity. Maximum
nozzle distance = 2 d = 2 x 75 = 150 mm
Maximum vertical distance for compensation provided outside the vessel
=2.5 th = 2.5 x 7= 17.5 mm
Area for compensation required A = d*tn = 75 x 4 = 300 mm2
Area available for compensation as follows:
• Portion on head having excess thickness
Ah = d (ts – ts’ – c) = 75 (7 – 5.81) = 89.25 mm2
• Portion of nozzle external to vessel
Ao = 2 x 2.5 tn (tn – tn’ – c) = 2 x 2.5 x 7 (7-0.186) = 238.49 mm2
• Portion of the nozzle inside the head is zero
As + Ao =327.74 mm2 > A
Nozzle Reinforcement is not required.

• Hand hole diameter: 250 mm


90
ts = p Di/ (2fJ – p) +c = 0.620 mm
4 mm standard nozzle thickness is used for safety and rigidity. Maximum
nozzle distance = 2 d = 2 x 250 = 500 mm
Maximum vertical distance for compensation provided outside the vessel
=2.5 ts = 2.5 x 7 = 17.5 mm
Area for compensation required A = d*tn = 250 x 4 = 1000 mm2
Area available for compensation as follows:
• Portion on head having excess thickness
Ah = d (ts – ts’ – c) = 250 (7-5.81)= 297.5 mm2
• Portion of nozzle external to vessel
Ao = 2 x 2.5 tn (tn – tn’ – c) = 2 x 2.5 x 7 (7 – 0.62) = 223.3 mm2
• Portion of the nozzle inside the head is zero
A > As + Ao
Area = 1000 – (297.5+ 223.3) = 479.2 mm2 is provided as reinforcement
ring.
• Reinforcement ring
Inside diameter = dn + 2t = 258 mm Outside diameter = 350 mm < 2dn
Thickness of ring = 6 mm
Area of compensation ring = (350 -258) x 6 = 552 mm2 (> 460 mm2)

91
5.4 STORAGE VESSEL :
Tank diameter, d = 20 m
Tank height, h = 12 m
Material of Construction: Carbon steel
Density of Liquid = 890 kg/m3
Superimposed load = 1250 N/mm2
Permissible stress, f = 140.6 N/mm2
Density of stainless steel = 7700 kg/m3
Modulus of elasticity = 2*105 N/mm2

Shell Thickness :
P = 𝜌𝜌*(H-0.3)*g
= 890*(12-0.3)*9.807*10-6 = 0.10206 N/mm2
Thickness of shell, ts = PD/2fJ
= (0.10206*20*103 )/(2*140.6*0.85)
= 8.54051mm
Take 10 mm thickness.
Assume 7 plates to be used with a gap of 2mm between the adjacent plates
Total circumference = (𝜋𝜋*20)-(7*2*10-3) = 62.82 m
Length of each plate = 62.82/7 = 8.975 m
The size of the plate selected from IS1730 is 9000(L) *1800(W)
Assume plate thickness to be 8mm
H = t*2*f*J)/(𝜌𝜌 *g*D)) +0.3
=((8*2*140.6*0.85)/(890*9.807*10-6*20*103)
= 11.2594 mm
The balance height =12-11.259 = 0.7405 mm is filled with 8mm plate.
One plate of 10 mm thickness should be used at the bottom which would cover a

92
height of 1.8 m
Remaining height = 12-1.8 = 10.2 mm
Assume plate of thickness 6 mm
H = t*2*f*J)/(𝜌𝜌 *g*D)) +0.3
= ((6*2*140.6*0.85)/(890*9.807*10-6*20*103)
= 8.5196 mm
The balance height =10.2-8.5196 =1.6803 mm is filled with 6 mm plate.
One plate of 8 mm thickness should be used which would cover a height of 1.8 m.
Remaining height = 12-1.8-1.8 = 8.4 mm
Assume plate of thickness 4 mm
H = t*2*f*J)/(𝜌𝜌 *g*D)) +0.3
= ((4*2*140.6*0.85)/(890*9.807*10-6*20*103)
= 5.779 mm
The balance height =8.4-5.779 =2.620 mm is filled with 4 mm plate.
Two plate of 6 mm thickness should be used which would cover a height of 1.8 m.
For the Remaining height 3 layers of 4 mm plates should be used.
Therefore 1 plate of 10 mm thickness,1 plate of 8mm thickness, 2 plates of 6mm
thickness and 3 plates of 4mm thickness can be used.
Tank Bottom :
Assume diameter of bottom extend beyond shell by 65mm.
Db = 20+((2*8)/1000) + ((2*65)/1000) = 20.15 m
Thickness of plate to be used to bottom Annular plate = 8 mm
Sketch plate = 6 mm
Bottom plate is lap welded
Minimum width of annular plate = 65+380+65+10 = 520 mm
Circumference of bottom = 𝜋𝜋*Db = 3.14*20.15 = 63.271 m

93
Self- Supporting Conical Roof :
Assuming plate thickness for roof plates to be 6 mm
Weight per unit area = 6*10-3*7700 = 46.2 kg/m2
Force acting due to load = 46.2*9.807 = 453.08 N/m2
Total load = superimposed load + load due to weight
= 1250 + 453.08 = 1703.08 N/m2
= 1703.08*10-6 N/mm2
sin 𝜃𝜃 = (D/t) √P/0.204E
= (20*103 /6) * √(1703.08*10-6 /0.204*2*105)
sin 𝜃𝜃 = 0.6810
tan 𝜃𝜃 = 0.930
The slope is acceptable.
Nozzle Design :
Nozzle diameter at head = 200 mm
Nozzle diameter at shell = 300 mm
Nozzle (in the head) tn= pDi / (2fJ – p)
= (0.11145*200)/(2*140.6*0.85)-0.11145) = 0.085 mm
For sake of rigidity, nozzle thickness is taken as 3 mm which is standard size.
Maximum nozzle distance = 2*d = 2*200 = 400 mm
Maximum vertical distance for compensation provided outside vessel
= 2.5* th = 2.5*4 =10 mm
Area for compensation required A = d*th = 200*4 = 800 mm2 Area available for
compensation is as follows:
• Portion on head having excess thickness
As = d*(ts – ts’ – c) = 200*(4-0.085) = 783 mm2
ts - actual thickness of head

94
ts’- theoretical thickness of head
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*4(4-0.085) = 78.3 mm2
• Portion of nozzle inside the head is zero
Therefore, area available for compensation = 783 + 78.3 = 861.3 mm2
(AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.

• Stream in nozzle (in the shell at top) :


tn= pDi / (2fJ – p) = (0.11145*300)/(2*140.6*0.85)-0.11145) = 0.128 mm
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*300 = 600 mm
Maximum vertical distance for compensation provided outside vessel = 2.5*ts
= 2.5*3 = 7.5 mm
Area for compensation required A = d*ts = 300*3 = 900 mm2
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 300*(3-0.128) = 861.1 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5*ts(tn – tn’ – c) = 2*2.5*4(3-0.17) = 57.44 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 861.1+57.44 = 919.04 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.
• Stream out nozzle (in the shell at bottom) :
tn= p*Di / (2fJ – p) = (0.11145*300)/(2*140.6*0.85)-0.11145) = 0.128 mm

95
Considering rigidity, nozzle thickness of standard size is taken as 3 mm.
Maximum nozzle distance = 2*d = 2*300 = 600mm
Maximum vertical distance for compensation provided outside vessel = 2.5*ts
= 2.5*3 = 7.5 mm
Area for compensation required A = d*ts = 300*3 = 900 mm2.
Area available for compensation is as follows:
• Portion on shell having excess thickness
As = d*(ts – ts’ – c) = 300*(3-0.128) = 861.1 mm2
• Portion of nozzle external to vessel
Ao = 2*2.5* ts(tn – tn’ – c) = 2*2.5*10(3-0.128) = 143.6 mm2
• Portion of nozzle inside the head is zero
Area available for compensation = 861.1+143.6 = 1004.7 mm2
AS+AO)>A, THIS IS SATISFACTORY.
Nozzle reinforcement not required.

96
97
5.5 PUMP :
Pipe specifications :
Diameter of pipe (D) = 0.03 m
Length of pipe (L) = 10 m
Material used : Cast iron
Absolute roughness of pipe (ε) = 0.000259 m
Cross sectional area of pipe (A) = (π/4) D2
= (π/4) 0.032
A = 0.0007069 m2
Fluid specifications :
ṁ = 13158 kg/hr
Density of fluid (ρ) = 986.221 kg/m3
Viscosity of fluid = 0.000622516 kg/ms
Volumetric flow rate (Q) = ṁ/ρ
Q = 13.341 m3/h
Calculation of Darcy friction factor :
Linear velocity (v) = Q/A
= 13.341 /(0.0007069)
v = 5.24 m/s
Reynolds number (Re) = ρvD/µ = 249044.10 ~ 2.5 * 105 (turbulent
regime)
Relative roughness = ε/D
= 0.000259 /0.03
= 0.008633
The value of friction factor is found from the values of Reynolds Number and
relative roughness from Moody’s chart.
Darcy Friction factor (fD) = 0.035
98
System Head calculation :
Heads measured are in the basis of WC (Water Column)
Pressure at suction = 101325 Pa
Velocity at suction = 5.24 m/s
Elevation at suction =1m
Pressure at discharge = 101325 Pa
Velocity at discharge = 5.24 m/s
Elevation at discharge = 5.5 m
Table No. 23 – Pump Head values
Formula Head
Head Suction Discharge
( Unit - m ) Difference

Pressure P/ρg 10.476 10.476 0


Elevation z 1 5.5 4.5
Velocity v2/2g 1.399 1.399 0
Total Head 4.5

Fig. 24 – Illustration of piping connections involved for pump design

99
Number Actual
Head losses K factor
of units K values
Head loss at entrance 0.5
0.5 1
(sharp edge)
Head loss due 90o elbow 0.3 2 0.6
Head loss due to Reducer (θ = 30o) 0.2 1 0.2
Head loss due to Globe Valve 10 1 10
Head Loss due to Expander (θ = 20o) 0.3 1 0.3
Head loss at exit 1 1 1
Overall K factor 11.6
Table No. 24 – Pump Minor Losses
Pump Selection :

Fig. 25 – Pump performance curve for a range of pumps


(Lines represent different pump models )

100
From Bernoulli’s equation, system curve equation is found to be
(𝑝𝑝𝑑𝑑 − 𝑝𝑝𝑠𝑠 ) 𝐿𝐿 𝑣𝑣 2
𝐻𝐻𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 = + (𝑧𝑧𝑑𝑑 − 𝑧𝑧𝑠𝑠 ) + �𝑓𝑓𝐷𝐷 + 𝐾𝐾𝑜𝑜𝑜𝑜𝑜𝑜 �
𝜌𝜌𝜌𝜌 𝐷𝐷 2𝑔𝑔
0.035∗10
Hsystem = 4.5 + � + 11.6�*1.399
0.3

= 22.36 m

For the given volumetric flow rate, at optimum operating condition is found when
Head offered by the (Hpump) = Hsystem ~ 22.5 m
This condition is satisfied by the pump model – 30.15

101
Fig. 26 – Extended Pump Characteristic curves for selected pump model

102
From the figure ,
NPSHrequired = 3.5 m
Efficiency, η = 32 %
Power, P = 2.5 kW
These are verified in the following section.

Pump Specification :
Vendor : LUTZ Pumps
Model : TMR 30.15
Suction ID : 50 mm
Discharge ID : 40 mm
Speed : 2900 min-1
Impeller Diameter : 130 mm
Frequency : 50 Hz
Max. Density : 1.35 kg/m3
Max. Head : 42 m
Max. flow rate : 48 m3/hr
Motor power : 5.5 kW
Motor : IE 3 class, 3 phase, 400v, 50 Hz, IP 55 water resistant motor
Operating Temperature : -5 to +80 °C
Materials of construction :
Volute casing : Polypropylene ( glass fibre reinforced )
Rear Casing : Polypropylene ( glass fibre reinforced )
Centrifugal impeller : Polypropylene
Guide bearing : Silicon Carbide
Shaft : Ceramics
Thrust ring : Ceramics

103
Screws : Stainless Steel
Calculation of Net Positive Suction Head :
𝑣𝑣𝑣𝑣𝑣𝑣
Vapor pressure of Mixture = ∑𝑖𝑖 𝑥𝑥𝑖𝑖 𝑝𝑝𝑖𝑖
= 1.725 kPa
NPSHavailable = Ps/ρg + zs – Pvapmix/ρg
= 10.476 + 1 – 0.176
NPSHavailable = 11.3 m
NPSHavailable > NPSHrequired
So cavitation is highly unlikely.
Calculation of Power required :
Power required by the pump = (ṁ /3600) g Hsystem
P = 801.73 W
P ( water horsepower ) = 1.075 hp
Pump efficiency = 32 %
Actual power required =1.075/.32 = 3.359 hp =2504.8 W

104
CHAPTER 6
ECONOMIC ANALYSIS

105
6. ECONOMIC ANALYSIS :
The purpose of chemical processes is to make money. An understanding of
process economics is therefore critical in process design. The total investment
required for a new design can be broken down into five main parts:

• Battery limits investment

• Utility investment

• Off-site investment

• Engineering fees

• Working capital
6.1 Total Equipment Cost:
The purchased equipment cost for common plant equipment is given by,
Ce = a + bSn
where the values of a, b and n are constants that depend on the equipment.

Table No. 24 – Equipment Base Cost Estimation

Equipment Property S a b n Cost (In $) Cost (In Rupees)


Pump Power(kW) 2.5 560 310 0.7 $ 1,148.73 ₹ 80,000
Diameter(m) 1.22 100 120 2 $ 278.61 ₹ 19,503
Column ₹ 20,00,000
Shell mass(kg) 3353.06 -10000 295 0.6 $ 28,466.87 ₹ 19,80,497
Heat
Area(m2) 48.01 4000 65 1 $ 7,120.65 ₹ 5,00,000
Exchanger
Reactor Volume(m3) 66 13000 68 0.7 $ 14,277.00 ₹ 10,00,000
Storage Volume(m3) 3769.91 2000 16 0.6 $ 4,238.30 ₹ 3,00,000

106
Table No. 25 – Total Equipment Cost Estimation

Bare Bare
Purchase Estimated
Type Module Module Quantity
Cost Cost
Factor Cost

Storage
₹ 3,00,000 3.21 ₹ 9,63,000 3 ₹ 28,89,000
Vessel

Pump ₹ 80,000 3.3 ₹ 2,64,000 4 ₹ 10,56,000


Column ₹ 20,00,000 2.15 ₹ 43,00,000 3
1,29,00,000

Heat ₹
₹ 5,00,000 4.16 ₹ 20,80,000 7
Exchangers 1,45,60,000

Reactor ₹ 10,00,000 4.16 ₹41,60,000 2 ₹ 83,20,000

Total Equipment Cost (EC) ₹3,97,25,000

6.2 Total Direct Cost:

Table No. 26 – Total Direct Cost Estimation

Services Factor (Multiply with EC) Estimated Cost

Installation cost 0.1 ₹ 39,72,500.0

Foundation cost 0.1 ₹ 31,78,000.0

Platform and support cost 0.1 ₹ 27,80,750.0

Erection of equipment cost 0.2 ₹ 59,58,750.0

Piping cost 0.2 ₹ 59,58,750.0

107
Service utilities 0.1 ₹ 39,72,500.0

Building cost 0.5 ₹ 1,98,62,500.0

Electrical cost 0.1 ₹ 39,72,500.0

Total Direct Cost (TDC) ₹ 4,96,56,250.0

Working capital cost = 25 % of TDC

= ₹ 1,24,14,062.5

Startup capital = 1 % of TDC

= ₹ 49,65,625.0

Total Direct Expenditure (TDE) = TDC + Working Capital + Startup capital

= ₹ 6,70,35,937.5

6.3 Total Indirect Cost:

Table No. 27 – Total Indirect Cost Estimation


Services Factor Estimated Cost

Engineering and supervision 0.4 ₹ 1,58,90,000.00

Construction expenses 0.425 ₹ 1,68,83,125.00

Contractor fee 0.1875 ₹ 74,48,437.50

Contingency 0.1875 ₹ 74,48,437.50

Total Indirect Cost (TIC) ₹ 4,76,70,000.00

Fixed Capital Investment (FCI) = TDC + TIC

= ₹ 9,73,26,250.00

108
Working Capital Investment (WCI) = 15 % of FCI

= ₹ 1,45,98,937.50

Total Capital Investment (TCI) = FCI + WCI

= ₹ 11,19,25,187

Local taxes = (6% of FCI) = ₹ 58,39,575.00

Insurance = (0.9% of FCI) = ₹ 8,75,936.25

Total Fixed Charges (FC) = (Local tax + insurance) = ₹ 67,15,511.25

6.4 Raw Material Cost:

Table No. 28 – Raw material Cost Estimation


Raw Material Cost (RS. /kg) Quantity(kg/yr) Total Cost

Propene 66 136126697.1 ₹ 8984362011

Butanol 39 49888080 ₹ 1945635120

Water 20 17780400 ₹ 355608000

Total Material Cost (RMC) ₹ 11285605131

6.5 Operating Labor Cost:

Table No. 29 – Operating Labor Cost Estimation


Post No.Of Posts Annual Salary Per Post Total Salary

General Manager 1 ₹ 9,00,000.00 ₹ 9,00,000.00

Production Manager 1 ₹ 6,00,000.00 ₹ 6,00,000.00

Engineers 5 ₹ 4,20,000.00 ₹21,00,000.00

Skilled Workers 14 ₹ 2,50,000.00 ₹35,00,000.00

109
Clerks 3 ₹ 2,20,000.00 ₹ 6,60,000.00

Medical Staffs 3 ₹ 1,50,000.00 ₹ 4,50,000.00

Unskilled Labour 10 ₹ 1,10,000.00 ₹11,00,000.00

Administrative 4 ₹ 1,20,000.00 ₹ 4,80,000.00

Security 3 ₹ 90,000.00 ₹ 2,70,000.00

Total Operating Labour Cost (TLC) ₹1,00,60,000.00

6.6 Total Utility Cost:

Cost of electricity = ₹ 2,00,00,000.00

Cost of water = ₹ 1,80,00,000.00

Cost of packing = ₹ 1,00,00,000.00

Total utility cost (TUC) = ₹ 4,80,00,000.00

Maintenance and repair cost = 6 % of TDC

= ₹ 29,79,375.00

Laboratory cost = ₹ 15,00,000.00

Insurance = 1 % of TDC

= ₹ 4,96,562.50

Plant Overhead cost = 2 % of TLC

= ₹ 20,12,000.00

Total miscellaneous cost (TMC) = ₹ 69,87,937.50

6.7 Revenue from Sales:

110
Selling price = ₹ 193.00

Annual production = ₹ 6,10,50,000.00

Sales revenue = Selling Price * Annual Production

= ₹ 11,78,26,50,000.00

6.8 Expenses:

Total Production Cost (TPC) = RMC + TUC + TLC + TMC

= ₹ 11,35,06,53,068.93

Patent and royalty cost = 3 % of Revenue

= ₹ 35,34,79,500.00

Research and development expenses = ₹ 20,00,000.00

Distribution and marketing cost = 0.2 % of Revenue

= 2,35,65,300.00

EXPENSES = ₹ 11,72,96,97,868.93

6.9 Profitability Study:

Profit before taxes = Expenses – Revenue

= ₹ 5,29,52,131.07

GST = 18 % of Profit before Taxes


= ₹ 95,31,383.59

Net profit = Profit before Taxes – GST

= ₹ 4,34,20,747.48

111
Actual value (V) = ₹ 9,73,26,250.00

Salvage value (Vs) = ₹ 97,32,625.00

N = 20

(𝑉𝑉−𝑉𝑉𝑉𝑉)
Depreciation (D) = = ₹ 43,79,681.25
𝑁𝑁

𝐹𝐹𝐹𝐹𝐹𝐹
Payback period = = 2.04 years
(𝑁𝑁𝑁𝑁𝑁𝑁 𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃+𝐷𝐷)

112
CHAPTER 7
PIPING AND INSTRUMENTATION
DIAGRAM

113
7. INSTRUMENTATION AND PROCESS CONTROL
7.1 INTRODUCTION

Process control is concerned with the control of unit operation and unit processes.
Chemical plant processes can be regulated to obtain the objectives and
effectiveness by applying the feed backward or feed forward principles using
various computing devices like sensors, transmitters, controllers etc. It requires
sensors for measuring variables and valves for implementing decisions. The piping
and instrumentation (P&I) diagram is a pictorial representation of a process plant
having all the equipment along with the piping, valves, insulation and
instrumentation.

7.2 INSTRUMENTS

The different instruments used in the P&I diagram generally are

• Flow meters

• Level Meters

• Pressure gauge

• Thermometers and thermocouples

• Quality analysis devices

• Radiation measuring devices

7.3 MODES OF CONTROLLER


The basic modes of controller are
• On-off control

• Integral control

• Proportional control

114
• Rate or derivative control

P-Controller
The most common application of the p-controller is level controller. There is an
offset in the p-controller. The maintaining of the level does not require any accurate
measurements. So, P-controller is used as level controller.

PI-Controller
The PI controller is used as flow rate controller. PI-controller does not have any
offset. The measurement of the flow rate must be accurate and does not have any
offset. So, PI- controller is most commonly used as a flow controller.

PID-Controller
The PID controller is used as temperature controller and pressure controller. In PID
controller, the response will be faster and accurate. the temperature and pressure
must measure accurate and faster for taking the control action. So, PID controller
is most used.

7.4 CONTROL OBJECTIVES

The main objective of process control and instrumentation on the chemical plants
are as follows:

• To suppress the external and internal disturbances on the process system.

• To ensure the stability of the process.

• To optimize the performance of the process there by making the process


more economical.

115
7.5 NECESSITY OF PROCESS CONTROL

• Safety - To look for hazardous situation and to mitigate those situations by


providing emergency alarms, control valves and automatic shutdown
systems.

• Product Specification - To maintain the production composition according


to its quality standards.

• Environmental Regulation - To avoid environmental pollution by treating


the waste and vent gases and only an appreciable amount accepted by
Pollution Control Board is made to release into the atmosphere.

• Plant Economy - To operate the plant at very low production and operating
cost to increase the plant economy.

7.6 MEASURING ELEMENTS

• Temperature Measurement - It is essential for the effective production of


the product. Thermocouples, Resistance thermometers, Pyrometers are
used for the measurement of temperature.

• Pressure Measurement - Mechanical and Electrical pressure sensors are


used for measuring pressure in the process plant.

• Level Measurement - Liquid head pressure devices, dielectric constant


measuring instruments, sonic resonance devices are used primarily for the
measurement of level.

• Flow Measurement - Obstruction type, inferential, electromagnetic,


ultrasonic, Mass flow meters. These are the type of flow meters widely
used.

116
7.7 P&ID Symbols and their Representations

S. No SYMBOLS REPRESENTATION
1. TI Temperature Indicator
2. TT Temperature Signal Transmitter
3. TC Temperature Controller System
4. FI Flow Indicator
5. FT Flow Signal Transmitter
6. FC Flow Controller System
7. FIC Flow Indication Controller System
8. LI Level Indicator
9. LT Level Signal Transmitter
10. LC Level Controller System

117
Fig.27
118
CHAPTER 8
SAFETY ANALYSIS

119
8.1 HAZOP ANALYSIS:
8.1.1 Introduction:
A hazard and operability study (HAZOP) is a structured and systematic
examination of a complex planned or existing process or operation to identify and
evaluate problems that may represent risks to personnel or equipment. The intention
of performing a HAZOP is to review the design to pick up design and engineering
issues that may otherwise not have been found. The technique is based on breaking
the overall complex design of the process into a number of simpler sections called
'nodes' which are then individually reviewed. It is carried out by a suitably
experienced multi-disciplinary team (HAZOP) during a series of meetings. The
HAZOP technique is qualitative and aims to stimulate the imagination of
participants to identify potential hazards and operability problems. Structure and
direction are given to the review process by applying standardized guideword
prompts to the review of each node.
8.1.2 Objectives:
There are basically four primary objectives of any HAZOP study (Nolan 1994):
1. To identify the causes of all deviations of changes from the intended design
function
2. To determine all major hazards and operability problems associated with any
identified deviations
3. To decide whether action is required to control the hazard or operability
problems
4. To ensure that the actions decided on are implemented and documented
To identify deviations, the team applies (systematically, in order) a set of Guide
Words to each node in the process. To prompt discussion, or to ensure completeness,
it may also be helpful to explicitly consider appropriate parameters which apply to
the design intent. These are general words such as Flow, Temperature, Pressure, and

120
Composition. The current standard notes that Guide Words should be chosen which
are appropriate to the study and neither too specific (limiting ideas and discussion)
nor too general (allowing loss of focus). A standard set of Guide Words is as follows
Table No.30 - Guide words for HAZOP analysis

S.No Guide Word Meaning

1 NO OR NOT Complete negation of the design intent

2 MORE Quantitative increase

3 LESS Quantitative decrease

4 AS WELL AS Qualitative modification/increase

5 PART OF Qualitative modification/decrease

6 REVERSE Logical opposite of the design intent

7 OTHER THAN / INSTEAD Complete substitution

8 EARLY Relative to the clock time

9 LATE Relative to the clock time

10 BEFORE Relating to order or sequence

11 AFTER Relating to order or sequence

(The last five guide words are applicable to batch or sequential operations.)
Where a guide word is meaningfully applicable to a parameter e.g. NO FLOW,
MORE TEMPERATURE, their combination should be recorded as a credible
potential deviation (from the design intent) that requires review.
HAZOP-type studies may also be carried out by considering applicable
guide words and identifying elements to which they are applicable or by
considering the parameters associated with plant elements and systematically

121
applying guide words to them; although this last approach is not mentioned in the
relevant standard, its examples of output include a study (B3) recorded in this way.
The following table gives an overview of commonly used guide word - parameter
pairs and common interpretations of them.
Table No.31 - Guide words with associated parameters
Parameter /
Guide More Less None Reverse As well as Part of Otherthan
Word
reverse Deviating Deviating
Flow Highflow Low flow No flow Contamination
flow concentration material
High Low
Pressure Vacuum Explosion
pressure pressure
High Low
Temperature Temperat tempera
ure ture
Different
Level Highlevel Low level No level
level
sequence
Too long Too short Missing
Time step Backward extra actions wrong time
/ Too late / too soon actions
skipped
Fast Slow No
Agitation
mixing mixing mixing
Fast
Slow No Unwanted
Reaction reaction/
reaction reaction reaction
runaway
Start-up / Too fast Too slow Actions

122
Shutdown missed
Draining/ Deviating
Too long Too short none
Venting pressure

8.1.3 HAZOP Study on Packed Bed Reactor:


Table No. 32 - HAZOP analysis of PBR-1-NODE 1
Study node: Packed bed reactor Cooling coil Date: 7/06/2022
Operating Temperature: 270°C Team composition: LG, XY, PX, QW
Operating Pressure: 4 bar

Design Intention: Converts reactants Propene, steam, Air into Acrolein


Parameter Guide Deviation Possible Consequences Action Required
word Causes
Flow No No Flow 1.Blockage 1.Reactor 1.Regular
temperature maintenance of valve
in pipeline.
decreases. and pipeline
2.Boiler
2. No product 2.Install PID
fault.
forms controller
3. Valve fails
Flow Low Low Flow Partial Diminished Regular maintenance
blockage in cooling ofvalve and pipeline
valve or possible
pipeline runaway Install PID controller
Flow High High Flow Control Reactor Instruct Operator to
valve fails temperatures respond quickly
to open increases.
Product Update
contamination instrumentation

Temperature Low Low Condensation Poor heating None as it is


Temperature performance. favorable
of steam.
Boiler fault. Rate of
reaction
Leakage of
decreases
steam.

123
Conversion of
acrolein
reduces.

Temperature High High 1.High steam Product is Install high


Temperature
flow flammable. temperature alarms.
2.Boiler fault Leads to fire Install high
and explosion.
performance
Controllers.
Pressure Low Low Low steam Increase in Install low pressure
Pressure
supply concentration alarm
of propene, Proper maintenance
ofvalves
steam, air
Pressure High High High steam Damage of Install high pressure
Pressure
supply reactor alarms and sensors.
Explosion

Table No. 33 - HAZOP analysis of PBR-1-NODE 2


Study node: Packed bed reactor Cooling coil Date: 7/06/2022
Operating Temperature: 270°C Team composition: LG,XY,PD,QW
Operating Pressure: 4 bar

Design Intention: Converts reactants Propene, steam, Air into Acrolein


Parameter Guide Deviation Cause Consequence Action To Be Taken
Word

124
Flow No No Flow No Excess retains Use valve thatfails open
(inlet)
reaction in equipment Install alarm orsensor
material Equipment
Closed damage
Inlet Shortage in
valve product
Flow Less Less Flow Partially Partially closed Install flow meter
(inlet) closed Valve.
valve Less
Conversion.
Flow More More Control Temperature Install flow regulator
(inlet) Flow
valve fail decreases. andflow splitter
to open. Contamination Install pressureregulator
Pressure of product.
drop
Decreases.
Flow Reverse Reverse Valve Damage of Install check valve
(inlet) flow failure previous
equipment

8.1.4 HAZOP Analysis of Heat Exchanger:


Table No. 34 - HAZOP analysis of Shell and Tube Heat Exchanger

Study node: Packed bed reactor Cooling coil Date: 7/06/2022


Inlet Temperature of process fluid: 300°C Team composition: LG, XY, PD, QW
Outlet Temperature of process fluid: 70°C

Design Intention: To Reduce the temperature of the Acrylic-acetic mixture


Parameter Guide Deviation Causes Consequence Action required
Word

125
Pipe blockage
Flow No No flow of cooling No heat Install temperature
water exchange indicator before and
Failure to
occurs after the steaminlet
open inlet. valve
Cooling water
valve.
No Cooling
water.
Inlet line
rupture.
Malfunction in
the boiler
column
Power failure Further process
Flow No No process fluid Install low
in the pump stops temperature alarm

Clogging inthe No heat


pipes exchange occurs
Pipe blockage Process fluid Installation of
Flow Less
Less cooling water
temperature is low / high
flow Failure to
not increased/ temperature alarm
open inlet
decreased
valve properly
accordingly. Timely maintenance
Line leakage
ofvalves
Inadequate
Defect in
coolingwater
cooling
for the process.
Less Processfluid Process stream Less Installation oflow and
Flow Less
flow
inlet valve yield and high temperature
partially conversion alarm

126
closed Excess heating/
Pump fails cooling of the
(motor fault, process fluid
electricity
breakdown)

Line clogging
/Leakage
More Processfluid Process fluid Bursting of Installation of
Flow More
flow tubes
Failure to temperature indicator
closeinlet
Bursting of
valve
pipelines
More cooling Fail to close Corrosion of Install check
Flow Reverse
water inlet valve pipelines and
valve
flow shell
2.Malfunction
in the HE
Cooling getting Cooling Line Reaction gets Proper maintenance
Flow As well
mixed with disturbed
as valve failure ofvalves
process fluid
Breakage of
tubes

Leakage of
Cooling water
from thetubes
More pressure on Failure of Bursting of tube Install high pressure
Pressure More
tube side process fluid
alarm
valve
Corrosion of Hardness of Less cooling Cleaning
Corrosion
Equipment coolingwater
Of pipelines andtubes.
Cracks in Treatment ofwater
pipelines and
tubes

127
8.1.5 HAZOP analysis of Absorber:

Table No. 35 - HAZOP analysis of Absorber


Study node: ABSORBER Date: 7/06/2022
Operating temperature: 70°C Team composition: LG, XY, PD, QW
Operating pressure: 0.15 bar
Design Intention: To absorb acrylic acid mixture and remove other impurities by water

Guide Deviation Action To Be


Parameter Cause Consequence
Word Taken
Feed Flow No proper
No Blockage in Regular
absorption
pipeline maintenance of
No flow valves and pipe line
Inlet valve
failure

Partial Reduced
Low flow blockage Install flow
Low product controller
invalve or
formation
pipeline
High Failure of Reduced residence Install high flow
Control valve time alarms

Reduced product
High flow Formation
Feed Flow
Install
Unfavorable
operating bypasslines
Conditions

Flooding of
column
Reverse flow Damage to the
Reverse Valve failure previous Install checkvalves
equipment

128
Low Decreased rate Install
temperature Reduced feed ofreaction
Low temperature
temperature
controllers

Reduced
Temperature conversion
High High feed Install high
High temperature Formation of
temperature temperature alarms
hotspots within the
column
Install high
Might lead performance
toexplosion controllers

Runaway
reactionoccurs
Reduced Install low
Unfavorable
Low nitrogen operating condition pressure alarm
supply
Low pressure Reduced Proper
Pressure Reduced Absorption of acid maintenance of
vapor flow mixture
valves
rate
Unfavorable
operating
High supply condition
of Install high
High pressure nitrogen Reduced absorption pressure alarms
Pressure High of acid mixture
and pressure
High vapor Explosion of relief vents
flow rate column

129
8.1.6 HAZOP analysis of Centrifugal Pump-P1:

Table No. 35 - HAZOP analysis of Centrifugal pump

Study node: Centrifugal Pump -P1 Date: 7/06/2022


Operating temperature: 70°C Team composition: LG, XY, PD, QW
Operating pressure: 1 bar
Design Intention: To pump ACRYLIC-ACETIC acid mixture to Distillation column
Parameter Guide Deviation Cause Consequence Action To Be
Word Taken
Temperature More More 1.Failure/leak/improper Vaporization of 1.Check
liquid increase
temperature system connections temperature
in pressure
2.Very low flow causing frequently
destruction of
3.High pressure 2.Check
pump internal
Pump not submerged pressure/vent/
explosion and
Valve
fire
Temperature Less Less 1.More open of 1.Lubricant 1.Check
temperature cooling system character and coolingsystem
Low flow rates viscosity 2.Check no of
changes engine rounds
2.Damage of
bearings
Pressure More More 1.Blockage in outlet 1.Deterioration Check drain
pipes
pressure valve of bearings
2.Faulty pressure 2.Stop replace the
production
sensor gasketand
explosion
Vaporizing liquid damage check
Pressure Less Less 1.Close suction valve 1.Cavitation 1.Loss in
pressure
fittings
2.Faulty sensor 2.Vibration
Air leaks in suction 2.Ensure
damaging
line NPSHa>

130
internal pump NPSHr

Pressure No No 1.Close suction valve 1.Stop 1.Loss in


pressure
2.Faulty pressure Production Fittings
sensor
2.Check type of
3.Pump power failure
liquid to be
2.Stop pump
vibration used,
Submerged
NPSHa>NPSHr
Flow Too High flow 1.Engine power is 1.Overheating of 1.Reduce the
high
more pump speed of motor
2.Blockage in outlet 2.Cavitation rotation
valve 2.Check
3.Destructionof
variation of
3.Power absorbed by internal parts
liquid density
excessive pump from nominal
Flow Less Less flow 1.Failure at outlet 1.Temperature 1.Increase the
valve increases and pump rotation
2.Low rotation speed causes speed
3.Operating fault vibrations 2.Check and
Formation of pockets
2.Destructionof drain the pipes
pump internal and systems

131
Flow No No flow 1.Motor failure 1.Stop 1.check the
2.Closed discharge production liquid level/
3.Power outage
2.Overheating of vent
pump 2.Ensure
Explosion NPSHa>NPSHr

8.1.7 HAZOP Analysis of Distillation column-D1:

Table No. 37 - HAZOP analysis of Distillation Column

Parameter Guide Deviation Causes Consequences Action


word Required
Flow No No feed Full Pipe blockage No separation Install
flow
occurs flow
Inlet line rupture indicators
before and
after inlet valve
Less Low vapor Reboiler load Weeping Ensure
flow is lesser than required proper fuel
Reboiler pump stops Dumping supply for
working the heating
High to take place
Condenser load
High 1.High Low coolant supply in Entrainment and Ensure
vapor flow condenser flooding proper supply of
coolant
Proper supply of
valves
Pressure Less Low Pipe leakage Boiling 1.Regular
pressure inspection
in point reduced
distillation
column Requires
packed column

132
instead of
tray column

More High Contamination in the feed Boiling High


pressure in
distillation point increased pressure alarm
column Condenser overloaded
with vapors due to More number of Rupture disc
condenser fouling stages required installed

Reduced reboiler duty Increase in


Reboiler
and
condenser load
Temperature Low Low low fuel supply Low vapor flow Ensure adequate
temperature supply of fuel to
in reboiler Weeping
Reboiler pump not Reduced produce enough
pumping the steam separation steam
sufficiently efficiency
Column must be
restarted
Low Leaking in .Low liquid flow Ensure proper
temperature .Ruptures of supply of coolant
in coolant That valves valves
Rupture in pipeline and
Regular
maintenance of
valves
High High .Excessive steam supply .Damage in the High temperature
reboiler internal tubes
load .High vapor flow alarm

133
8.2 FAULT TREE ANALYSIS:

FTA is a top-down process by which an undesirable event (failure in a project


objective or a critical failure that can affect the project), referred to as the top event,
is logically decomposed into possible causes in increasing detail to determine the
causes or combinations of causes of the top event. FTA can yield both qualitative
and quantitative information about the system under study.

1. Qualitative information may include failure paths, root causes, and weak areas
of the system/project.

2. Quantitative analysis of a fault tree gives a probabilistic estimation of the top


event
Table No. 38 - List of symbols used in Fault Tree Analysis

SYMBOL NAME DESCRIPTION


Top event; Secondary or Contributing events; A
Rectangle
system
state requiring more investigation on lower levels
Circle
Basic fault event; no further development required

House Not a fault event; an event that is expected to occur


under normal operation

Diamond Undeveloped event; one that, by either choice or


necessity, will not be developed further

Oval An event that places qualified conditions on the


fault sequence
AND Describes an operation where all input events must
GATE occur for the operation to occur
Describes an operation where one or more of the
OR GATE
input events can occur for the output to occur
Used to show logic flow between two parts of the fault
F Transfer
GATE tree;
Transfers everything under the event it is attached to;

134
Reference is made by an alphanumeric code

8.2.1 Fault Tree Analysis of Packed bed reactor:


FAILURE OF
PBR

Fig. 28 – Fault Tree Analysis of Packed bed reactor

135
8.2.2 Fault tree analysis of Shell and Tube Heat Exchanger:

Reduced/Increased
process fluid
temperature

Fig. 29 – Fault Tree Analysis of Shell and Tube Heat Exchanger

136
8.2.3 Fault tree analysis of Storage tank:

Fig. 30 – Fault Tree Analysis of Storage Tank

137
8.2.4 Fault Tree analysis of Centrifugal pump:

Low pump outlet


throughput

Fig. 31 – Fault Tree Analysis of Centrifugal Pump

138
8.2.5 Fault tree analysis of Distillation Column:
Undesired purity of the
desired product

Fig. 32 – Fault Tree Analysis of Distillation Column

139
CHAPTER 9
PROCESS SIMULATION

140
9. Process Simulation of Production of n-Butyl acrylate From Propene in
ASPEN PLUS V 12.O

In industry complicated problems are often not solved by hand for two reasons:
human error and time constraints. There are many different simulation programs
used in industry depending on the field, application, and desired simulation
products (entire process unit, one piece of equipment, etc.). When used to its full
capabilities, Aspen can be a very powerful tool for a Chemical Engineer in a
variety of fields including oil and gas production, refining, chemical processing,
environmental studies, and power generation to name a few.
Beginning a Simulation:
1. Start the Aspen program. It can be found in the start menu under:
Start/Programs/Chem E/Aspen Plus User Interface
2. Choose what type of simulation you would like to use. Enter the components
involved in the process.
3. Select the Appropriate model for the process. Here UNIFAC MODEL is chosen
4. Create the flowsheet for production of N-Butyl acrylate.
5. Provide all the necessary details to run each unit.
6. Stream Results will be available after each run.

Below the images of Stream results involved in Production N-Butyl Acrylate from
propene are attached.

141
Fig.33 – Components and selected model for the process

142
Fig.34 – Raw materials streams
143
Fig.35 – Heater (H1) stream Results
144
Fig.36 – Reactors 1 and 2 stream Results
145
Fig.37 – Absorber stream Results

146
Fig.38 –Distillation column stream Results

147
Fig.39 –Reactive Distillation column stream Results

148
CHAPTER 10
PLANT LAYOUT

149
10.1 INTRODUCTION:

The economic construction and efficient operation of a process unit will depend
on how well the plant and equipment specified on the process flowsheet is laid out.

Plant Layout Considerations:

The principal factors to be considered are:

1. Economic considerations: construction and operating costs.

2. The process requirements.

3. Convenience of operation

4. Convenience of maintenance.
5. Safety.

6. Future expansion.

10.2 EXPLANATION OF VARIOUS PLANT UNITS :

Processing Area:
Processing area are also known as plant area in the main part of the plant where
the actual production takes place. There are two ways of laying out the processing
area:

• Grouped Layout
• Flow line Layout

Grouped Layout:
Grouped layout places all similar pieces of equipment adjacent. This provides
for ease of operation adjacent. This provides for ease of operations and switching
from one unit to another. This is suitable for all plants.

Flow line layout:


Flow line layout uses the line system which locates all the equipment in the
order in which it occurs on the flow sheet. This minimizes the length of transfer line

150
and therefore reduces the energy needed to transport materials. This is used mainly
for small volume products.

Storage house:
The main storage areas should be placed between the loading and unloading
facilities and the process they serve. The amount of space required for storage is
determined from how much is to be stored and in which containers. In raw material
storage, liquids are stored in small containers or in a pile on the ground.

Laboratories:
Quality control laboratories are a necessary part of any plant must be included
in all cost estimates. Adequate space must be provided in them for performing all
tests and for clearing and storage laboratory sampling and testing containers.

Costs:
The cost of construction can be minimized 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.

Process requirement:
All the required equipment has to be placed properly within process. Even the
installation of the auxiliaries should be done in such a way that it will occupy the
least space.

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

Offices:
The location of this building should be arranged so as to minimize the time
spent by personnel in travelling between buildings. Administration offices in which
a relatively large number of people working should be located well from potentially
hazardous process.
Canteen:

151
Canteen should be spacious and large enough for the workers with good and
hygienic food.

Fire station:
Fire station should be located adjacent to the plant area, so that in case of fire
or emergency the service can be put into action.

Medical facilities:
Medical facilities should be provided with at least basic facilities giving first
aid to the injured worker. Provision must be made for the environmentally
acceptable disposal of effluent.

The layout of the plant can be made effective by

• Adopting the shortest run of connecting pipe between equipment and the
least amount of structural steel work and thereby reducing the cost
• Equipment that needs frequent operator attention should be located
convenient to control rooms.
• Locating the vessels that require frequent replacement of packing or
catalyst outside the building.
• Providing at least two escape routes for operators from each level in
process buildings.
Safety :
Blast walls may be needed to isolate potentially hazardous equipment, and
confine the effects of an explosion. At least two escape routes for operator must be
provided from each level in the process building.

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

Utilities :
The word utilities are now generally used for ancillary services needed in the
operation of a production process. These services will normally be supplied from a
central side facility and will include:

• Electricity
• Steam for process heating

152
• Cooling water
• Water for general use
• Inert gas supplies

153
GATE 3

ELECTRIC
SUBSTATION
DISPATCHING
UNIT PLANT EXPANSION AREA

PLANT UTILITIES

CANTEEN
VPPACKING UNIT
HEA

ABSORBER
T EX

NBA
EFFLUENT TANK
HEALTH
CENTRE TREATMENT

GATE 2
REACTO
RS
VREACTIVE VDISTILLATIO
BUTANO DISTILLATION N
GATE 4

R&D L TANK

PROPE
NE
ADMINISTRATIVE BLOCK CONTROL ROOM PLANT EXPANSION AREA TANK

PARKING AREA SECURITY 1 FIRE STATION

GARDEN AREA GARDEN AREA


154
GATE 1

Fig.40 – Plant Layout for n-Butyl Acrylate production


CHAPTER 11

MATERIAL SAFETY DATA SHEET-N BUTYL ACRYLATE

155
156
157
158
159
160
161
162
163
164
165
166
REFERENCES :

[1] Takashi Ohara,Takahisa Sato,Noboru Shimizu,Günter Prescher,Helmut


Schwind,Otto Weiberg,Klaus Marten,Helmut Greim,Timothy D. Shaffer,Partha
Nandi, ”Acrylic Acid and derivatives”, Ullmann’s Encyclopedia of Industrial
Chemistry, https://doi.org/10.1002/14356007.a01_161.pub4

[2] Butyl Acrylate Market Research Analysis(2015-2035), Chemanalyst,


(Accessed on March 2022, Butyl Acrylate Market Size, Share | Global Industry
Analysis Report, 2015- 2035 | ChemAnalyst)

[3] PubChem [Internet]. Bethesda (MD): National Library of Medicine (US),


National Center for Biotechnology Information; 2004-. PubChem Compound
Summary for CID 8846, Butyl acrylate; [cited 2022 Mar. 15]. Available from:
https://pubchem.ncbi.nlm.nih.gov/compound/Butyl-acrylate

[4] Pal, R., Sarkar, T., and Khasnobis, S., Arkivoc. 2012, vol. 2012, part (i), p.
570: https://doi.org/10.3998/ark.5550190.0013.114

[5] Xuezheng Liang; Shan Gao; Guozhen Gong; Youfei Wang; Jian-Guo Yang
(2008). Synthesis of a Novel Heterogeneous Strong Acid Catalyst from p-
Toluenesulfonic Acid (PTSA) and its Catalytic Activities. , 124(3-4), 352–356.
doi:10.1007/s10562-008-9474-9
[6] Simulation of the acrylic acid production process through catalytic oxidation
of gaseous propylene using ChemCAD ® simulator:
http://dx.doi.org/10.4067/S0718-33052019000100142
[7] Yunus A. Çengel, John M. Cimbala, Fluid Mechanics: Fundamentals And
Applications Fourth Edition In SI Units

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