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A

Project Report
On
Trazodone (Phase I)
And

Acotiamide HCl Trihydrate (Phase II)


Submitted in partial fulfillment towards the Bachelor’s
Degree in the field of Chemical Engineering
Prepared By
Tadiwala Baman Percy
Ch-066 ( I.D.No. 15CHUON049 )

Under the Guidance of


Dr. P.A. Joshi

Department of Chemical Engineering


Faculty of Technology, Dharmsinh Desai University
College Road, Nadiad – 387 001
April -2019
COMPANY TRAINING CERTIFICATE (PHASE -I)

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COMPANY TRAINING CERTIFICATE (PHASE -II)

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CERTIFICATE

This is to certify that Tadiwala Baman Percy (CH-066, I.D.


NO. 15CHUON049) has duly submitted his Project Report on
Trazodone and Acotiamide HCl Trihydrate as a partial
fulfillment towards Bachelor’s degree in Chemical Engineering
at Dharmsinh Desai University, Nadiad in the year 2019.

Dr. P.A. Joshi Dr. M.S. Rao


Professor, Professor & Head,
Dept. Of Chemical Engg., Dept. Of Chemical Engg.,
DDU, Nadiad. DDU, Nadiad.
DATE: DATE:

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DECLARATION

I, Tadiwala Baman Percy declare that, the project report on

Trazodone and Acotiamide HCl Trihydrate comprises my original work

towards the degree of Bachelor of Technology in Chemical Engineering

at Dharmsinh Desai University and is not copied from any published or

proprietary source. I further declare that this work is not submitted

elsewhere towards degree or diploma in any university or college. The

whole content of this project work is genuine and distinctive.

Tadiwala Baman Percy,


CH-066 (I.D. No. 15CHUON049),
Semester VIII,
Department of Chemical Engineering,
Faculty of Technology,
Dharmsinh Desai University, Nadiad.

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ACKNOWLEDGEMENT

I would like to express my sincere gratitude to my guide Dr. P.A.


Joshi for providing his invaluable guidance, comments, and suggestions
throughout the course of the project. I would also thank Dr. M.S. Rao,
Head of Chemical Engineering Department for providing motivation and
support throughout the course of the project. I would also express my
special gratitude and thanks to people in industry for giving me such
attention and time as well as for providing necessary information
regarding the project. I would also like to thank my parents for their
co-operation and encouragement which helped me in completion of this
project.
My thanks and appreciation also goes to my colleagues in
developing the project and people who have helped me throughout the
course

Tadiwala Baman Percy

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PREFACE

As a part of curriculum and in order to gain practical knowledge of


Chemical Engineering, I was supposed to undergo training in Industry. I
was also required to make a report for the same. I did my Phase I training
at Zydus Cadila Healthcare Ltd. and Phase II training at Lupin Limited.
The basic objective behind this project report is to get knowledge of real
life situation in work field and to gain experience from them.
In this report, I have included various concepts regarding material
balance, energy balance, equipment, cost estimation as well as covered
health, safety and environment.

Tadiwala Baman Percy

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PHASE I
TRAZODONE

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Table of Contents

LIST OF FIGURES......................................................................................................xii
LIST OF TABLES....................................................................................................... xii
ABBRIVATIONS....................................................................................................... xiv
NOMENCLATURE....................................................................................................xvi

CHAPTER 1 INTRODUCTION............................................................................... 1
1.1 History of Product ............................................................................................. 2
1.2 IUPAC Name..................................................................................................... 2
1.4 Capacity of Product............................................................................................ 3
1.5 Market Value of Product.................................................................................... 3
1.6 Details of Product...............................................................................................3
1.7 Technicial as well as Commercial Competitors................................................. 3
1.8 Applications........................................................................................................3
1.9 Physical as well as Chemical Properties of Trazodone......................................4
1.10 Material Safety Data Sheet (MSDS)................................................................ 5
1.11 Conclusion......................................................................................................20

CHAPTER 2 SELECTION OF PROCESS............................................................ 21


2.1 Raw Material Specification..............................................................................22
2.1.1 Raw Mateiral Supply...............................................................................22
2.1.2 Transportation..........................................................................................22
2.1.3 Cost of Raw Materials............................................................................. 22
2.2 Physical and Chemical Properties of Raw Materials...................................... 23
2.2.1 Properties of KSM-01.............................................................................23
2.2.2 Properties of KSM-02.............................................................................24
2.3 Detailed Process Description..........................................................................25
2.3.1 Process Block Diagram.........................................................................25
2.3.2 Process Description.............................................................................. 26
2.3.3 Process Flow Diagram..........................................................................27
2.4 Conclusion.....................................................................................................27

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CHAPTER 3 MATERIAL BALANCE...................................................................28
3.1 Introduction...................................................................................................... 29
3.2 Overall Material Balance..................................................................................29
3.2.1 Material Balance over first Stainless Steel Reactor(SSR) .....................31
3.3 Material Balance Across Each Equipment.......................................................35
3.3.1 Material Balance over Pressure Nutsch Filter(PNF)..............................35
3.3.2 Material Balance over second Stainless Steel Reactor(SSR)................. 37
3.3.3 Material Balance over Centrifuge(CF)................................................... 38
3.3.4 Material Balance over Vacuum Tray Dryer(VTD)................................ 39
3.4 Conclusion.......................................................................................................39

CHAPTER 4 ENERGY BALANCE........................................................................40


4.1 Introduction......................................................................................................41
4.2 Energy Balance Across Each Equipment........................................................42
4.2.1 Energy Balance Across First Reactor (SSR).......................................... 42
4.2.2 Energy Balance Across Second Reactor (SSR)......................................44
4.3 Conclusion.......................................................................................................46

CHAPTER 5 PLANT UTILITIES.......................................................................... 47


5.1 Introduction...................................................................................................... 48
5.2 Steam Supply....................................................................................................49
5.3 Steam Supply....................................................................................................49
5.4 Chilling Plant....................................................................................................50
5.5 Power Supply................................................................................................... 50
5.6 Cooling Towers................................................................................................ 50
5.7 Conclusion........................................................................................................51

CHAPTER 6 DESCRIPTION OF THE EQUIPMENT........................................ 52


6.1 Introduction...................................................................................................... 53
6.2 Stainless Steel Reactor..................................................................................... 53
6.3 Pressure Nutsche Filter.....................................................................................54
6.4 Centrifuge........................................................................................................54
6.5 Vacuum Tray Dryer..........................................................................................54
6.6 Conclusion........................................................................................................55

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CHAPTER 7 DESIGNING OF EQUIPMENTS.................................................... 56
7.1 Introduction...................................................................................................... 57
7.2 Design of Reactor ............................................................................................58
7.3 Mechanical Design of Pressure Vessel............................................................ 60
7.3.1 Nozzle Design.........................................................................................62
7.3.2 Agitator and Shaft Design...................................................................... 64
7.4 Pump Design..................................................................................................... 67
7.5 Storage Vessel Design.......................................................................................70
7.6 Conclusion.........................................................................................................71

CHAPTER 8 PUMPS AND VALVES.....................................................................72


8.1 Details of Pump................................................................................................ 73
8.2 Details of Valves.............................................................................................. 74
8.3 Control Valve................................................................................................... 75
8.4 Conclusion........................................................................................................76

CHAPTER 9 HEALTH, SAFETY AND ENVIRONMENT................................. 77


9.1 Introduction...................................................................................................... 78
9.2 Safety Measures Taken By Industry................................................................ 79
9.3 Safety Equipment............................................................................................. 81
9.4 Safety Related Equipment with their Location .............................................. 83
9.5 Environment..................................................................................................... 84
9.5.1 Treatment for Waste Water.................................................................... 85
9.5.2 Effluent Treatment Plant.........................................................................85
9.5.3 Source of Air and Usage.........................................................................87
9.5.4 Source of Air Pollution...........................................................................87
9.5.5 Control Measures taken for Air Pollution.............................................. 87
9.5.6 Solid Waste Generation.......................................................................... 87
9.6 Conclusion........................................................................................................88

CHAPTER 10 PLANT LAYOUT AND PLANT LOCATION.............................89


10.1 Introduction.................................................................................................... 90
10.1.1 Plant Layout..........................................................................................90

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10.1.2 Plant Location........................................................................................90
10.2 Principle of Plant Layout.................................................................................91
10.3 Factors for Plant Location............................................................................... 92
10.4 Drawing of Plant Layout................................................................................. 93
10.5 Conclusion.......................................................................................................94

CHAPTER 11 COST ESTIMATION..................................................................... 95


11.1 Introduction.................................................................................................... 96
11.2 Purchased Equipment Cost.............................................................................96
11.2.1 Based on MOC................................................................................... 96
11.3 Capital Cost................................................................................................. 100
11.3.1 Fixed Capital Investment (F.C.I)...................................................... 100
11.3.2 Working Capital Investment (W.C.I)............................................... 102
11.4 Manufacturing Cost.....................................................................................103
11.4.1 Fixed Charges................................................................................... 103
11.4.2 Direct Production Cost..................................................................... 103
11.4.3 General Expenses..............................................................................104
11.4.4 Total Production Cost....................................................................... 104
11.5 Profitability Analysis...................................................................................105
11.5.1 Yearly Production.............................................................................105
11.5.2 Gross Profit.......................................................................................105
11.5.3 Net Profit.......................................................................................... 105
11.5.4 Rate of Return...................................................................................105
11.5.5 Payback Period................................................................................. 106
11.6 Conclusion...................................................................................................106

CHAPTER 12 CONCLUSION.............................................................................. 107

CHAPTER 13 BIBLIOGRAPHY..........................................................................108

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LIST OF FIGURES

Figure Name Page


No. No.

1.1 Structure of Trazodone 2

2.1 Process Block Diagram of Trazodone 25

2.1 Process Flow Diagram of Trazodone 27

3.1 Block Diagram representing input and output stream in first 31


SSR

3.2 Block Diagram representing input and output stream of PNF 35

3.3 Block Diagram representing input and output stream in second 37


SSR

3.4 Block Diagram representing input and output stream in CF 38

8.1 Block Diagram of Control Valve 75

8.2 Schematic view Control System 75

10.1 Overall Plant Layout 93

LIST OF TABLES

Table Name Page


No. No.

1.1 Physical Properties of Trazodone 4

1.2 Exposure Limit 9


2.1 Cost of Raw Material 22

2.2 Properties of KSM01 23

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2.3 Properties of KSM02 24

3.1 Overview of Mass Balance over SSR-1 (X=100%) 32

3.2 Overview of Mass Balance over SSR-1 (X=100%) 34

3.3 Overview of Mass Balance over PNF 36

3.4 Overview of Material Balance over SSR-2 37

3.5 Overview of Material Balance over CF 38

3.6 Overview of Material Balance over VTD 39

4.1 Molar Heat Capacity 41

4.2 Heat of Formation 24

4.3 Specific Heat Capacity 44

5.1 Boiler Data 49

5.2 Cooling Tower Data 51

6.1 Detailed Description of SSR 53

6.2 Detailed Description of PNF 54

6.3 Detailed Description of CF 54

6.4 Detailed Description of VTD 54

7.1 Computed Values of Thickness 71

8.1 Detailing of Pump 73

8.2 Detailing of Valves 74

9.1 Types of Fire Extinguishers 84

11.1 Purchased Equipment Cost 100

11.2 Direct Cost Factor 100

11.3 Indirect Cost Factor 101

11.4 Direct Production Cost 103

11.5 General Expenses 104

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ABBRIVATIONS

MW Molecular Weight of Compound

BD Blank Diameter

O.D Outside Diameter

I.D Inside Diameter

SR Slenderness ratio

CAS Chemical Abstracts Service

NIOSH National Institute for Occupational Safety and Health

DEA Drug Enforcement Administration

SDS System Design Specification

ACGIH American Conference Of Governmental Industrial Hygienists

TLV Threshold Limit Value

STEL Short Term Exposure Limit

OSHA Occupational Safety and Health Administration

CFR Code of Federal Regulations

IDLH The term immediately dangerous to life or health

ADR American Depository Receipts

IMDG International Maritime Dangerous Goods

IUPAC International Union of Pure and Applied Chemistry

Kg Weight in Kilograms

mm Length in Millimeter

m Length in Meter

cm Length in Centimeter

J Energy in Joules

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cal Energy in Calories

K Temperature in Kelvin

W Power in Watts

L.M.T.D Logarithmic Mean Temperature Difference

H.T.C Heat Transfer Coefficient

TEMA Tubular Exchanger Manufacturers Association

SS Stainless Steel

MS Milled Steel

ETP Effluent Treatment Plant

Hp Horse Power

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NOMENCLATURE

ρ Density of Fluid, kg/m3

μ Viscosity of Fluid, g/cm.s

 Latent Heat of Vaporization, KJ/mol

τ Reaction Time, hr

m Mass Rate, kg/hr

M Mass of Solid, kg

V Volume of Liquid, lit or m3

v Velocity of Fluid, m/s

N Normality of Liquid, mole/lit

C Molar Concentration of Fluid, mole/lit

Cp Specific Heat Capacity of Fluid, KJ/kg.K

Q Amount of Heat, J

T Actual Temperature, ℃ or K

Tr Reduced Temperature, ℃ or K

Tc Critical Temperature, ℃ or K

H Heat of Formation, KJ/mol

Hr Heat of Reaction, KJ/mol

t Temperature Difference

A, β Constants for Vaporization Data

K Reaction Constant, (concentration)1-n time-1

X Conversion

-rA Rate of Reaction

P Pressure, KPa

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θ Space Time, hr

R Gas Constant, lit.atm/mol.K

D Diameter, m

H Height, m

f Allowable Stress, kg/cm2

J Joint Efficiency Factor

Rc Crown Radius, m

Rk Knuckle Radius, m

W Weight, kg

trs Actual Thickness, mm

td Thickness with Corrosion, mm

tf Design Thickness, mm

tn Nozzle Thickness, mm

Dc Diameter of Coil, mm

Dj Diameter of Jacket, mm

bw Width of Blade, mm

N Speed of impeller, rpm

σ Stress, kgf/cm2

E Modulus of Elasticity, kgf/cm2

Nre Reynolds Number

Np Power Number

P Power, hp

Τc Torque, kgf.m

Zp Section Modulus, cm3

Rb Radius of Blade, m

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M Bending Moment, kgf.m

I Moment of Inertia, cm4

δ Maximum Deflection, cm

Pb Bearing Pressure, N/mm2

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CHAPTER 1
INTRODUCTION

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1.1 History of Product

Trazodone was discovered in Italy in the 1960’s by Angelini Research Laboratories as


a second-generation antidepressant. It was developed according to mental pain
hypothesis, which was postulated from the studying patients and which proposes that
major depression is associated with a decreased pain threshold. In sharp contrast to
most antidepressants available at that time of its development, trazodone showed
minimal effects on muscarinic cholinergic receptors. Trazodone was patented and
marketed in many countries all over the world. It was approved by the Food and Drug
Association (FDA) in 1981 and was first non-tricyclic antidepressant approved by US
government.

1.2 IUPAC Name

2-[3-[4-(3-chlorophenyl) piperazin-1-yl] propyl]-[1,2,4] triazolo [4,3-a] pyridin-3-one

1.3 Structure

Figure 1.1 Structure of Trazodone

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1.4 Capacity of Product

 Total Capacity of Plant: 10 tons per annum.


 World wide capacity: 106 tons per annum.

1.5 Market Value of Product

 Lamotrigine(Product): 4000 rupees/kg

1.6 Details of Product

 Trazodone is one of the slight expensive chemical; and is organic compound that
contains one or more functional group of (-Cl).
 Trazodone as final product is a white powder having light smell.

1.7 Technicial as well as Commercial Competitors

 Sun Pharma Ltd.


 Cipla Ltd.
 Intas Pharma Ltd.
 Dagon Pharma Pvt. Ltd.

1.8 Applications

 It is used as an antidepressant.
 It is used for balancing certain natural chemical(serotonin) in brain.
 It may help to improve your mood, appetite, and energy level as well
as decrease anxiety and insomnia related to depression.

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1.9 Physical as well as Chemical Properties of Trazodone

Table 1.1 Physical and Chemical Properties of Trazodone

Chemical Formula C19H22ClN5O

Molecular Weight 371.87 g/mol

Appearance White powder

Physical State Solid

Odor Light

Density 1.39 g/cm3

Vapour Pressure 8.03*10-9 mmHg

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1.10 Material Safety Data Sheet (MSDS)

Section 1: Product Identification

Trade name: Trazodone Tablets


Chemical Name: 2-[3-[4-(3-chlorophenyl) piperazin-1-yl] propyl]-[1,2,4]
triazolo [4,3-a] pyridin-3-one
Chemical Class: Active Ingredient: Triazolopyridine
Therapeutic Class: Central Nervous System Stimulant
Relevant use of substance: Human Pharmaceutical
How it is Supplied: In form of Round White Tablets

Section 2: Hazard Identification

Product Description: This product consists of odorless, round, white tablets


(50and 100 mg), or trapezoid-shaped, white (150 mg)
Health Hazards: In the workplace, dusts from damaged tablets may cause
irritation of contaminated skin or eye. Non-therapeutic ingestion may be harmful. In
therapeutic use, the most common adverse effects reported include sleepiness,
dizziness, constipation,blurry vision. Use can aggravate manic conditions or suicidal
thoughts. May cause adverse central nervous, cardiovascular and neurological effects.
Non-specific allergic reactions have been reported. As a selective serotonin reuptake
inhibitor, this material may cause harm to the fetus. These effects may be possible as
a result of workplace exposure
Flammability Hazards: This product is combustible and can ignite if highly heated
or if exposed to direct flame. When involved in a fire, this material may decompose
and produce irritating vapors and toxic compounds (including carbon and nitrogen
oxides and hydrogen chloride).
Reactivity Hazards: This product is not reactive.
Environmental Hazards: May cause harm to aquatic organisms if accidentally
released. All environmental release should be avoided.
Emergency Recommendations: Emergency responders must wear personal
protective equipment suitable for the situation to which they are responding

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Section 3: First Aid Measures

Skin Exposure: No specific effect is expected from skin contact. If this product
contaminates the skin and adverse effect occurs, begin decontamination with running
water. The contaminated individual must seek medical attention if any adverse effects
occur after flushing.
Eye Contact: Hold eyelids apart and flush eyes with plenty of water for at least 15
minutes. Have eyes examined and tested by medical personnel.
Inhalation: Supply Fresh air. If person is not breathing, give artificial respiration or
give oxygen by trained personnel. Get immediate medical attention.
Ingestion Wash out mouth with water provided person is conscious. Never give
anything by month to an unconscious person. Get medical attention. Do NOT induce
vomiting unless direction to do so by medical personnel.

Section 4: Fire Fighting Measures

Flammability of the Product: Not available


Flash Points: Not applicable
Auto-ignition Temperature: Not applicable
Flammable Limits: Not applicable
Exposure Hazard: Not applicable
Fire-Fighting and Instructions: Use alcohol-resistant foam, carbon dioxide, water,
or dry chemical spray. Use water spray to cool fire-exposed containers. As in any fire,
wear self-contained breathing apparatus pressure-demand (NIOSH approved or
equivalent), and full protective gear to prevent contact with skin and eyes.

Section 5: Accidental release measures

Personal, Precautions, Protective Equipment and Emergency Procedures: Spill


kits, clearly labeled, should be kept in or near preparation and administrative areas. It
is suggested that kits include a respirator, chemical splash goggles, two pairs of
gloves, two sheets (12” x 12”) of absorbent material, 250-mL and 1-liter spill control
pillows, a small scoop to collect glass fragments (if applicable) and two large waste

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disposal bags. Absorbents should be able to be incinerated. Avoid generating airborne
dusts of this material during spill response procedures as described below.
Protective Equipment: Small Spills/Spills in Hoods: Personnel wearing nitrile or
other appropriate gloves, labcoat or other protective clothing and eye protection
should immediately clean incidental spills (e.g. a single container). Large Spills: For
large spills (e.g., a pallet of containers), proper protective equipment, including
double nitrile or appropriate gloves, and protective clothing (i.e., disposable Tyvek
coveralls). When there is any danger of airborne dusts being generated, use a fullface
respirator equipped with a High Efficiency Particulate (HEPA) filter. Self-Contained
Breathing Apparatus (SCBA) can be used instead of an air-purifying respirator.
Methods for cleanup and contaminants: Cleanup of Small Spills: Pick-up or
wipe-up spilled tablets with damp absorbent sheets to prevent generation of dusts.
Decontaminate the spill area (three times) using a bleach and detergent solution and
then rinse with clean water. Large Spills: Restrict access to the spill areas. Gently wet
down area and carefully sweep up spilled product, avoiding the generation of airborne
dusts. The dispersion of particles into surrounding air and the possibility of inhalation
is a serious matter and should be treated as such. Do not apply chemical in-activators
as they may produce hazardous by-products. Thoroughly clean all contaminated
surfaces three times using a bleach and detergent solution and then rinse with clean
water. All Spills: Use procedures described above and then place all spill residues in
an appropriate, labeled container and seal. Move to a secure area. Dispose of in
accordance with Federal, State, and local hazardous waste disposal regulations (see
Section 13, Disposal Considerations). For spills on water, contain, minimize
dispersion and collect. Dispose of recovered material and report spill per regulatory
requirements. Disposal of this product has requirements under DEA regulations as a
narcotic substance.
Environmental Precautions: Prevent material from entering sewer or confined
spaces, waterways, soil or public waters. Do not flush to sewer. For spills on water,
contain, minimize dispersion and collect.

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Section 6: Handling and Storage

Precaution for safe handling: All employees who handle this material should be
thoroughly trained to handle it safely. As with all chemicals, avoid getting this
material ON YOU or IN YOU. Do not eat or drink while handling this material. After
handling this material, wash face and hands thoroughly prior to eating, drinking,
smoking or applying cosmetics. Ensure this material is used with adequate ventilation.
Appropriate personal protective equipment must be worn (see Section 8, Exposure
Controls - Personal Protection). Open containers slowly on a stable surface in areas
that have been designated for use of this material. Minimize all exposures to this
material. Avoid generation of dusts. Areas in which this material is used should be
wiped down, so that this material does not accumulate.
Condition for safe storage: Containers of this material must be properly labeled.
Store containers in a cool, dry location, away from direct sunlight and sources of
intense heat. Recommended Storage Temperature: 20-25°C (68-77°F). Store away
from incompatible materials (see Section 10, Stability and Reactivity). Material
should be stored in secondary containers. Keep containers tightly closed when not in
use. Inspect all incoming containers before storage, to ensure containers are properly
labeled and not damaged. Have appropriate extinguishing equipment in the storage
area (e.g., sprinkler system, portable fire extinguishers). Empty containers may
contain residual material; therefore, empty containers should be handled with care and
disposed of properly.
Specific end use(s): This product is a human pharmaceutical.
Protective practices during maintenance of contaminated equipment: When
cleaning nondisposable equipment, wear nitrile or other appropriate gloves (double
gloving is recommended), goggles, and lab coat. Prevent dispersion of particulates by
wetting or dampening surfaces prior to clean up of equipment. If applicable, wash
equipment using a bleach and detergent solution and then rinse with clean water.

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Section 7: Exposure Control - Personal Protection

Ventilation and Engineering Control: General: Use with adequate ventilation.


Follow standard operating procedures and requirements for handling this product.
Ensure eyewash stations and deluge showers are available and accessible in areas
where this product is used. Wear appropriate personal protect equipment consistent
with the recommendations of this SDS. Prevent accumulation of product on work
surfaces by routinely cleaning areas appropriately.

Workplace exposure Limits:

Table 1.2 Exposure Limits

Chemical CAS Exposure Limit


Name No.

ACGIH-TLVs OSHA-PELs NIOSH-RELs NIOSH OTHER

mg/m3 mg/m3
TWA STEL TWA STEL TWA STEL IDLH
mg/m3 mg/m3 mg/m mg/m3 mg/m3 mg/m3 mg/m3 mg/m3
3

Trazodone 25332- NE NE NE NE NE NE NE Cadila


39-2 OEL
Range
µg/m3 ≥
100 - <
3000
Colloidal 112945 NE NE NE NE NE NE NE NE
Silicon -52-5
Dioxide

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Lactose 63-42- NE NE NE NE NE NE NE NE
Anhydrous 3
Magnesium 557-04 10 NE NE NE NE NE NE Carcinog
Stearate -0 en:
Exposure TLV-A4
limits are
for
Stearates
Microcryst 9004-3 10 NE 15 NE 15 NE NE NE
alline 4-6 (total (total
Cellulose dust), dust), 5
Exposure 5 (resp.
limits are (resp. fractio
for fractio n)
cellulose n)
Sodium 9063-3 NE NE NE NE NE NE NE Carcinog
Starch 8-1 en:
Glycolate IARC-3
(*NE=Not Established)

Protective Equipment: The following information on appropriate Personal


Protective Equipment is provided to assist employers in complying with OSHA
regulations found in 29 CFR Subpart I (beginning at 1910.132, including U.S. Federal
OSHA Respiratory Protection (29 CFR 1910.134), OSHA Eye Protection 29 CFR
1910.133, OSHA Hand Protection 29 CFR 1910.138, OSHA Foot Protection 29 CFR
1910.136 and OSHA Body Protection 29 CFR1910.132), equivalent standards of
Canada (including CSA Respiratory Standard Z94.4-02, Z94.3-M1982, Industrial Eye
and Face Protectors and CSA Standard Z195-02, Protective Footwear), or standards
of EU member states (including EN 529:2005 for respiratory PPE, CEN/TR
15419:2006 for hand protection, and CR 13464:1999 for face/eye protection).
Respiratory Protection: Maintain airborne contaminant concentrations below
exposure limits listed above, if applicable. For materials without listed exposure limits,
minimize respiratory exposure. If necessary, use only respiratory protection

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authorized under appropriate regulations. Oxygen levels below 19.5% are considered
IDLH by U.S. OSHA. In such atmospheres, use of a full-facepiece pressure/demand
SCBA or a full facepiece, supplied air respirator with auxiliary self-contained air
supply is required under U.S. OSHA’s Respiratory Protection Standard
(1910.134-1998).
Eye Protection: Wear splash goggles or safety glasses as appropriate for the task. If
necessary, refer to appropriate regulations.
Hand Protection: Wash hands and wrists before putting on and after removing
gloves. During manufacture or other similar industrial operations, wear the
appropriate hand protection for the process. When used in medical administration of
the product, double glove with nitrile or other appropriate gloves to avoid contact
and/or absorption of the product. Use double gloves for spill response, as stated in
Section 5 (Accidental Release Measures) of this SDS. Because all gloves are to some
extent permeable and their permeability increases with time, they should be changed
regularly (hourly is preferable) or immediately if torn or punctured. If necessary refer
to appropriate regulations.
Skin Protection: Use appropriate protective clothing for the task (e.g., lab coat, etc.).
If necessary, refer to the U.S. OSHA Technical Manual (Section VII: Personal
Protective Equipment) or other appropriate regulations.

Section 8: Physical and Chemical Properties

Physical Form: Round or trapezoid tablets.


Odor: Practically odorless
Odor Threshold: Not applicable
Solubility in Water: Not available.
Molecular weight: 371.869
Molecular Formula: C19H22ClN5O
Boiling Point at 760 mmHg: 528.5°C (983.3°F) [est.]
Melting Point: 223-226°C (433.4-438.8°F)
Specific Gravity (water = 1): Not available
pH: Not available.
Decomposition Temperature: Not available

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Other Solubility: Not available
Vapor Pressure (air = 1) at 25°C: 2.94E-11 mmHg [predict.]
Evaporation Rate (nBuAc = 1): Not applicable
Flash Point: 273.4°C (524.1°F) [est.]
Solubility in Water at 25°C: Freely soluble.
Coefficient Water/Oil Distribution: Log P(oct) = 1.661 (est)

Section 9: Stability and Reactivity

Chemical Stability: Stable under normal conditions.


Decomposition Products: Combustion: Products of thermal decomposition may
include carbon and nitrogen oxides and hydrogen chloride.
Hydrolysis: None known.
Materials with which substance us incompatible: Incompatible with strong
oxidizing agents.
Possibility of Hazard Reaction/Polymerization: Will not occur.
Conditions to Avoid: Exposure to or contact with extreme temperatures,
incompatible chemicals

Section 10: Toxicological Information

Symptoms of Exposure by route of exposure: The main route of occupational


exposure to this product is via inhalation of dusts and skin contact. The anticipated
symptoms of exposure, by route of exposure are described further in this section
Inhalation: Inhalation of airborne dusts generated by damaged tablets of this product
may slightly irritate the nose, throat, and lungs. In addition, inhalation may result in
adverse effects as described under ‘Other Potential Health Effects’.
Contact with skin or eyes: It is anticipated that this product may irritate
contaminated skin or eyes. Symptoms of skin contact may include itching and redness.
Symptoms of eye contact can include redness, pain, and watering (mechanical
irritation).
Skin Absorption: No information is available.

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Ingestion: Ingestion of this product (i.e., through poor hygiene practices) may be
harmful. Effects may occur as described under ‘Other Potential Health Effects’.
Injection: Not a potential route of exposure for tablets
Other Potential Health Effects: In therapeutic use, the most common adverse effects
include sleepiness, dizziness, constipation, blurry vision. Use can aggravate manic
conditions or suicidal thoughts. May cause adverse central nervous, cardiovascular
and neurological effects. Non-specific allergic reactions have been reported. As a
selective serotonin reuptake inhibitor, this material may cause harm to the fetus.
These effects may be possible as a result of workplace exposure. The actual risk in the
workplace is not known. Body systems adversely affected during therapeutic use are
provided below. More details are given in the Cadila Active Ingredient SDS for this
product.

Health Effects or risk from Exposure:


Acute: Dusts from product may cause irritation if inhaled and in contact with skin or
eyes. Accidental ingestion may be harmful. Acute exposure may cause effects
described in “Other Potential Health Effects”.
Chronic: Chronic exposure may lead to symptoms described under ‘Other Potential
Health Effects’. May cause harm to fetus, based on animal test data. No chronic
effects have been reported from workplace exposure.

Target Organs: It is anticipated that for Occupational Exposure the target organs are:
Acute: Skin.
Chronic: Fetal harm. In therapeutic use this material may have an impact on the body
systems described under ‘Other Potential Health Effects’

Toxicity Data: The following toxicity data are currently available for the active
ingredient. Additional data are available for excipients, but are not provided in this
SDS.

13
Below is the toxicity data for Trazodone in various formulations:

TDLo (Oral-Woman) 100 mg/kg: Behavioral: sleep, somnolence (general depressed


activity); Vascular: BP elevation not characterized in autonomic section
TDLo (Oral-Woman) 750 µg/kg: Behavioral: hallucinations, distorted perceptions
TDLo (Oral-Woman) 720 mg/kg/34 weeks-intermittent: Liver: hepatitis
(hepatocellular necrosis), zonal, other changes; Kidney/Ureter/Bladder: other changes
in urine composition
TDLo (Oral-Woman) 80 mg/kg: Behavioral: somnolence (general depressed activity);
Vascular: BP lowering not characterized in autonomic section; Lungs, Thorax, or
Respiration: respiratory depression
TDLo (Oral-Woman) 0.03 gm/kg: Behavioral: somnolence (general depressed
activity); Cardiac: arrhythmias (including changes in conduction); Gastrointestinal:
nausea or vomiting
TDLo (Oral-Man) 5714 µg/kg/4 days-intermittent: Behavioral: euphoria, excitement
TDLo (Oral-Man) 43 mg/kg/30 days-intermittent: Blood: agranulocytosis, other
changes
TDLo (Oral-Man) 46 mg/kg/8 days-intermittent: Behavioral: excitement; Cardiac:
pulse rate increase, without fall in BP; Kidney/Ureter/Bladder: urine volume
increased
TDLo (Oral-Man) 667 µg/kg: Cardiac: cardiomyopathy including infarction
TDLo (Oral-Man) 159 mg/kg: male 7 week(s) pre-mating: Reproductive: Paternal
Effects: impotence
TDLo (Oral-Man) 112 mg/kg: male 6 week(s) pre-mating: Reproductive: Paternal
Effects: other effects on male
TDLo (Oral-Man) 667 µg/kg: male 1 day(s) pre-mating: Reproductive: Paternal
Effects: other effects on male LD50 (Oral-Rat) 690 mg/kg: Behavioral: convulsions
or effect on seizure threshold; Lungs, Thorax, or Respiration: cyanosis;
Gastrointestinal: changes in structure or function of salivary glands LD50
(Oral-Mouse) 584 mg/kg
LD50 (Oral-Dog) 500 mg/kg: Behavioral: altered sleep time (including change in
righting reflex), convulsions or effect on seizure threshold, aggression

14
LD50 (Oral-Rabbit) 560 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary glands
LD50 (Intraperitoneal-Rat) 178 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary glands
LD50 (Intraperitoneal-Mouse) 255 mg/kg
LD50 (Intravenous-Rat) 91 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary glands
LD50 (Intravenous-Mouse) 91 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary LD50 (Intravenous-Dog) > 40 mg/kg
LD50 (Intravenous-Monkey) 25 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary glands
LD50 (Intravenous-Rabbit) 52 mg/kg: Behavioral: convulsions or effect on seizure
threshold; Lungs, Thorax, or Respiration: cyanosis; Gastrointestinal: changes in
structure or function of salivary glands
LD50 (Subcutaneous-Rat) 2729 mg/kg
LD50 (Subcutaneous-Mouse) > 1500 mg/kg
TDLo (Oral-Rat) 3300 mg/kg: female 7-17 day(s) after conception: Reproductive:
Effects on Embryo or Fetus: fetotoxicity (except death, e.g., stunted fetus), fetal death;
Specific Developmental Abnormalities: musculoskeletal system
TDLo (Oral-Rat) 750 mg/kg: female 7-20 day(s) after conception lactating female 21
day(s) post-birth: Reproductive: Effects on Newborn: growth statistics (e.g.%,
reduced weight gain)
TDLo (Oral-Rat) 1100 mg/kg: female 7-17 day(s) after conception: Reproductive:
Effects on Newborn: physical
TDLo (Oral-Mouse) 66175 mg/kg/78 weeks-continuous: Endocrine: changes in
adrenal weight, changes in thyroid weight; Related to Chronic Data: changes in
testicular weight

15
TDLo (Oral-Dog) 2730 mg/kg/13 weeks-intermittent: Blood: changes in serum
composition (e.g. TP, bilirubin, cholesterol); Biochemical: Enzyme inhibition,
induction, or change in blood or tissue levels: phosphatases
TDLo (Intraperitoneal-Rat) 3 mg/kg: Behavioral: changes in psychophysiological
tests
TDLo (Intraperitoneal-Rat) 5 mg/kg: Reproductive: Paternal Effects: other effects on
male
TDLo (Intraperitoneal-Rat) 10 mg/kg: Behavioral: somnolence (general depressed
activity); Reproductive: Paternal Effects: other effects on male
TDLo (Intraperitoneal-Rat) 30 mg/kg: Behavioral: somnolence (general depressed
activity), rigidity (including catalepsy); Reproductive: Paternal Effects: other effects
on male

Irritably of Product: Inhalation of dusts from this product may be irritating to the
respiratory system. Dusts will also be irritating to the eyes.
Sensation to product: Use of this product has been reported to cause rash and other
non-specified allergic reactions.
Reproductive Toxicology Information: There are no adequate and well-controlled
studies of Trazodone in pregnant women; however, Trazodone may cause fetal harm
when administered to a pregnant woman. In the workplace, the risk to the fetus should
be communicated and the appropriate action should be taken to prevent exposure in
accordance with company policy and regulatory requirements. This product is rated
by the FDA for therapeutic risk as Pregnancy Risk Category C (refer to Definition of
Terms for full category definitions).
Mutagenicity: Adequate studies have not been performed in animals to determine
whether Fludrocortisone Acetate has mutagenic activity.
Embryotoxicity/Teratogenicity: Trazodone has been shown to cause increased fetal
resorption and other adverse effects on the fetus in two studies using the rat when
given at dose levels approximately 30 to 50 times the proposed maximum human dose.
There was also an increase in congenital anomalies in one of three rabbit studies at
approximately 15 to 50 times the maximum human dose.
Reproductive Toxicity: Adequate studies have not been performed in animals to
determine whether Trazodone affects fertility in males or females. Priapism has been
reported with all SSRIs. Trazodone and/or its metabolites have been found in the milk

16
of lactating rats, suggesting that the drug may be secreted in human milk. Because of
the potential for serious adverse reactions in nursing infants, nursing mothers should
be advised of these effects and the appropriate action should be taken to prevent
exposure.
Biological Exposure Indices: Currently, there are no Biological Exposure Indices
(BEIs) determined for the components of this product.

Section 11: Ecological Information

Mobility: This product has not been tested for mobility in soils. No predicted values
are available.
Persistence and biodegradability of product: This product has not been tested for
persistence and biodegradability. No predicted values are available.
Bio-accumulation and biodegradability: This product has not been tested for
bio-accumulation potential.
Ecotoxicity: This product may be harmful or fatal to contaminated plant and
animal-life (especially if large quantities are released). This product has not been
tested for aquatic toxicity. No aquatic toxicity data are available for components of
this product.
Other Adverse Effects: The components of this product are not listed as having
ozone depletion potential.
Environmental Exposure Control: Controls should be engineered to prevent release
to the environment, including procedures to prevent spills, atmospheric release and
release to waterway

Section 12: Disposal Considerations

Waste Treatment/Disposal Methods: Waste disposal must be in accordance with


appropriate Federal, State, and local regulations. This product, if unaltered by use,
may be disposed of by treatment at a permitted facility or as advised by your local
hazardous waste regulatory authority. All protective clothing, gloves, and disposable
materials used in the preparation or handling of this drug should be disposed of in
accordance with established hazardous waste disposal procedures. It is the

17
responsibility of the generator to determine at the time of disposal whether the
product meets the criteria of a hazardous waste per regulations of the area in which
the waste is generated and/or disposed. Incineration is recommended for the product
and disposable equipment. Shipment of wastes must be done with appropriately
permitted and registered transporters. Reusable equipment should be cleaned with
soap and water and thoroughly rinsed.
Disposal Containers: Waste materials must be placed in and shipped in appropriate
5-gallon or 55-gallon poly or metal waste pails or drums. Permeable cardboard
containers are not appropriate and should not be used. Ensure that any required
marking or labeling of the containers be done to all applicable regulations.
Precautions to be followed while waste handling: Wear proper protective
equipment when handling waste materials.

Section 13: Transport Information

UN number

ADR/RID: 3077 IMDG: 3077 IATA: 3077

UN proper shipping number

ADR/RID: ENVIRONMENTALLY HAZARDOUS SUBSTANCE, SOLID, N.O.S


(Trazodone)
IMDG: ENVIRONMENTALLY HAZARDOUS SUBSTANCE, SOLID, N.O.S
(Trazodone)
IATA:Environmentally hazardous subtsance, solid, n.o.s (Trazodone)

Transport Hazard Classes

ADR/RID: 9 IMDG: 9 IATA: 9

18
Packaging group

ADR/RID: III IMDG: III IATA: III

Environmental Hazards

ADR/RID: yes IMDG: no IATA: yes

Section 15: Regulatory Information

Safety, Health, and Environmental regulations/legislation specific for the


substance or mixture: This datasheet complies with the requirement of Regulation
(EC) No. 1272/2008

Chemical safety assessment: For this product a chemical safety assessment was not
carried out.

Section 16: Other Information

WINGESTION MAY BE HARMFUL. MAY CAUSE HARM TO FETUS DURING


PREGNANCY, BASED ON ANIMAL DATA. COMBUSTIBLE IF EXPOSED TO
HIGH TEMPERATURES. Do not taste or swallow. Avoid contact with skin, eyes,
and clothing. Keep container closed. Use gloves, safety glasses, and appropriate
respiratory and body protection.
First Aid: If exposed, seek immediate medical attention. If swallowed, do not
induce vomiting. If alert, give victim up to three glasses of water. Never give
anything by mouth to an unconscious person. In case of contact, immediately flush
skin with copious amounts of warm water for 20 minutes. Remove contaminated
clothing and shoes. If inhaled, remove to fresh air. If not breathing, give artificial
respiration. If breathing is difficult, give oxygen.
In case of fire: Use water fog, dry chemical or CO2, or alcohol foam. IN CASE OF
SPILL: Refer to Safety Data Sheet for complete spill response procedures. Spill
response should be performed by persons properly trained to do so. Decontaminate

19
area with bleach and detergent solution and triple rinse area. Place spill debris in a
suitable container. Refer to SDS for additional information.
GLOBAL HARMONIZATION AND EU CLP REGULATION (EC) 1272/2008
LABELING AND CLASSIFICATION: According to Article 1, item 5 (a) of CLP
Regulation (EC) 1272/2008, medicinal products in the finished state for human use, as
defined in 2001/83/EC, are excepted from classification and other criteria of
1272/2008.
67/548/EEC EU LABELING/CLASSIFICATION: According to Article 1 of
European Union Council Directive 92/32/EEC, medical products in the finished state
for human use (as defined by European Union Council Directives 67/548/EEC and
87/21/EEC) are not subject to the regulations and administrative provisions of
European Union Council Directive 92/32/EEC.

1.11 Conclusion

This introductory chapter gives a general overview of the product. We got the
information about the history of the product, the IUPAC name, and the structure of
the compound. Alongside, we also discussed the names of Technical and Commercial
competitors and various properties of the product. In the end, we got to know about
the MSDS of the product.

20
CHAPTER 2
SELECTION OF PROCESS

21
2.1 Raw Material Specification

2.1.1 Raw Mateiral Supply

 Raw material comes from Ami Organics Ltd. and Sukhram Pvt. Ltd.

2.1.2 Transportation

 Company is situated in an area where good number of industries are available, so


raw material transportation is easily done through national highway 8 joining
Dabhasa to Vadodara via Padra. Vadodara being the main city is just 30 km from
Dabhasa making the transportation more convenient.

2.1.3 Cost of Raw Materials

Table 2.1 Cost of Raw Materials

Sr. No. Name of Raw Material Cost per kg

KSM-01
1 Rs. 1000
1-(3-chlorophenyl)-4-(3-chloropropyl)piperazine
hydrochloride

KSM-02
2 Rs. 1500
(1,2,4) triazolo [4,3-a] pyridine 3 (2H) one

22
2.2 Physical and Chemical Properties of Raw Materials

2.2.1 Properties of KSM-01

Table 2.2 Properties of KSM-01

Chemical Formula C13H19Cl3N2

Molecular Weight 309.66 g/mol

Appearance White Powder

Odor Irritating

Physical State Solid

Melting Point 130-133 ℃

Density NA

Specific Heat NA

Reactivity NA

Solubility NA

Freezing Point NA

23
2.2.2 Properties of KSM-02

Table 2.3 Properties of KSM-02

Chemical Formula C6H5N3O

Molecular Weight 135.13 g/mol

Appearance White Powder

Odor Light

Physical State Solid

Auto Ignition Temperature NA

Flash Point NA

Instability NA

Melting Point 125 ℃

Reactivity NA

24
2.3 Detailed Process Description

2.3.1 Process Block Diagram


IPA

SSR KSM-01, KSM-02, Sodium Carbonate

Pressure
Nutsche Filter
NaCl

SSR

Centrifuge
mL

Vacuum Tray Dryer Trazodone

Figure 2.1 Process Block Diagram of Trazodone

25
2.3.2 Process Description

First we ensure that the reactor is cleaned, dried and ready to be used. Then we charge
900 L of IPA in the reactor. After charging IPA; KSM-01, KSM-02 and Sodium
Carbonate are further added to the reactor. KSM-01 and KSM-02 are in solid state,
and IPA is added to dissolve the two chemicals for initiating the reaction. Thus,
condensation reaction takes place and as a products, Trazodone and HCl are formed.

The HCl further reacts with Sodium Carbonate and NaCl. This reaction yields Water
and CO2. The reaction is heated at 80℃ for about 12 hours. After heating, due to the
reaction between raw materials, undesired NaCl is formed. This NaCl is removed by
passing the reacted mixture through Pressure Nutsche Filter. NaCl is insoluble in IPA,
hence it is filtered out.

The filtrate is then passed into another SSR. Here it is cooled between 0-5℃
temperature. At this temperature, Trazodone becomes insoluble in IPA and its
crystallization occurs. This cooled mixture is passed into a Centrifuge where the
remaining solvent and other constituents are removed in the form of mother liquor
and wet cake of Trazodone is obtained. The wet cake is sent into a vacuum dryer
where remaining moisture is removed and we obtain our final product, Trazodone,

26
2.3.3 Process Flow Diagram

Figure 2.2 Process Flow Diagram of Trazodone

2.4 Conclusion

This chapter gives detail about selection of process including the raw material
specification and the cost of the product.. We conclude that various physical and
chemical properties of raw material are distinctive. Also, the process block diagram,
process flow diagram and the process description of the product is noted.

27
CHAPTER 3
MATERIAL BALANCE

28
3.1 Introduction

Material flow rates for the various streams are determined based on desired plant
capacity using material balance calculation.

This chapter includes material balance of Reactor, Centrifuge separator and Vacuum
Tray Dryer. Material balance gives us an idea about the quantity of feed entering and
the product leaving along with unreacted material of particular equipment. It also
helps us to determine the composition in the feed and in the product which is
unreacted for given conversion.

For conversion, the quantity of reactant reacted is identified. The material balance is
governed by Law of Conservation of Mass, viz. Input - Output = Accumulation.

In our calculation, 64% of excess of original is taken for carrying our Material
Balance.

3.2 Overall Material Balance

Trazodone production seems a single step reaction, but however it takes place in two
steps as shown below.

(i) C13H19N2 + C6H5N3O → C19H22ClN5O + 2HCl

(ii) 2HCl + Na2CO3 → 2NaCl + H2O + CO2

Thus the overall Reaction is,


IPA
C13H19N2 + C6H5N3O + Na2CO3 → C19H22ClN5O + 2NaCl + H2O + CO2

C
A + B + D → E + 2G + H + I

29
Where,
A= KSM-01 (Raw Material); C13H19N2
B= KSM-02 (Raw Material); C6H5N3O
C= Isopropyl Alcohol (Raw Material); C3H8O
D= Sodium Carbonate (Raw Material); Na2CO3
E= Trazodone (Main Product); C19H22ClN5O
F= Hydrochloric acid (Intermediate); HCl
G= Sodium Chloride (By Product); NaCl
H= Water(By Product); H2O
I= Carbon dioxide; CO2

Since the data of the company is confidential, batch size is assumed.

Let, the batch size= 148 kg

ORIGINAL BASIS: Batch Capacity= 148 kg/batch

But,
Actual Capacity= Original Capacity*(1.Roll Number) kg/batch

⸫ Actual Capacity= 148*(1.66) kg/batch

⸫ Actual Capacity= 246 kg/batch

NEW BASIS: Batch Capacity= 246 kg/batch

Here, we also assume that conversion is 100%

30
3.2.1 Material Balance over first Stainless Steel Reactor(SSR)

KSM-01 → → Trazdone
→ HCl
KSM-02 → SSR → NaCl
→ H2O
Na2CO3 → → CO2

Figure 3.1 Block Diagram representing input and output stream in first SSR

(1) Moles of Trazodone to be produced= 246/371.869


= 0.66 kmol

(2) Kg of KSM-01 needed= M.W. of KSM-01*moles of Trazodone


= 309.66*0.66
= 204.3756 kg

(3) Kg of KSM-02 needed= M.W. of KSM-02*moles of Trazodone


= 135.12*0.66
= 89.1792 kg

(4) Kg of HCl produced= 2*36.46*0.66


= 48.1272 kg

(5) To neutralize 48.1272 kg of HCl


Moles of HCl= 48.1272/36.46
= 1.32 moles
1.32= Na2CO3 needed/105.988
139.9 kg of Na2CO3 needed.

(6) Kg of NaCl produced= 1.32*58.4*2

31
= 100.6148 kg

(7) Kg of H2O produced= 1.32*18


= 28.76 kg

(8) Kg of CO2 produced= 44*1.32


= 58.08 kg

Summary Table

Table 3.1 Overview of Material Balance over SSR (X=100%)

CHEMICALS INLET (KG) OUTLET (KG)


A 204.3756 0
B 89.1792 0
C 900 L 900 L
D 139.9 0
E 0 246
F 0 0
G 0 100.6148
H 0 28.76
I 0 58.08
Total 433.4548 433.4548

32
Now, Let us assume that conversion is 90%

(1)1 mol of KSM-01= 0.90 mol of Trazodone


⸫ Mol of Trazodone produced for 90% conversion= 0.66/0.90
= 0.73 kmol

(2) Kg of KSM-01 needed= M.W. of KSM-01*moles of Trazodone


= 309.66*0.73
= 226.0518 kg

(3) Kg of KSM-02 needed= M.W. of KSM-02*moles of Trazodone


= 135.12*0.73
= 98.6376 kg

(4) Kg of HCl produced= 2*36.46*0.73


= 53.2316 kg

(5) To neutralize 53.2316 kg of HCl


Moles of HCl= 53.2316/36.46
= 1.46 moles
1.46= Na2CO3 needed/105.988
154.74248 kg of Na2CO3 needed.

(6) Kg of NaCl produced= 2*58.44*0.73


= 83.27294 kg

(7) Kg of H2O produced= 1.46*18.015


= 26.28 kg

(8) Kg of CO2 produced= 1.46*44


= 64.24 kg

(9) Unreacted KSM-01= 226.0518 - 203.44662 = 22.60518 kg

33
(10) Unreacted KSM-02 = 98.6376 - 88.77384 = 9.86376 kg

Summary

Table 3.2 Overview of Material Balance over SSR (X=90%)

CHEMICALS INLET (KG) OUTLET (KG)


A 226.0518 22.60518
B 98.6376 9.86376
C 900 L 900 L
D 154.74248 0
E 0 246
F 0 0
G 0 83.27294
H 0 26.28
I 0 64.24
Total 479.43188 479.43188

34
3.3 Material Balance Across Each Equipment

3.3.1 Material Balance over Pressure Nutsch Filter(PNF)

Slurry→ PNF → Salt


Mother Liquor

Figure 3.2 Block Diagram representing input and output stream of PNF

Here, Slurry contains Product, IPA, Sodium Carbonate, Salt, and Unreacted
Reactants.

So, if we are assuming 100% of separation over PNF, then salt which is formed
during the reaction will be totally removed and Mother Liquor will contain our
product, IPA, and unreacted reactants.. The Data is as shown in the table 3.3.

35
Summary Table
Table 3.3 Overview of Mass Balance over PNF

CHEMICALS INLET(KG) OUTLET(KG) OUTLET(KG)


SALT ML
A 22.60518 0 22.60518
B 9.86376 0 9.86376
C 900 L 0 900 L
D 0 0 0
E 246 0 246
G 83.27294 89.27294 0
H 26.28 26.28
TOTAL 388.02188 83.27294 304.74894

36
3.3.2 Material Balance over second Stainless Steel Reactor(SSR)

SSR
ML from→ → Crystals + ML
PNF

Figure 3.3 Block Diagram representing input and output stream in second SSR

Here only crystallization process takes place where Trazodone particles are
crystallized from IPA solution under cooling. Since, no chemical reaction takes place,
Input= Output is summarized in table 3.4.

Summary

Table 3.4 Overview of Material Balance over SSR-2

CHEMICALS INLET(KG) OUTLET(KG)


A 22.60518 22.60518
B 9.86376 9.86376
C 900 L 900 L
E 246 246
H 26.28 26.28
TOTAL 304.74894 304.74894

37
3.3.3 Material Balance over Centrifuge(CF)

Slurry→ CF →Wet Cake(Product)


IPA + Unreacted Reactant(ML)

Figure 3.4 Block Diagram representing input and output stream in CF

In CF, ML is separated from solid wet cake. Here, the unreacted reactants are
dissolved in IPA and that IPA containing ML is separated out. Some part of IPA
going into the Trazodone is known as wet cake.
The final Trazodone wet cake which is coming out from CF will contain about 2% of
IPA part which is sent to VTD for drying.

Summary

Table 3.5 Overview of Material Balance over CF

CHEMICALS INLET(KG) OUTLET(KG) OUTLET(KG)


WET CAKE ML
A 22.60518 0 22.60518
B 9.86376 0 9.86376
C 707 14.14 692.86
E 246 246 0
TOTAL 985.46894 260.14 752.32894

38
3.3.4 Material Balance over Vacuum Tray Dryer(VTD)

Moisture

Wet Product → VTD → Trazodone


From CF

Figure 3.5 Block Diagram representing input and output stream in VTD

The wet product contains 2% moisture and remaining is pure solid product.
Solid in wet solid=Solid in product.
Moisture in final product= NMT 0.5%
So, in final product moisture content=(246*0.5)/100=1.23 kg
IPA removed with use of VTD=14.14-1.23=12.91 kg

Summary

Table 3.6 Overview of Material Balance over VTD


CHEMICAL INLET(KG) OUTLET(KG) MOISTURE(KG)
E 246 246 0
Moisture 14.14 1.23 12.91
TOTAL 260.14 247.23 12.91

3.4 Conclusion

We conclude that the material balance is governed by Law of Conservation of Mass,


viz. Input - Output = Accumulation. The material balance of Reactor, Centrifuge
separator and Vacuum Tray Dryer was carried out which gave us information about
the quantity of feed entering and the product leaving along with unreacted material of
particular equipment.

39
CHAPTER 4
ENERGY BALANCE

40
4.1 Introduction

Energy Balance is done based on Heat of Reaction, Heat Capacities, Expected


Temperatures, and Pressure at various points to calculate amount of heating and
cooling needed at various places and to size equipments.
In this chapter, energy balance of Reactor at various stages and dryer is given. There
us one major conservation law which provides an additional equation called Law of
Conservation of Energy. E denotes the entire amount of energy in system.

Law of Conservation of Energy:


Ein - Eout = Eaccumulated

Kinetic Energy and Potential Energy are generally very small compared to the
enthalpy, except in case of very rapid flow or when there are no significant
temperature changes occurring in the system. Therefore, they are often neglected in
performing energy balances.
Here Cp values are found using Kopp’s Law and heat of formation is found using
group contribution method.

Table 4.1 Molar Heat Capacities

MATERIAL MOLAR HEAT CAPACITY (J/mol K)


KSM 01 409.9
KSM 02 187.7
Trazodone 526.4

41
4.2 Energy Balance Across Each Equipment

4.2.1 Energy Balance Across First Reactor (SSR)

∆T = 80℃ - 30℃ = 50 ℃

Heat in with feed,

QKSM 01 = mCp∆T
=0.73*409.9*50
=14961.35

QKSM 01 = mCp∆T
=0.73*187.7*50
=6851.05

Heat out with product,


QTrazodone = mCp∆T
=0.73*526.4*50
=19213.6

42
Table 4.2 Heat of Formation

MATERIAL HEAT OF FORMATION (KJ/mol)


KSM 01 -56.62
KSM 02 100.8
Trazodone -70.30
HCl -92.3

∆Hr = Reactant - Product


= (-56.62 + 100.8) - (-70.30 + (2*(-92.31)))
= 299.1 KJ/mol

Qsupply = Qin -Qout - ∆Hr


=14961.36 + 6851.05 - 19213.6 - 299.1
=2299.71 KJ/mol

Temperature of Hot Water in = 80℃


Temperature of Hot Water out = 40℃

Now,
Qsupply = mCp∆T
⸫ 2299.71 = m * 4.18 * 40
⸫ m = 13754.24 mol
⸫ Kg of Water = m * 18
= 13754.24 * 18
= 247.576 kg

Mass Flow = Kg of Water / Batch Time


= 247.576 / 12
= 20.63 kg/hr

43
4.2.2 Energy Balance Across Second Reactor (SSR)

In this reactor only crystallization process takes place. The temperature thus falls from
80℃ to 2.5℃.

Table 4.3 Specific Heat Capacity

MATERIAL SPECIFIC HEAT CAPACITY


(KJ/KgK)
KSM 01 1.32
KSM 02 1.39
Trazodone 1.41
IPA 2.68

Heat change with KSM 01,


QKSM 01 = MCp∆T
= 22.60518 * 1.32 * (80 - 2.5)
= 2312.509914 KJ

Heat change in KSM 02,


QKSM 02 = MCp∆T
= 9.86376 * 1.39 * 77.5
= 1062.573546 KJ

Heat change in IPA, (where density of IPA = 763 kg/m3)


Q IPA = MCp∆T
= 707 * 2.68 * 77.5
= 146843.9 KJ

Heat change in Trazodone,


QTrazodone = MCp∆T
= 246 * 1.41 * 77.5
= 26881.65 KJ

44
We have to reduce the total heat of KSM 01, KSM 02, and Trazodone.
So,
The total heat required to be reduced = QKSM 01 + QKSM 02 + QIPA + QTrazodone
= 2312.509914 + 1062.573546 + 146843.9
+ 26881.65
= 177100.6335 KJ

So to remove the above value of total heat, three stage cooling technique is implanted.

Firstly, cooling water is used to remove some amount of heat.


Assuming that temperature is initially brought to 15℃
QTotal Heat = MCp∆T
⸫ 177100.6335 = M * 4.18 * 15
⸫ M = 2824.57150 kg
So for reducing above mentioned temperature level, we require 2824.57150 kg of
cooling water.

For the second stage cooling, assuming that the temperature drop is around 10℃.
Chilled water is used for second stage cleaning.
QTotal Heat = MCp∆T
⸫ 177100.6335 = M * 4.18 * 10
⸫ M = 4236.857271 kg
So for reducing above mentioned temperature level, we require 4236.857271 kg of
chilled water.

For the third stage cooling, assuming that the temperature drop is around 2.5℃.
Brine solution is used for third stage cooling.
QTotal Heat = MCp∆T
⸫ 177100.6335 = M * 4.18 * 2.5
⸫ M = 20533.40678 kg
So for reducing above mentioned temperature level, we require 20533.40678 kg of
brine solution.

45
4.3 Conclusion

We conclude that the energy balance is governed by Law of Conservation of Energy:


Ein - Eout = Eaccumulated. Energy Balance was done based on Heat of Reaction, Heat
Capacities, Expected Temperatures, and Pressure at various points to calculate
amount of heating and cooling needed at various places and to size equipment.

46
CHAPTER 5
PLANT UTILITIES

47
5.1 Introduction

Just as any plant requires raw materials to produce the final product, it equally
requires various other services called Utilities for smoothly carrying out the processes.
Utilities are neither a product nor a reactant, but they are required for maintaining
adequate conditions of manufacturing unit. Thus, Utility area is an important section
of a plant which is house to various boilers, large compressors, cooling towers, water
treatment plants etc. Plant also requires electric power, so Power Plants are also
considered as a part of Utilities.
The bad management of of utilities can make even the most profitable processes
unprofitable. Utilities can be used to maintain processing parameters like pressure,
temperature, etc., without which it is impossible to carry out the process.

Some properties of Utilities are as follows:


 They are generally reusable.
 Their composition doesn’t change.
 They cannot be stocked, so regular supply is must.
 They must be readily available.

The following are the Utilities present in the plant:


 Steam
 Portable Water
 Power Supply
 Chilling Water
 Cooling Tower

48
5.2 Steam Supply

The steam us supplied to the plant from boiler house. This steam is used for heating
purpose and in drying. The boiler used here is Water Tube Boiler. The heating surface
of Water Tube Boiler is much more effective than equivalent area of surface in
ordinary Tubular Boiler and they generate steam at a much higher pressure. The
specification of the boiler used in the company is tabulated below:

Table 5.1 Boiler Data

Type of Boiler Water Tube Type


Heating Medium Coal
Capacity 12 ton/hr
Pressure 10-12 kgf/cm2
MOC of Shell Mild Steel
MOC of Tubes SS
Insulating Material (inner wall) Fire Bricks
Insulating Material (outer wall) Glass Wool

5.3 Steam Supply

Ordinary water cannot be directly used in the process or in the bolier as this may
cause scaling in the bolier and formation of undesirables during the reaction.
Therefore, it is necessary to make water free from hardness and purify it before use.

First of all, water is passed through cation exchange resins which are capable of
exchanging cations in water by hydrogen ions. Then the water is passed through anion
exchange resins which are capable of exchanging anion in water by hydraulic ion.

The resins are then washed with strong acid so that the pH of water is reduced (up to
7pH). It is then washed with alkali like NaOH. Now, this water is stored in an

49
intermediate storage tank. From here it is sent to sterilization unit for removing
pathogenic microorganisms and then finally sent to main storage tank.

5.4 Chilling Plant

This plant supplies water which is chilled up to 20℃to 15℃ for cooling of the reactor
after the use. The chilled water is sometimes required in the processing step of the
product, while it may also be used to cool down the reactor before the final cleaning.

The plant uses RA 404 refrigerant as a primary refrigerant and water as secondary
refrigerant. The capacity of the chiller is 20 TR(max). So this type of chillers are also
capable for brine plant where methanol-water solution is used instead of water.

Throttling device, evaporator, condenser, compressor are the major components of the
refrigeration unit. Here, RA 404 is passed through cooling coil which is surrounded
by water, thus leading to cooling of water up to desired temperature. But during this
heat transfer, RA 404 will take up the heat so it sent to heat exchanger where it is
cooled. The cooled refrigerant is sent to compressor and then through a throttling
device. This way whole cycle is repeated. The temperature of chilling water is around
22℃ which is good enough for the process. Before applying the chilling water to
reactor jacket, we should ensure that steam inlet valve is closed.

5.5 Power Supply

Power is needed everywhere in the plant, so there are three phase 15A supply. The
company also has backup power units in case of power failure. The approximate per
day consumption of power is around 50 KW to 100 KW.

5.6 Cooling Towers

Cooling Towers are used to cool the process hot water coming from the equipment
like heat exchangers and reactor jackets. The cooled water from the cool water basin

50
of the tower is again supplied for its reuse as cooling medium in heat exchangers and
reactor jackets.
The cooling towers used is induced type cooling tower which counter current fashion
of air-water. To increase their efficiency they are located at the top of the plant. The
other reason is the easy pumping of cooled water back to the required operation.

The fills are made up of plastic which are pf honeycomb shape. This geometry
provides good contact between air-water.

Table 5.2 Cooling Tower Data

MOC of Casing Glass Fiber -


MOC of Fill Plastic -
Pumped used Centrifugal pump -
Head of pump 37 m
Change in Temperature 10-15 ℃
Fan Propeller type -
Area 5 m2

5.7 Conclusion

We conclude that Utility area is an important section of a plant which is house to


various boilers, large compressors, cooling towers, water treatment plants etc.
The bad management of of utilities can make even the most profitable processes
unprofitable. Utilities are used to maintain processing parameters like pressure,
temperature, etc., without which it is impossible to carry out the process.

51
CHAPTER 6
DESCRIPTION OF THE EQUIPMENT

52
6.1 Introduction

Numerous equipment are involved in the construction of any plant. After selection
process it becomes inevitable to decide the equipment necessary to accomplish the
process.

Suitable MOC is decided according to the fluid to be handled considering their nature,
properties, corrosion, fouling and reactivity with their material of the equipment. The
MOC should be selected which is capable enough to withstand these conditions and
work efficiently getting damage and at the same time providing maximum conversion
and yield.

6.2 Stainless Steel Reactor

Table 6.1 Detailed Description of SSR

Number of Reactor 2
Material of Construction SS 304
Type of Vessel Closed type jacketed vessel
Shell Capacity 200 L
Volumetric Capacity 2500 L
Stirrer Anchor
Diameter 1500 mm
Length 1700 mm

53
6.3 Pressure Nutsche Filter

Table 6.2 Detailed Description of PNF

Material of Construction SS 316


Maximum Pressure 6 kg/cm2
Pore size 5 microns
Filter cloth Alkali cloth

6.4 Centrifuge

Table 6.3 Detailed Description of Centrifuge

Material of Construction SS 316


Basket Diameter 1200 mm
Basket Height 1050 mm
Spinning Speed 1000 rpm
Capacity 377 L/batch
Filter Medium Alkali cloth

6.5 Vacuum Tray Dryer

Table 6.4 Detailed Description of VTD

Material of Construction SS 316


Number of Trays 96
Mode of Heating Hot Water under the plates
Maximum Vacuum 760 mmHg

54
6.6 Conclusion

From this chapter we conclude that suitable MOC is to decided according to the fluid
to be handled considering their nature, properties, corrosion, fouling and reactivity
with their material of the equipment. The MOC should be selected which is good
enough to withstand these conditions and work efficiently getting damage and at the
same time providing maximum conversion and yield. The important selected
equipment are to be designed in the next chapter.

55
CHAPTER 7
DESIGNING OF EQUIPMENTS

56
7.1 Introduction

The processing, storage, or transportation of any raw material, product or utility


requires specific equipment to serve its purpose. These equipment are to be designed
keeping in mind optimum conditions of the process, its residence time and its
orientation to get maximum yield.

Designing is the most creative work carried out by Chemical Engineer. Equipment
Designing is basically divided in two parts:
(i) Process Design
(ii) Mechanical Design

Process design is a basic design and it is done by Chemical Engineers which includes
calculations of volume and residence time in case of Reactors, Number of Stages,
Feed Location, Design of down comer, weir design in case of a distillation column,
overall heat transfer coefficient, dirt factor, and pressure drop calculations in case of
Heat Exchanger and NPSH calculation in case of pump design.

Mechanical design deals with the calculations of height, daimater, thickness of shell,
thickness of head, thickness of nozzles, flanges, number of bolts and calculation for
supports.

Thus design of any equipment is the one of the main aspect in the industry. Somewhat
over design is provided by the design engineers considering the safety aspect but too
much over design is also unfavorable.

57
7.2 Design of Reactor

Data Given:
XA=0.90 (assumed value)
Density of KSM 01 = 1.46 g/cm3
M.W. of KSM 01 = 309.66 kg/kmol
Mass of KSM 01 = 152.35 kg
Batch Time = 12 hr.

Reaction:

IPA
C13H19N2 + C6H5N3O + Na2CO3 → C19H22ClN5O + 2NaCl + H2O + CO2

C
A + B + D → E + 2G + H + I

Where,
A= KSM-01 (Raw Material); C13H19N2
B= KSM-02 (Raw Material); C6H5N3O
C= Isopropyl Alcohol (Raw Material); C3H8O
D= Sodium Carbonate (Raw Material); Na2CO3
E= Trazodone (Main Product); C19H22ClN5O
F= Hydrochloric acid (Intermediate); HCl
G= Sodium Chloride (By Product); NaCl
H= Water(By Product); H2O
I= Carbon dioxide; CO2

Order of Reaction = 2
Rate Constant, k = unknown (mol/lit-hr)-1
But we know that batch time in this process = 12 hr.

Initial volume of KSM 01 at time t=0


NAO = mass of KSM 01 / M.W. of KSM 01

58
= 152.35 / 309.66
= 0.492 Kmol

Volume of KSM 01,


V = mass/density
= 152.35 / 1.46
= 0.104 m3

Initial concentration of KSM 01,


CA = NAO / V
= 0.492 / 0.104
= 4.73 mol/lit

Now,
τ = 12 hr.
τ / CAO = XA / -rA
-rA = 0.370 mol/lit hr

Rate of Reaction -rA = K CA2 (⸪ Second order reaction)


We know, CA = CAO(1-XA)
⸫ -rA = kCAO2(1-XA)2
⸫ 0.370 = k * 4.732 * (1-0.9)2
⸫ k = 1.65 (mol/lit hr)-1

PA0 = CA0RT
R = 0.082 lit atm/mol K
T = 288 K (inside temperature of reactor)

PA0 = 8 * 0.082 * 288


= 188.928 atm
= 19.143 MPa

59
Summary of Process Design of SSR

Conversion = 90 %
Rate of Reaction = 0.370 mol/lit hr
Order of Reaction = 2
Rate Constant = 1.65 (mol/lit hr)-1

7.3 Mechanical Design of Pressure Vessel

Feed rate of KSM 01 = 226.058 kg/batch


Feed rate of KSM 02 = 98.6376 kg/batch
Density of KSM 01 = 1.46 kg/lit
Density of KSM 02 = 1.65 kg/lit
Total Feed Rate = (226.058 / 1.46) + (98.6376 / 1.65) lit/batch
= 214.6146102 lit/batch
The amount of IPA used per batch = 900 L
Hence, the total capacity = 1114.614 L
Available volume = 1200 L

Let, L/D = 1
V = π/4 * D2 * L
⸫ 1.2 = π/4 * D2 * D
⸫ D = 1.24 m
So, L = 1.145 m
Volume contained in head V” = 0.089D3
= 0.089 * (1.24)3
= 0.11 m3

MOC used is SS 316

60
 For Thickness of Shell:

P0 = 3.52 atm = 3.6369 psi


Pd = 1.1*P0 = 3.872 atm = 4 psi
Di = 1.2409 m
f = 1124.91 psi
J = 0.85

Thickness, ts = P*Di / (2*f*J - P)


ts = (4* 1240.9) / ((2 * 1124.91 * 0.85) - 4)
= 0.26 m

C.A. = 2.6 mm + 2 mm
= 4.6 mm

tf = 5 mm

 For Torispherical Head:

Thickness, th = (P * D * CS) / (2*f*J + (CS - 0.2)*P)


where,
CS = 1/4 * (3 + (Rc / Rk)0.5)
Rc = 12.409 cm
Rk = 10% of Rc
= 1.2409 cm
CS = 1/4 * (3 + (12.409 / 1.2409)0.5)
= 1.541

For J = 0.85
f = 1124.91 psi
P = 4 psi
Tf = (4 * 124.09 * 1.541) / ((2 * 1124.91 * 0.85) + (1.541 - 0.2)*4))
= 0.39 cm
= 3.9 mm + 2 mm

61
= 5.9 mm
= 6 mm

B.D. = ((Inner Diameter + Outer Diameter)/2) * 1.15 + SF

O.D. = I.D. + 2t
= 124.09 + (2 * 0.6)
= 125.2 cm

B.D. = ((124.09 + 125.2)/2) * 1.15) + (3* 0.6)


= 144.49 cm

Weight of closure = (π/4) * (B.D.)2 * tf * ρ


= (π/4) * (144.49)2 * 0.59 * 0.008
= 78.66 kg

7.3.1 Nozzle Design

 Man Hole:

Diameter = 1000 mm
Thickness, tm = P * Do / (2 * f * J)
= (4 * 1000) / (2 * 1124.91 * 0.85)
= 2.091 mm

Take corrosion allowance = 2 mm


⸫ Design Thickness = 4.091 m
⸫ Fabrication Thickness = 5 mm

 Jacket Design:

Internal Diameter of Jacket, Di = 1920.2 mm


Thickness of Jacket, trj = P * Di / (2*f*J - P)

62
trj = 4 * 1920.2 / (2 * 1124.91 * 0.85 - 4)
= 4.02 mm

tj = trj + C
where, C = Corrosion Allowance = 2 mm

⸫ tj = 4.02 + 2
= 6.02 mm
So, take thickness of Jacket tj = 8 mm

Outside Diameter of Jacket,


Djo = Dj + 2tj
= 1920.2 + (2*8)
= 1936.2 mm

Now take diameter of coil, Dc = 150 mm


Thickness of coil, trc = P * Dc / 2 * f
= 4 * 150 / (2 * 1124.91)
= 0.4 mm

tc = trc + C
where, C = Corrosion Allowance = 2 mm

tc = 0.4 + 2
= 2.4 mm
So, take thickness of coil tc = 4 mm

Circumferential stress in the shell,


fps = fp + fac
= (P * D) / (2 * ts) + (P * Dc) / (4 * tc + 2.5 * ts)
= (4 * 1900) / (2 * 4) + (4 * 150) / (4 * 4 + 2.5 * 4)
= 973.076 kgf/cm2 < 1124.91 kgf/cm2
Thus, our design is safe.

63
7.3.2 Agitator and Shaft Design

Diameter of agitator, Da = Diameter of reactor/2 = 1908.2/2 = 954.1 mm


Length of agitator shaft between bearing and agitator, L = 3 m
Width of Blade, bw = 120 mm
Number of baffles at tank wall = 4

MOC of Shaft and Agitator blade is IS-2062 Grade ST 42-W

Ultimate tensile stress = 4200 kgf/cm2


Yield Stress = 2300 kgf/cm2
Maximum Allowable Shear Stress in Shaft = 550 kgf/cm2
Modulus of Elasticity, E = 19.5 * 105 kgf/cm2
Power required for motor = 7.5 hp

Continuous average torque is given by,


τc = hp * 75 * 60 / (2 * π * N)
Assume N = 60 rpm
τc = 7.5 * 75 * 60 / (2 * π * 60)
= 89.524 kgf.m

Maximum possible torque in agitation system at start up condition is give by,


τm = 1.5 to 2.5 τc
Let us make τm = 2 * τc
= 2 * 89.524
= 134.286 kgf.m

Maximum shear stress created in shaft,


fs = τm / Zp
where, Polar sectional modulus for circular shaft, Zp = π d3 / 16
⸫ 550 = (134.286 * 100) / ( π d3 / 16)
⸫ d3 = 124.41 cm3
⸫ d = 4.99 cm

64
Bending Moment,
M = Fm * L
Fm = m / (0.75 * Rb)
where, Rb = Radius of Blade = (Da/2) = 954.1/2 = 477.05 mm
Fm = 179.048 * 1000 / (0.75 * 477.05)
= 375.32 kgf

M = Fm * L
= 375.32 * 3
= 1125.97 kgf.m

Me = 0.5 (M + (M2 + τm2)0.5)


= 0.5 (1125.97 + (11252 + 134.282)0.5)
= 629.95 kgf.m

Stress created by equivalent bending moment, f = Me / Z


f > yield stress = 2300 kgf/cm2
f = Me / Z
⸫ 2300 = 629.95 * 100 / ( π d3 / 32)
⸫ d = 6.53 m

Let diameter of shaft, d = 12 cm = 120 mm


f = Me / Z
= 629.95 * 100 / (π * (12)3 / 32) = 1871.59 kgf/cm2
f < yield stress = 2300 kgf/cm2
Hence, we can provide d = 120 mm

Moment of Inertia, I = π d4 / 64
= π * 124 / 64
= 1017.34 cm4

65
Maximum Deflection in Shaft,
∆ = F m * L3 / 3 * E * I
= 375.32 * 3003 / 3 * 19.5 * 105 * 117.79
= 14.70 cm

Critical Speed, Nc = 60 * 4.187 / ∆0.5


= 65.19 %
Hence shaft diameter = 120 mm

Blade Thickness calculation:


Endurance limit for Carbon Steel = Ultimate Tensile Stress / Factor of Safety
= 4200 / 2
= 2100 kgf/cm2
Maximum stress created in blade material,
f=m/Z
f = Max. B.M. / Z
⸫ 2100 = m / (bt * bw / 6)
⸫ 2100 = 179.048 * 100 / (bt * 122 / 6)
⸫ bt = 0.355 cm
⸫ bt = 3.55 + 2C
= 3.55 + 2*1.5
= 6.55 mm
Use 8 mm thick agitator Blade

66
7.4 Pump Design

Pump for charging IPA to the reactor.


Required flow rate (Q) = 0.002 m3/s
Internal diameter of pipe (d) = 0.06 m
Viscosity of fluid (μ) = 0.0024 kg.m/s
Density of fluid (ρ) = 786 kg/m3
Height up to which water is to be pumped = 15 m
Horizontal distance traveled by water = 5 m

Velocity of Fluid

v = Q / (π/4)*d2
= 0.002 / (π/4)*0.062
= 0.707 m/s

Reynold’s Number,
Nre = d * v * ρ / μ
= 0.06 * 0.707 * 786 / 0.0024
= 13892.55
⸫ Flow is Turbulent.

Head Losses

1) Loss due to fittings:


(a) Due to 90° Elbow:
Hf90 = [K * v2 / (2 * 9.81)] * n (where, n = number of elbow used)
= [1.3 * 0.7072 / (2 * 9.81)] * 4
= 0.132 m

(b) Due to 45° Elbow:


Hf45 = [K * v2 / (2 * 9.81)] * n
= [0.4 * 0.7072 / (2 * 9.81)] * 4

67
= 0.0407 m

2) Losses due to Valves:


(a) Due to Valve:
Hf Ball Valve = [K * v2 / (2 * 9.81)] * n
= [0.05 * 0.7072 / (2 * 9.81)] * 2
= 0.0025 m
(b) Due to Check Valve:
Hf Check Valve = [K * v2 / (2 * 9.81)] * n
= [2 * 0.7072 / (2 * 9.81)] * 1
= 0.05 m

3) Losses due to Pipe Friction:


As the flow is turbulent flow, the following equation will be used:
f = 0.25 / (log(e/3.7D) + (5.74 / Re)0.9)2)
Roughness factor for cast iron pipe (e) = 0.0004 for cast iron pipe
f = 0.25 / (log(0.0004/3.7*0.06) + (5.74/13892.55)0.9)2
= 0.0332

∆Hfp = (f * v2 / D * 2 * g) * L
= (0.0332 * 0.7072 / 0.06 * 2 * 9.81) * (15 + 5)
= 0.28 m

Total friction losses = losses due to (fittings + valves + pipe friction)


= (0.132 + 0.04079 + (0.0025 + 0.05) + (0.28)
= 0.5052 m

Net Positive Suction Head (NPSH)

NPSH = Patm + Hs + Psurface - Pvapour pressure - total losses

(i) Patm = Pressure in PSI * 2.31 / SP.GR


= (14.7 * 2.31 / 0.7851) / 3.28
= 13.1865 m

68
(ii) Hs = 0.5 m

(iii) Psurface = 0 (because the pressure at the surface is atmospheric pressure)

(iv) Pvapor pressure = Vapor of IPA pressure in PSI * 2.31 / SP.GR


= (0.773 * 2.31 / 0.7851) / 3.28
= 0.6934 m

NPSH = 13.1865 + 0.5 + 0 - 0.6934 - 0.5052


= 12.4879 m

69
7.5 Storage Vessel Design

The storage vessel is used to store IPA which is used as a solvent in the production of
Trazodone. Amount of IPA used per batch can is about 1500 L.

Data available:

V = 1500 L
MOC used is SS 304
P’ = 0.0125 kgf/cm2
F = 180 kgf/cm2
E = 2 * 106 kgf/cm2
Density = 7800 kgf/cm2
J = 0.85
Plate size = 1 m * 2 m

Since volume is around 1500 L, so H/d ratio will be around 1.5

⸫ H/d = 1.5
⸫ V = (π/4) * 1.5 * d3
⸫ 1.5 = (π/4) * 1.5 * d3
⸫ d3 = 1.27388535
⸫ d = 1.084 m
⸫ H = 1.6256

Now,
P = ρ (H - 0.3) + P’
= 786 (1.626 - 0.3) + 0.0125
= 0.14612 kgf/cm2

Also,
t=Pd/2fJ
= 5.17 mm

70
Similarly,

Table 7.1 Computed Values of Thickness


Height from Pressure Thickness Available Actual
bottom (kgf/cm2) (mm) Thickness Thickness
(mm) (mm)
1 0.14612 5.17 6 6
2 0.0612 2.4 3 4

Now for the Design of Torispherical head,


Rc = 1094 mm
Rk = 65.04 mm
C = 0.92
th = Pi * Rc * C / ((2 f J) + CA)
⸫ th = 101325 * 1.094 * 0.92 / (2 * 0.85 * 1.765 * 107)
⸫ th = 3 mm
But minimum thickness = 5 mm
SF = 3th = 15 m

BD = Do + (Do/42) + 2SF + (2/3)Rk


⸫ BD = 1094 + (1092/42) + 30 + (2/3)(65.04)
⸫ BD = 1193.40 mm

7.6 Conclusion

In this chapter, we carried out the process design and mechanical design of the major
equipment used in the process. We conclude that Process design of Reactor gave us
Kinetics while Mechanical design deals with the calculations of height, daimater,
thickness of shell, thickness of head, thickness of nozzles, flanges, number of bolts
and calculation for supports. Somewhat over design is provided considering the safety
aspect.

71
CHAPTER 8
PUMPS AND VALVES

72
8.1 Details of Pump

Table 8.1 Detailing of Pumps

Sr. Type of Pump Specification Application MOC Supplier


No.

1 Centrifugal Head = 22 m Feed Supply SS Investa


pumps
Imp dia = 133 mm

Speed = 2900 rpm

Flow rate = 5 m3/hr

H.P = 2.2 KW

2 Centrifugal Head = 22 m Feed Supply SS Investa


pumps
Imp dia = 150 mm

Speed = 2900 rpm

Flow rate = 3 m3/hr

H.P = 1.8 KW

3 Centrifugal Head = 22 m Mother liquor SS Investa


to storage pumps
Imp dia = 150 mm tank

Speed = 2900 rpm

Flow rate = 9 m3/hr

H.P = 5 KW

4 Centrifugal Head = 22 m Mother liquor SS Investa


to ETP pumps
Imp dia = 250 mm

Speed = 2100 rpm

Flow rate = 18
m3/hr

H.P = 9.5 KW

73
8.2 Details of Valves

Table 8.2 Detailing of Valves

Sr. No. Type of Valve Application Selection MOC Supplier


Criteria
1 Ball Valve Water Inlet On-off purpose, SS 304 Inflow
cheaper, Low Valve
Maintenance
2 Ball Valve Product On-off purpose, SS 304 Inflow
Outlet cheaper, Low Valve
Maintenance
3 Ball Valve N2 line On-off purpose, SS 304 Inflow
cheaper, Low Valve
Maintenance
4 Ball Valve Vent line On-off purpose, SS 304 Inflow
cheaper, Low Valve
Maintenance
5 Ball Valve Safety On-off purpose, SS 304 Inflow
Valve line cheaper, Low Valve
Maintenance
6 Ball Valve Pressure On-off purpose, SS 304 Inflow
Gauge line cheaper, Low Valve
Maintenance
7 Globe Valve Steam Inlet Flow regulation, CS Inflow
and Outlet No leaks Valve
8 Butterfly Valve In hopper On-off purpose CS Inflow
and powder Valve
transferring

74
8.3 Control Valve

There are no control valves in this plant but one can implement a control valve for
controlling the steam flow rate which in turn controls the temperature of the reactor.
The basic control loop for such a control valve is given below.Cost of such control
system would be around Rs. 35000. Installing such a controller would be good from
safety point of view.

Error Error Signal Heat


Comparator Reactor/
Controller Steam Valve
Jacket

Thermocouple

Figure 8.1 Block Diagram of Control Valve

Water
Inlet

Hot Steam
Water
Tank
Sensor

HE Reactor

Figure 8.2 Schematic view Control System

75
8.4 Conclusion

Unlike in any Chemical Process Industry, in Pharmaceutical Industries DCS system is


mostly not implemented. However, recent developments show the applications of
DSC system even in Pharmaceutical Industries. Mostly for material handling,
Centrifugal pump was used. Ball valve is preferred owing to the smoothness in
operation.

76
CHAPTER 9
HEALTH, SAFETY AND ENVIRONMENT

77
9.1 Introduction

Safety is the state of being “safe”, the condition of being protected against physical,
social, spiritual, financial, political, emotional, occupational, psychological,
educational or other types or consequences of failure, damage, error, accidents, harm
or any other event which could be considered non-desirable. This can take the form of
being protected from the event or from exposure to something that causes health or
economical losses. It can include protection of people or of possessions.

Accidents are analyzed and developed a separate engineering branch of safety and this
analysis was required due to:
 Rising trend of accidents.
 Increased use of machinery.
 Increased material handling.
 Lack of safety standard.
 Lack of training.
 Better reporting of accidents.

No industry can afford to neglect the fundamentals of safety in design and operation
of its plant and machinery. It is important that all the people responsible for
management and operation of any industry should have a good knowledge of
industrial safety.

78
9.2 Safety Measures Taken By Industry

 No mobile phones, flammable items, cameras are allowed within the company.
Food items, tobacco, or smoking are strictly prohibited within the premises.

 Interns are not allowed to enter the plant unless they have been granted the
permission of HR Department and Head of Department of the respective plant.

 All people within the premises have to wear helmet, and safety shoes including
the interns.

 Accidents and incidents are investigated and recorded and maintained time to
time. All employees are informed regarding the cause.

 Inherent safety inspection is done on regularly safety officer, plant in-charge, and
head of the plant.

 To create awareness of safety in worker and employees, “Daily Talks” are


conducted which involves topic such as:

(a) Good House Keeping


(b) GDP
(c) GMP
(d) SOPs
(e) Health and Hygiene
(f) Handling of Raw Material and Products
(g)Labeling Procedure
(h) Disposal Technique for used PPEs, Labels, etc.

 Standard Operating Procedures are employed for cleaning of equipment, loading


and unloading of materials, changing and discharging of equipment.

79
 Powder transferring system is used for charging powdered material to the reactor
which provides safe working operation. The open lines of PTS are kept covered
with POLYBAG.

 Intermediate and Products are stored in DEDICATED STORAGE DRUM to


avoid cross contamination. Also, dedicated hose pipes are used for fluid transfer.

 Nitrogen blanketing is used while charging the solvents. Solvents are stored
under inert atmosphere for safe storage condition.

 Do’s and Don’t are mentioned within Solvent Tank Farm are to be followed.

80
9.3 Safety Equipment

 Respiratory Protective Device

(a) Breathing Apparatus - used while handling gas leakages.

(b) Canister Mask - used while cleaning vessels or reactor inner wall.

(c) Air Mask - used while doing internal cleaning of vessel.

(d) Dusk Mask - used where there is much exposure of dust.

 Non-Respiratory Protective Device

(a) Eye Protection - Safety goggles, Chipper goggles, Gas tight goggles, are used.

(b) Head Protection - Helmet

(c) Face Shield - used during welding.

(d) Hand Protection - Gloves

(e) Foot Protection - Safety Shoes

(f) Body Protection - Apron, PVC Suit

(g) Hearing Protection - Ear Plug/Ear Muff

(h) Fire Fighting Equipment

(i) Safety Belts and Harness

81
 Head Protection

Head protectors are hard hats, caps, helmets made of aluminum, PVC, fiberglass,
laminated plastic or vulcanized rubber. They may be fitted with breckres for fixing
marks, protective faces screen or lamp. The hats and caps are provided with
replaceable harness, which provides sufficient clearance between the top of the head
and shell. Soft caps and hoods are also used for protection against heat, sparks, and
other dangerous material and are made up of appropriate materials.

 Eye and Face Protection

Eye injuries can be caused by dust, flying particle, splashes and harmful radiations.
Eye protectors are safety spectacles, mono goggles, impact goggles, wilding goggles,
foundry goggles, chemical goggles, and gas tight goggles, face shield, etc

 Eat Protection

Noise level above 90 DBA is hazards if human body is expose to it for more than 8
hrs/day or 48 hrs/week. It may cause deafness, loss of efficiency, irritation, and also
loss of hearing, noise level can measure by a Noise Average Meter or a Noise Dose
Meter, Earplug or Earmuff reduce to at 25 to 49 DBA ear plug is made of plastic,
rubber of polyurethane foam. Ear Muff covers external ear and provides better
attenuation than earplug.

 Body Protection and Foot Protection

Body Protectors are coats, aprons, overall jackets and complete head to toe protective
suits. Nature of potential hazard, degree of hazard involved and nature of activities of
the earner are important in the selection of safety clothing. Although complete of the
body and legs are not needed in many cases, unnecessary safety clothing may hamper
the efficiency of the wearer.

82
Rubber boots protects against chemical splashes, aromatic liquids or solvents and
heavy weight.

9.4 Safety Related Equipment with their Location

 Personal Protection Equipment

The PPEs are kept in “PPE BOX” and such boxes are located nearby the process
controlling equipment. The already contains all the PPEs which are mandatory for the
safety purpose, Such boxes are regularly maintained.

 Mobile Fire Extinguisher

They are used for blowing off fire if needed. They are located on specific spots, where
the chance of fire is prominent such as near by solvent day tanks, reactors, offices,
office, stores, etc.

 Fire Hydrant

They are fixed to ground and are located outside the plant. There is a hydrant line
connected to it through which water is continuously flowing. They are helpful for
blowing large and external fire outside the plant.

 Powder Transferring System

This equipment is used for charging powdered material into the reactor when the
reaction is going on. This equipment ensures that no foreign substance falls along the
desired material. It gives inert charging atmosphere.

83
Table 9.1 Types of Fire Extinguishers

Type Capacity Unit Fire Class Description

Dry Chemical 51 kg A,B,C Fire due to paper, cloth,


Powder petroleum product, electric fire,
gas fire.

Foam Type 10 kg A,B Fire due to paper, cloth,


cardboards, gas fire.

Carbon 5 kg B,C Fire due to gas fire, welding gas


Dioxide Type fire, electric fire.

9.5 Environment

 Source of Water

The source for water is bore well water. There are total 4 bore well within the
company premises which provides the source for water. This water is used as utilized
utility and in boiler. The water is not used straight away, it is processed and utilized.

The treatment involves water softening by ion exchange, and then followed by RO
process and it is finally used for utility purpose and as boiler feed water.
Some of the parameters which are continuously measured are pH, TDS, TSS,
Turbidity, Hardness, Biological content, etc.

 Usage of Water

The treated water is sent across the premise as raw water is not desired anywhere.
Water is used right from the beginning as a form of raw material till the end of
process.

84
Many processes utilize treated water as primary solvent i.e. for dissolving solids to
prepare aqueous solution. Even boiler feed, cooling water utilize the same treated
water. Water wash is also given in centrifuge, reactors and many other equipment.

 Sources of Waste Water Generation

The primary source of waste water generation is washed water from reactors and
centrifuge. This water contains high amount of process chemicals hence resulting in
high COD levels. This also includes water which is used for housekeeping, wash of
small apparatus such as dedicated scoops, hose pipes, cleaning of equipment, drums,
etc.
The secondary source of waste water generation is blow down water from boiler
section and cooling towers.

9.5.1 Treatment for Waste Water

The waste water generation is treated in Effluent Treatment Plant (ETP) and Multi
Effect Evaporator (MEE). The effluent containing high COD are treated in MEE and
the effluent containing low COD are treated in ETP.

High COD effluent is generally by washing of centrifuge, reactors, mother liquor


were water is main component. Where as low COD effluent is generated by water
used for housekeeping, cleaning of small apparatus, etc.

9.5.2 Effluent Treatment Plant

The low COD water is first collected in LOW COD TANK which is provided at the
plant site itself. Once the tank is filled, then it is sent to equalization tank. All the
LOW COD water from all plant is collected in this tank.

In this large tank the pH of waste water is adjusted nearby 7-8 by addition of Acid or
Caustic whichever is desired. Once the pH is adjusted sodium hypo chloride is added.

85
Now the water is transferred to primary clarifier where most of the solids are settled
out and they are removed in form of sludge. This sludge is collected separately.

The water is now transferred to flocculation tank where coagulants are added to it.
After addition of coagulants air is passed from the bottom of the tank and water is
stirred vigorously with the help of turbine type agitator. As a result of this, flocs are
formed which are settled out again as sludge.

The treatment up till now given is primary treatment. The water is now feed to new
tank where a biological culture is added to fulfill the oxygen demand. Here, the
microorganisms culture consumes the organic matter and liberated carbon dioxide,
resulting in formation of sludge. This sludge is settled out in secondary settling tank.
Apart of sludge is recycled back to maintaining concentration of microorganisms in
the water.

The water is decolorized by addition of activated charcoal and then it is passed


through filter press. The filtered water is collected in collection tank. From here the
water is loaded and sent to Common Effluent Treatment Plant (CEPT). The CEPT is
located nearby the company premise.

The high COD is treated in MEE plant. Multiple Effect Evaporator (MEE) is a
thermal evaporation process widely used for concentration of liquids and is
accomplished by boiling of solvents, water. The evaporators used are film type
evaporators.

Waste water is passed through the main effect and then followed by remaining two
effect. The evaporators used are Agitated Thin Film Dryer (ATFD) which removes
water completely and discharge only solid form bottom. This gives zero discharge of
waste water. The solid waste generated is collected in bags and disposed by help of
third party.

86
9.5.3 Source of Air and Usage

The air used within the premises is atmospheric air which is first treated and then
utilized. The atmospheric air is filtered and compressed in multi-stage compressor.
This compressed air is now utilized for drying purpose of vessels, reactors, and other
equipment.

9.5.4 Source of Air Pollution

The major source of Air Pollution is the Boiler Chimney. As the coal is combusted,
SOx, NOx, CO, etc are generated. Along with this particulates matter are also emitted
from the boiler chimney. The other source of air pollution is the release of vents into
atmosphere which mainly contain CO2.

9.5.5 Control Measures taken for Air Pollution

 Boiler Section: Electrostatic precipitator and bag filters are used to collect the
small particulate matter emitting from the fire box of the boiler. The outlet of this
equipment contains less than 100 ppm of particles.

 Process Section: Scrubbers are used for scrubbing undesirable gases emitting to
atmosphere. They are operated in counter current fashion where the solvent is fed
from the top and gas mixture is fed from bottom.

9.5.6 Solid Waste Generation

No solid waste is generated as such. Only the used filter cloth of filters, used cellulose
pad of sparkler filters, and antistatic bags are generated as solid waste. They are
disposed by handling them to third party.

87
9.6 Conclusion

We conclude that no industry can afford to neglect the fundamentals of safety in


design and operation of its plant and machinery. Each Industry has its own policy and
approach towards safety as discussed above. Various safety equipment as used as per
their application and need. Industries need to follow the Environment norms set by the
state and treat the waste accordingly with suitable technology and technique.

88
CHAPTER 10
PLANT LAYOUT AND PLANT LOCATION

89
10.1 Introduction

10.1.1 Plant Layout

After process flow diagram are completed and before detailed piping, structural and
electrical design can begin, the layout of process units in plant and equipment within
these process units must be planned. This layout can play important role in
determining construction and manufacturing costs and thus must be planned carefully,
with attention being given to future problems that may arise.

Proper layout will include arrangement of processing area, storage area, and handling
areas in efficient coordination and with regard to such factors as:

 Type and quality of product to be produced.


 Type of product and process control.
 Type of building needed and building code requirement.
 Operational accessibility and convenience.
 Space available and space needed.
 Health and safety consideration.

10.1.2 Plant Location

The geographic location of final plant can have a strong influence on the success of an
industrial venture. Primarily, the plant should be located where minimum cost of
production and distribution can be obtained, but other factors such as room for
expansion and safe living conditions for plant operation as well as the surrounding
community are also important.

The choice of final site should be based on complete survey of advantages and
disadvantages of various geographic areas and ultimately on available real estate.

90
10.2 Principle of Plant Layout

 Storage Layout

Storage facilities for raw material, intermediates, and finished products may be
located in isolated or adjoining area. This will reduce the internal transportation and
material handling cost. Liquids are commonly stored in cylindrical or rectangular
tanks. While gases are stored in spherical or hemispherical or cylindrical pressurized
tanks. Solids which are not affected by open atmosphere conditions can be stored in
open bins or silos.

 Equipment Layout

During modeling of equipment layout, ample space should be assigned to each piece
of equipment. Identical equipment which are repeated several times in flow of
material should be arranged in group or series and this may reduce operating cost.

 Plant Expansion

During the procedure of plant layout, there must be a specified provision for plant
expansion. As this provision will be helpful for future expansion of existing plant.
There will be sufficient space available during the time of expansion.

 Building

The plant building may be either in-house or open plant. When there is a need of inert
atmosphere one should go for in-house plant or else open plant are constructed. The
plant buildings are provided with ventilation, lighting, electrical supply, labors,
platforms, etc.

91
10.3 Factors for Plant Location

The factors to be considered are as followed:

 Raw Material availability

 Market

 Energy availability

 Transportation facilities

 Water Supply

 Climate

 Waste Disposal

 Labor Supply

 Community Factors

 Taxation and Legal Restriction

92
10.4 Drawing of Plant Layout

Figure 10.1 Overall Plant Layout

93
10.5 Conclusion

We conclude that factors as discussed above are vital for making the final layout of
the plant. The layout presented above is the same as the actual layout of the plant
which not much accurate as per the need of the ideal plant layout. The layout was
prepared as the methods of unit area sizing each blocks based on the size of the
equipment kept inside the unit.

94
CHAPTER 11
COST ESTIMATION

95
11.1 Introduction

Cost estimation is done to calculate the total cost of the plant including fixed cost,
direct cost, production cost, raw material cost, cost for labor, maintenance, powder
and utilities, along with cost for the plant and administrative overhead, distribution of
final products and other miscellaneous items.

As soon as the final process design stage is completed, it becomes possible to make
accurate cost estimation because detailed equipment specification and definite plant
facility information are available. Direct price quotations based on detailed
specifications can then be obtained from various manufacturers. However, no design
project should proceed to the final stages before costs are considered, and cost
estimates should be made throughout all the early stages of design when complete
specifications are not available.

The cost estimation also gives us an idea about the direct charges, indirect charges,
fixed capital investment, working capital, plant overhead expenses, etc.

11.2 Purchased Equipment Cost

11.2.1 Based on MOC

Reactor installed is jacketed vessel operating at atmospheric condition having


adequate openings for inlet and outlet and for measuring device. MOC used for vessel
is SS 316 plate of dimension 150 × 120 mm.

Cost of SS 316 is Rs. 300/kg

Volume of vessel = π/4 × (Do2 –Di2) × Height


= π/4 × (125.22 – 124.092) × 114.5
= 24871.55 cm3

96
Here density of material = 8000 kg/m3
= 0.008 kg/cm3

So weight of vessel = (volume × density of material)


= (24871.55 × 0.008)
= 198.97 kg

Now,
Cost of MOC = (material cost per kg × weight of vessel)
= (300 × 198.97)
= Rs. 55,691

Weight of Jacket = π/4 × (Do2 –Di2) × Height × Density


= π/4 × (193.622 –192.022) × 114.5 × 0.008
= 443.67 kg

Cost of Jacket = (material cost per kg × weight of vessel)


= 300 × 443.67
= Rs. 1,33,101

Weight of torispherical head = π/4 × BD2 × thickness of head × Density of MOC


= π/4 × 144.49 × 0.6 × 0.008
= 78.66 kg

Cost of torispherical head = (material cost per kg × weight of head) = 33936 INR
= 300 × 78.66
= Rs. 23,599.76
⸫ Total cost of head = 2 × 23599.76 = Rs. 47,199.53

Weight of nozzles = π/4 × (Dno2 – Dni2) × (Hi + Ho) × Density of MOC


⸫ Weight of manhole nozzle = π/4 × (60.822 – 602) × (3.476) × 0.008
= 2.1 kg

97
So,
Total weight of 7 Nozzles = 7 × 2.1
= 14.76 kg
⸫ Total cost of 7 nozzles = weight of 7 nozzles × material cost per kg
= 14.76 × 300
= Rs. 4428

Cost of Flange and bolt

Weight of flange = π/4 × (Dfo2 – Dfi2) × Flange thickness × Density of MOC


⸫ Weight of manhole flange = π/4 × (70.4622 – 60.822) × 6.20 × 0.008
= 49.37 kg

So,
Total weight of 7 flanges = 150 kg
Total cost of flanges = (total weight × cost per kg)
= (150 × 300)
= Rs. 45000

Cost of bolts = Number of bolts × Cost per unit


= 92 × 10 INR per 3/8 UNC 56 bolt
= Rs. 920

Cost of fabrication

Perimeter = 3.14 × 124.09 = 389.64 cm


Length = 114.5.7 cm

Now if we select (150×120) cm plates


Then,
Plates required of 150 cm = 3
Plates required of 120 cm = 1

Total no of plates required = 3

98
So total area of plates = 3*1.8
= 5.4 m2
= 58.12 ft2

Now total cost of fabrication = Total area × cost per unit area
= 58.12 × 100
= Rs. 5812

Cost of welding
Length = 150 cm
Width = 120 cm
No. of plates = 3

Total length of welding = 2(length + width) ×no of plates


= 2× (150 + 120) × 3
= 1620 cm
= 16.20 m

Cost of welding = (Total length of welding × 100 Rs/m)


= 16.20*100
= Rs. 1620

Cost of agitator = Rs. 65,000

Total cost of Reactor = (cost of MOC+ cost of jacket + Cost of heads + cost of
nozzles + cost of flanges + cost of fabrication + cost of welding + cost of agitator)
=(55691+133101+23600+47200+4428+4500+920+5812+1620+55000) = Rs. 331572
Therefore,
Cost of reactor = Rs. 3,31,572
⸫ Cost of 2 reactors = 2 * 331572
= Rs. 6,63,144

99
Table 11.1 Purchased Equipment Cost

Sr. No. Equipment Quality Cost (Rs.)

1 Stainless Steel Reactor (SSR) 2 664000

2 Centrifuge 1 696000

3 Pressure Nutsche Filter (PNF) 1 500000

4 Vacuum Tray Dryer (VTD) 1 1500000

5 Pump 2 22000

6 Storage Tank 2 90000

So, Total Purchased Equipment Cost = Rs. 3472000

11.3 Capital Cost

Purchased Equipment Cost (PEC) = Rs. 3472000

But we know that,


Total Capital Investment = Fixed Capital Investment + Working Capital Investment

T.C.I = F.C.I + W.C.I

11.3.1 Fixed Capital Investment (F.C.I)

F.C.I = Direct Cost + Indirect Cost

Table 11.2 Direct Cost Factor

Sr. No. Item % of PEC

1 Purchased Equipment Cost 100

2 Insulation Cost 8
3 Installation Cost 39

100
4 Instrumentation & Control 26

5 Piping 31

6 Electrical Installation 10

7 Building including services 29

8 Yard Improvement 12
9 Service Facilities 55

TOTAL 310

Total Direct Cost = 3472000 * 310/100


= Rs. 1,07,63,200

Table 11.3 Indirect Cost Factor

Sr. No. Item % of PEC

1 Construction Expenses 34

2 Contractor Fee 19
3 Contingencies 37

4 Legal Expenses 4
5 Engineering and Supervision 32

TOTAL 126

Total Indirect Cost = 3472000 * 126/100


= Rs. 4374720

Total Fixed Capital Investment (FC)


= Total Direct Cost + Total Indirect Cost
= 10763200 + 4374720
= Rs. 15137920

101
11.3.2 Working Capital Investment (W.C.I)

It includes the total cost invested in:


 Raw Material and supplies carried in stocks.
 Finished product in stocks and semi finished products in process of being
manufactured.
 Accounts receivable
 Cash kept on hand for monthly payment of operation expenses.
 Account Payable
 Taxes Payable

It is in the range of 20% of Total Capital Investment (T.C.I)


T.C.I = F.C.I - W.C.I
⸫ T.C.I = F.C.I + (0.2) T.C.I
⸫ (0.8) T.C.I = F.C.I
⸫ T.C.I = F.C.I / (0.8)
⸫ T.C.I = 15137920 / 0.8
⸫ T.C.I = Rs. 18922400

Now,
W.C.I = T.C.I - F.C.I
⸫ W.C.I = 18922400 - 15137920
⸫ W.C.I = Rs. 3784480

Capital Investment Cost (Rs.)


F.C.I 15137920
W.C.I 3784480
T.C.I 18922400

102
11.4 Manufacturing Cost

11.4.1 Fixed Charges

(1) Depreciation
For Machinery, 10% of F.C.I = Rs. 1513792
For Building, 2.5% of F.C.I = Rs. 378448
Total = 1513792 + 378448
= Rs. 1892240

(2) Local Taxes


1% of F.C.I = Rs. 151279.2

(3) Insurance
2% of F.C.I = Rs. 302758.4

Total fixed charges = 1892240 + 1512792 + 3027584


= Rs. 2346377.6

Plant overhead cost is 10% of total fixed charges.


Plant overhead cost = 10 % of 23463776
= Rs. 234637.76

11.4.2 Direct Production Cost

Table 11.4 Direct Production Cost

Sr. No. Item % Cost Cost (Rs.)


1 Operating Labour 10% of Total Equipment Cost 347200
2 Direct Supervision 10% of Operating Labour 34720
3 Utilities 12% of Total Equipment Cost 416640
4 Maintenance and Repairs 7% of F.C.I 1059654.4
5 Operating Supplies 10% of Maintenance and Repair 105965.44

103
6 Laboratory Charges 12% of Operating Labour 41664
7 Patent and Royalties 5% of Total Equipment Cost 173600
8 Plant Overhead Cost 10% of Total Equipment Cost 347200
9 Raw Material Cost 60% of F.C.I 9082752

So, Total Direct Production Cost = Rs. 11609395.84

Manufacturing Cost = Direct Production Cost + Plant Overhead Cost +


Fixed Charges
= 11609395.84 + 234637.76 + 2346377.6
= Rs. 14190411.2

11.4.3 General Expenses

Table 11.5 General Expenses

Item %Cost Cost(Rs.)


Administration Cost 12% of F.C.I 1816550.4
Distribution and Selling Cost 10% of F.C.I 1513792
R&D Cost 5% of F.C.I 756896

Sales and Services 5% of F.C.I 756896

So, Total General Expenses = Rs. 4844134.4

11.4.4 Total Production Cost

Total Production Cost = Manufacturing Cost + General Expenses


= 14190411.2 + 4844134.4
= Rs. 19034545.6

104
11.5 Profitability Analysis

11.5.1 Yearly Production

Total 10 tons of Trazodone is expected to be made per year.


The average value of Trazodone at which it is sold is Rs. 4000/kg
Thus, the Total Income = 4000 * 10000
= Rs. 40000000

11.5.2 Gross Profit

Gross Profit = Total Income - Total Production Cost


= 40000000 - 19034545.6
= Rs. 20965454.4
11.5.3 Net Profit

Income Tax (IT)

It is in range of 30-50% of Income


Assume 40% of Income
So,
Income Tax (IT) = 0.40*20965454.4
= Rs. 8386181.76

Net Profit = Gross Profit - Income Tax


= 209655454.4 - 8386181.76
= Rs. 12579272.64

11.5.4 Rate of Return

Rate of return = (Net Profit / TCI) * 100


= 12579272.64 / 18922400
= 66.47%

105
11.5.5 Payback Period

Payback Period = F.C.I / Net Profit


= 15137920 / 12579272.64
= 1.2
= 2 year

11.6 Conclusion

All calculations are based on percentage of purchased equipment cost method. From
the product value we found annual production cost which actually is raw material
inventory saving cost. From that we concludes that average 1 crore rupees net profit is
obtained by running of the plant. Also we calculated direct cost, indirect cost,
depreciation, local taxes, plant overhead cost, insurance policy, manufacturing cost,
general expenses, etc.

106
CHAPTER 12
CONCLUSION

After completing this Phase-I training, I came to study practical elements of Chemical
Engineering. Also this training has helped me learn a lot in terms of technical along
with social things. I got an opportunity to understand the practical functioning of
various equipment with their basic design and application along with running
processes. I also tried to observe important aspects of industrial management,
discipline, and safety precautions. What I studied here is some general information
about product, process description, salient features of the plant, diagrams, mass
balance, energy balance, Functioning of major & minor process equipment, safety
rules, utilities, ETP along with cost estimation of the plant.

107
CHAPTER 13
BIBLIOGRAPHY

Joshi M.V.; Mahajani V.V. Process Equipment Design, 3rd ed.; Macmillan India Ltd:
New Delhi, 1976; p.96, 106,115,126 to 131,201,202,334,340,368,369.

Peters Max S.; Timmerhaus Klaus D. Plant Design and Economics for Chemical
Engineers, 4th ed.; McGraw-Hill, Inc.: New York, 1991; p.300.

Robert E. Treybal; MASS TRANSFER OPERATION; 3rd edition; McGraw Hill:


1980.

Thakore S.B.; Bhatt B.I. Stoichiometry, 5th ed.; TMHEPL: New Delhi, 2010; p.
11,111,187,193,382,397.

Thakore S.B.; Bhatt B.I. Introduction to Process Engineering and Design, 1st ed.;
TMHEPL: New Delhi, 2007; p. 55, 60,135 - 82,663,664.

Warren L. Mc-Cabe, Julian C. Smith, Peer Harriolt; Unit Operations of Chemical


Engineering , 5th edition; McGraw Hill: 1993

108
Phase II
Acotiamide HCl Trihydrate
Table of Contents

LIST OF FIGURES........................................................................................................v
LIST OF TABLES......................................................................................................... v
ABBRIVATIONS........................................................................................................ vii
NOMENCLATURE....................................................................................................viii

CHAPTER 1 INTRODUCTION............................................................................. 1
1.4 Capacity of Product............................................................................................ 3
1.5 Market Value of Product.................................................................................... 3
1.6 Details of Product...............................................................................................3
1.7 Commercial Competitors................................................................................... 3
1.8 Technical Competitors....................................................................................... 4
1.9 Applications........................................................................................................4
1.10 Physical as well as Chemical Properties.......................................................... 5
1.11 Material Safety Data Sheet (MSDS)................................................................ 6
1.12 Conclusion......................................................................................................10

CHAPTER 2 SELECTION OF PROCESS.......................................................... 11


2.1 About Raw Materials........................................................................................12
2.1.1 Raw Material Supply.............................................................................. 12
2.1.2 Transportation.........................................................................................12
2.1.3 Cost of Raw Materials............................................................................ 13
2.2 Physical and Chemical Properties of Raw Materials....................................... 14
2.3 Detailed Process Description............................................................................15
2.3.2 Process Description................................................................................ 16
2.3.3 Process Flow Diagram............................................................................17
2.4 Conclusion......................................................................................................17

CHAPTER 3 MATERIAL BALANCE.................................................................18


3.1 Introduction...................................................................................................... 19
3.2 Overall Material Balance..................................................................................19
3.2.1 Material Balance over Centrifuge(CF)................................................... 25

i
3.2.2 Material Balance over Tray Dryer..........................................................26
3.2.3 Material Balance around the Multi Mill................................................. 27
3.3 Conclusion........................................................................................................27

CHAPTER 4 ENERGY BALANCE......................................................................28


4.1 Introduction...................................................................................................... 29
4.2 Energy Balance Across SSR............................................................................ 30
4.3 Conclusion........................................................................................................32

CHAPTER 5 PLANT UTILITIES........................................................................ 33


5.1 Introduction...................................................................................................... 34
5.2 Boiler Section................................................................................................... 35
5.3 Attachments to the Boiler.................................................................................36
5.4 Brine Chilling plant.......................................................................................... 37
5.5 Water chilling plant.......................................................................................... 38
5.6 Cooling Tower..................................................................................................38
5.7 Air Compressor................................................................................................ 38
5.8 Conclusion........................................................................................................39

CHAPTER 6 DESCRIPTION OF THE EQUIPMENT......................................... 39


6.1 Introduction...................................................................................................... 40
6.2 Stainless Steel Reactor..................................................................................... 41
6.3 Centrifuge.........................................................................................................41
6.4 Sparkler Filter...................................................................................................42
6.5 Multi Mill......................................................................................................... 43
6.6 Tray Dryer........................................................................................................ 43
6.7 Conclusion........................................................................................................44

CHAPTER 7 DESIGNING OF EQUIPMENTS.................................................. 45


7.1 Introduction...................................................................................................... 46
7.2 Design of Reactor.............................................................................................47
7.3 Design of Distillation Column......................................................................... 50
7.4 Design of Heat Exchanger................................................................................53
7.5 Mechanical Design for Agitator....................................................................... 56

ii
CHAPTER 8 PUMPS AND VALVES...................................................................59
8.1 Various pumps used in the plant...................................................................... 60
8.1.1 Centrifugal Pumps.................................................................................. 60
8.1.2 Diaphragm Pumps.................................................................................. 60
8.1.3 Vacuum pump.........................................................................................61
8.2 Various valves used in the plant.......................................................................62
8.2.1 Ball Valves..............................................................................................63
8.2.2 Globe valve.............................................................................................63
8.2.3 Plug Valves.............................................................................................64
8.3 Control Valve................................................................................................... 65
8.4 Piping................................................................................................................66
8.5 Conclusion........................................................................................................66

CHAPTER 9 HEALTH, SAFETY AND ENVIRONMENT............................... 67


9.1 Introduction...................................................................................................... 68
9.2 Safety in process plant......................................................................................68
9.2.1 Facilities for the handling the material and firefighting equipment....... 68
9.2.2 Safety related equipments .....................................................................69
9.2.3 Hazop of the plant ................................................................................. 69
9.2.4 Equipment Location According to the Wind Load Direction................ 70
9.2.5 Safety related Equipments, their Locations and Reasons.......................70
9.3 Pollution control measures............................................................................. 70
9.3.1 Water Pollution Control........................................................................71
9.3.2 Air Pollution Control............................................................................ 72
9.4 Conclusion………………………………………………..………………….72

CHAPTER 10 PLANT LAYOUT AND PLANT LOCATION...........................73


10.1 Introduction.................................................................................................... 74
10.1.1 Plant Layout........................................................................................74
10.1.2 Plant Location.....................................................................................74
10.2 Principle of Plant Layout................................................................................75
10.3 Factors for Plant Location............................................................................. 76
10.4 Drawing of Plant Layout.............................................................................. 77
10.5 Conclusion....................................................................................................78

iii
CHAPTER 11 COST ESTIMATION................................................................... 79
11.1 Introduction.................................................................................................... 80
11.2 Purchased Equipment Cost.............................................................................80
11.2.1 Based on MOC................................................................................... 80
11.3 Capital Cost.................................................................................................. 84
11.3.1 Fixed Capital Investment (F.C.I)...................................................... 85
11.3.2 Working Capital Investment (W.C.I)............................................... 86
11.4 Manufacturing Cost.................................................................................87
11.5 Profitability Analysis.............................................................................. 89
11.6 Conclusion.............................................................................................. 90

CHAPTER 12 CONCLUSION................................................................................. 91

CHAPTER 13 BIBLIOGRAPHY.............................................................................92

iv
LIST OF FIGURES

Figure Name Page


No. No.

1.1 Structure of Acotiamide HCl Trihydrate 2

2.1 Process Block Diagram of Acotiamide HCl Trihydrate 15

2.2 Process Flow Diagram of Acotiamide HCl Trihydrate 17

3.1 Material Balance across SSR 20

3.2 Material Balance across CF 25

3.3 Material Balance across Tray Dryer 26

5.1 Block Diagram of Boiler 35

7.1 Equilibrium curve of Methanol and Water 50

8.1 Block Diagram of Control Valve 65

10.1 Overall Plant Layout 76

LIST OF TABLES

Table Name Page


No. No.

1.1 Technical Competitors 4

1.2 Physical and Chemical Properties of Acotiamide Hcl 5


Trihydrate
2.1 Raw Material Supply 12

2.2 Cost of Raw Material 13

2.3 Physical and Chemical properties of raw material 14

3.1 Overview of Material Balance across SSR (X=100%) 22

v
3.2 Overview of Material Balance across SSR (X=86%) 24

3.3 Overview of Material Balance across CF 25

3.4 Overview of Material Balance across Tray Dryer 26

4.1 Molar Heat Capacity 29

4.2 Heat of Formation 31

5.1 Boiler Data 35

6.1 Detail Description of SSR 40

6.2 Detail Description of CF 41

6.3 Detail Description of Sparkler Filter 41

6.4 Detail Description of Multi Mill 42

6.5 Detail Description of Tray Dryer 43

7.1 Equilibrium data of Methanol and Water at different 49


temperatures

9.1 Classification of fire 68

11.1 Purchased Equipment Cost 83

11.2 Direct Cost Factor 84

11.3 Indirect Cost Factor 84

11.4 Direct Production Cost 87

11.5 General Expenses 87

vi
ABBRIVATIONS

MW Molecular Weight of Compound

O.D : Outside Diameter

I.D Inside Diameter

CAS Chemical Abstracts Service

IUPAC International Union of Pure and Applied Chemistry

Kg Weight in Kilograms

mm Length in Millimeter

m Length in Meter

cm Length in Centimeter

J Energy in Joules

cal Energy in Calories

K Temperature in Kelvin

W Power in Watts

L.M.T.D Logarithmic Mean Temperature Difference

H.T.C Heat Transfer Coefficient

TEMA Tubular Exchanger Manufacturers Association

SS Stainless Steel

MS Milled Steel

ETP Effluent Treatment Plant

Hp Horse Power

vii
NOMENCLATURE

ρ Density of Fluid, kg/m3

μ Viscosity of Fluid, g/cm.s

 Latent Heat of Vaporization, KJ/mol

τ Reaction Time, hr

m Mass Rate, kg/hr

M Mass of Solid, kg

V Volume of Liquid, lit or m3

v Velocity of Fluid, m/s

N Normality of Liquid, mole/lit

C Molar Concentration of Fluid, mole/lit

Cp Specific Heat Capacity of Fluid, KJ/kg.K

Q Amount of Heat, J

T Actual Temperature, ℃ or K

Tr Reduced Temperature, ℃ or K

Tc Critical Temperature, ℃ or K

H Heat of Formation, KJ/mol

Hr : Heat of Reaction, KJ/mol

t Temperature Difference

A, β Constants for Vaporization Data

K Reaction Constant, (concentration)1-n time-1

X Conversion

-rA Rate of Reaction

P Pressure, KPa

viii
θ Space Time, hr

R Gas Constant, lit.atm/mol.K

D Diameter, m

H Height, m

bw Width of Blade, mm

N Speed of impeller, rpm

σ Stress, kgf/cm2

E Modulus of Elasticity, kgf/cm2

Nre Reynolds Number

Np Power Number

P Power, hp

Τc Torque, kgf.m

Zp Section Modulus, cm3

Rb Radius of Blade, m

M Bending Moment, kgf.m

I Moment of Inertia, cm4

δ Maximum Deflection, cm

Pb Bearing Pressure, N/mm2

ix
CHAPTER 1
INTRODUCTION

1
1.1 History of Product
Acotiamide, a novel oral prokinetic drug, was produced by Zaria Pharmaceutical Co.
Ltd.(Tokyo,Japan) for treatment of patients with functional dyspepsia (FD).
Acotiamide hydrochloride is a gastroprokinetic drug that upgrades acetylcholine
discharge in the Enteric Nervous System (ENS) by means of muscarinic receptor
enmity and acetyl cholinesterase (ACheE) Inhibition. Dyspepsia is gotten from Greek
and actually signifies "awful processing" (dys=bad, pepsia=digestion). Functional
dyspepsia (FD) is a typical gastrointestinal issue characterized as manifestation based
conditions without natural malady. Side effects are ordered as postprandial misery
and epigastric torment disorders, which are related with disabled gastric convenience
and discharging. Gastric convenience and discharging are prompted by planning
motility of gastric fundus, body, and antrum, which are directed by complex sensory
systems including cholinergic neurons anticipated from dorsal engine core of the
vagus to the stomach.

1.2 IUPAC Name

N-[4[N-[2-(Diasoproylamino)ethyl]carbonyl]thiazole-2-yl]-2-hydroxyl-4,5-
dimethoxybenzamide hydrochloride trihydrate

1.3 Structure

O O .3H2O
H3C
S .HCl CH3
H3C NH
O NH
N N CH3
OH
O
H3C CH3

N-[4-[N-[2-(Diisopropylamino)ethyl]carbamoyl] thiazole-2-yl]-2-hydroxy-4,5-dimethoxybenzamide hydrochloride trihydrate

Figure 1.1 Acotiamide HCl Trihydrate Chemical Structure


ACOTIAMIDE HYDROCHLORIDE HYDRATE

C21H37ClN4O8S

2
1.4 Capacity of Product

 Total Capacity of Plant: 15 tons per annum.


 World wide capacity: 107 tons per annum.

1.5 Market Value of Product

 Acotiamide HCl Trihydrate: 20000 Rs./kg

1.6 Details of Product

 Acotiamide HCl Trihydrate is an expensive chemical; and is organic compound


that contains oneof the functional group of NH-HCl-3H2O
 Acotiamide HCl Trihydrate as final product is a white powder having light smell.

1.7 Commercial Competitors

 Kimia Bioscience Ltd.


 Enmennar Pharma Pvt. Ltd.
 Zaria Pharmaceutical Co. Ltd.

3
1.8 Technical Competitors

Table 1.1 Technical Competitors


Sr.no. Name of Equipment Technology Provider
1. Reactor GMM Production,
De Dietrich Process system,
Dyke Engi. Service.
Amod Engineering Works
2. Heat Exchanger(spiral) Keivion India Pvt. Ltd.
Transter India Ltd.
Heat Exchanger(plate) Transter India Ltd.

3. Centrifuge Joflo India Pvt. Ltd.

4. Centrifugal Pump Fluorolined Equipment Pvt. Ltd.


KSB Pumps Ltd.
Anticorrosive Equipment Pvt. Ltd

5. Storage Tank Chemtek fiber glass Industries.

6. Valve Delta, Baroda.

7. Pressure Gauge Baumer,


Honnywell

8. Cooling Tower Himgiri Technology

1.9 Applications

 It is a used for treatment of functional dyspepsia (FD).


 It targets Enteric Nervous System (ENS) by means of muscarinic receptor.
 It may help to improve your mood, appetite, and energy level as well as decrease
anxiety and insomnia related to depression.

4
1.10 Physical as well as Chemical Properties

Table 1.2 Physical and Chemical Properties of Acotiamide HCl Trihydrate

Chemical Formula C21H37ClN4O8S

Molecular Weight 541.057 g/mol

Appearance White to off-white powder

Physical State Solid

Odor Light

Density 0.729 g/cm3

Melting Point 180ºC-195ºC

5
1.11 Material Safety Data Sheet (MSDS)

Section 1: Product Identification

Chemical Name:
N-[4[N-[2-(Diasoproylamino)ethyl]carbonyl]thiazole-2-yl]-2-hydroxyl-4,5-
dimethoxybenzamide hydrochloride trihydrate
Chemical Formula: C21H37ClN4O8S
CAS No.: 773092-05-0
Relevant use of substance: Human Pharmaceutical
How it is Supplied: In form of Round White Tablets

Section 2: Hazard Identification

GHS Classification:
Acute toxicity, Oral (Category 4)
Skin corrosion/irritation (Category 2)
Serious eye damage/eye irritation (Category 2A)
Specific target organ toxicity-single exposure(Category 3),Respiratory system

GHS Label elements, including precautionary Statements

Pictogram:

Signal word: Warning


Hazard statement(s):
H302 Harmful if swallowed
H315 Causes skin irritation
H319 Causes serious eye irritation
H335 May cause respiratory irritation
Precautionary Statement(s):
P261 Avoid breathing dust/fume/gas/mist/vapours/spray.

6
P305+351+338 IF IN EYES: Rinse cautiously with water for several minutes.
Remove contact lenses, if present and easy to do. Continue rinsing.

Section 3: Composition, Information of Ingredients

Ingredient name: Acotiamide hydrochloride trihydrate


CAS number: 773092-05-0
Molecular Formula: C21H37ClN4O8S
Molecular Weight: 541.070

Section 4: First Aid Measures

In case of eye contact: Rinse thoroughly with plenty of water for at least 15 minutes
and consult a physician.
If inhaled: If breathed in, move person into fresh air. If not breathing, give artificial
respiration. Consult a physician.
In case of skin Contact: Wash off with soap and plenty of water for at least 15
minutes while removing contaminated clothing and shoes. Call a physician.
If swallowed: Never give anything by mouth to an unconscious person. Rinse mouth
with water. Consult a physician.

Section 5: Fire Fighting Measures

Suitable extinguishing media: Use carbon dioxide, dry chemical powder,


alcohol-resistant or polymer foam.
Special protective equipment for firefighters: Wear self-contained breathing
apparatus for fire-fighting if necessary.

Section 6: Accidental Release Measures

Personal precautions: Use personal protective equipment. Avoid breathing vapors,


mist or gas. Ensure adequate ventilation. Evacuate personnel to safe areas.
Environmental precautions: Do not let product enter drains.

7
Methods and Materials for containment and cleaning up Absorb spills on sand or
vermiculite and place in closed container for disposal.

Section 7: Handling and Storage

Precautions for safe handing: Avoid contact with skin and eyes. Avoid inhalation of
vapor or mist. Wash thoroughly after handling.
Conditions for safe storage: Keep container tightly closed in a cool, dry,
well-ventilated place.
Recommended storage temperature: Store at 0-8 °C

Section 8: Exposure Controls/Personal Protection

Contains no substances with occupational exposure limit values.


Engineering Controls: Use only in a chemical fume hood.
Personal Protective equipment: Wear chemical-resistant gloves, safety googles.
General Hygiene measures: Handle in accordance with good industrial hygiene and
safety practice. Wash thoroughly after handling. Wash contaminated clothing before
reuse.

Section 9: Physical and Chemical Properties

Appearance: White to Off White Powder


Odor: Light
Physical State: Solid
Density: 0.729 g/cm3
Melting Point: 180ºC-195ºC

Section 10: Stability and Reactivity

Chemical stability: Stable under recommended storage conditions.


Materials to avoid: No data available
Conditions to avoid: No data available

8
Possible hazardous combustion products: carbon oxides; hydrogen chloride;
nitrogen oxides; sulfur dioxide.

Section 11: Toxicological Information

No Data

Section 12: Ecological Information

No Data

Section 13: Disposal Considerations

Arrange disposal as special waste, by licensed disposal company, in consultation with


local waste disposal authority, in accordance with national and regional regulations.

Section 14: Transportation Information

Non-hazardous for air and ground transportation. Or not available.

Section 15: Regulatory Information

Indication of danger: No data


Risk Statement: No data
Safety Statement: In case of contact with eyes, rinse immediately with plenty of
water and seek medical advice. Wear suitable gloves and eye/face protection

Section 16: Other Information

Revision: 2
Revision Date: Update: 2017-12

9
The above information is believed to be correct at the date of its publication but does
not supposed to be all-inclusive and shall be used only as a guide. Individuals
receiving the information must exercise their independent judgment in determining its
appropriateness for a particular purpose.

1.12 Conclusion

This introductory chapter gives a general overview of the product. We got the
information about the history of the product, the IUPAC name, and the structure of
the compound. Alongside, we also discussed the names of Technical and Commercial
competitors and various properties of the product. In the end, we got to know about
the MSDS of the product.

10
CHAPTER 2
SELECTION OF PROCESS

11
2.1 About Raw Materials

2.1.1 Raw Material Supply

Table 2.1 Raw Material Supply

Sr.No. Chemical name Molecular Manufacturer


Formula
1. R-1 C10H11O4Cl Merck

2. R-2 C6H9O2N2S Merck

3. TEA C6H15N Merck

4. R-3 C8H20N2 Merck

5. Water H2O Prepared in


laboratory
6. Hydrochloric acid HCl Merck

7. Thionyl chloride SOCl2 Sigma Aldrich

8. Toluene C7H8 Sigma Aldrich

9. Isopropyl alcohol C3H8O Sigma Aldrich

2.1.2 Transportation

 Company is situated in an area where good number of industries are available, so


raw material transportation is easily done through national highway 8 joining
Dabhasa to Vadodara via Padra. Vadodara being the main city is just 30 km from
Dabhasa making the transportation more convenient.

12
2.1.3 Cost of Raw Materials
Table 2.2 Cost of Raw Materials

Sr.No. Chemical name Molecular Cost/kg


Formula (Rs.)

1. R-1 C10H11O4Cl 6122.7454

2. R-2 C6H9O2N2S 3461.525

3. TEA C6H15N 200

4. R-3 C8H20N2 18207.6215

5. Water H2O 22

6. Hydrochloric acid(35%) HCl 5

7. Thionyl chloride SOCl2 30

8. Toluene C7H8 45

9. Isopropyl alcohol(99%) C3H8O 120

13
2.2 Physical and Chemical Properties of Raw Materials

Table 2.3 Physical and Chemical properties of raw material

Sr.no Chemical Density Sp.Heat Viscocity Boiling Vapor


(Kg/m3) (KJ/KgK) (Pa Point Pressure(kP
s)*106 (0C) a)
(At 250C)
1 SOCl2 1683 1.017 600 74.6 15.7

2 HCl 1490 0.798 311 -85.05 25


3 SO2 1383 1.37 403 -10 350
4 Triethyl 728 - 368 90 7.0
amine
5 IPA 786 0.212 2400 82 44
6 Water 996 4.18 798 100 3.1628

7 Methanol 768.3 2.53 544 64.5 12.7

8 Toluene 867 1.717 583 110.6 2.8

9 R-3 798 1.23 - 169 57

14
2.3 Detailed Process Description

2.3.1 Process Block Diagram

CTA-1 + R-3 + (HCl +H20)

SSR

CENTRIFUGE

TRAY
DRYER

MULTI
MILL

PACKAGING

Figure 2.1 Process Block Diagram of Acotiamide HCl Trihydrate

15
2.3.2 Process Description

STEP-1: R-1 to CTA-1

This stage involves the acid chloride formation of R-3 by using thionyl-chloride in
toluene at 80-85 C for 1-2 hrs to get intermediate (P-1). The intermediate (P-1) is
condensed as Insitu with R-2 in presence of TEA at 80-85 C for 12-14 hrs to form
CTA-1. After completion of reaction filtered reaction at NMT 35 C. Wet cake leached
in water and aqueous sodium carbonate solution and washed with water and dried wet
cake under vacuum to get CTA-1.
R-1 + SOCl2 P-1 + HCl +SO2 R-2 + TEA CTA-1 + TEA*HCl

STEP-2 : CTA-1 to CTA-crude

CTA-1 and R-3 are reacted at 125-13C C for 9-13 hrs. After completion of the
reaction, the direct hydrochloride salt of Acotiamide base was prepared by addition of
HCl at 20-30 C followed by methanol charging in the reaction mixture. The Product
isolated by filtration at 0-5 C and washed with methanol with methanol dried to get
Acotiamide hydrochloride hydrate crude (CTA crude).
CTA-1 + R-3 + HCl + H2O CTA-crude + CH3CH2OCH

STEP-3: Acotiamide hydrochloride hydrate crude(CTA-crude) to Acotiamide


hydrochloride Trihydrate(CTA-pure)

Acotiamide hydrochloride hydrate crude was purified in 20% aqueous IPA solution at
80-85 C followed by charcolization product filtered at 15-20 C and washed with 20%
aqueous IPA solution and then dried at not more than 35 C under vacuum to get
Acotiamide hydrochloride Trihydrate.
CTA-crude + 2H2O CTA-pure(Acotiamide HCl Trihydrate)

16
2.3.3 Process Flow Diagram

Figure 2.2 Process Flow Diagram of Acotiamide HCl Trihydrate

2.4 Conclusion

This chapter gives detail about selection of process including the raw material
specification and the cost of the product.. We conclude that various physical and
chemical properties of raw material are distinctive. Also, the process block diagram,
process flow diagram and the process description of the product is noted.

17
CHAPTER 3
MATERIAL BALANCE

18
3.1 Introduction

Material flow rates for the various streams are determined based on desired plant
capacity using material balance calculation.

This chapter includes material balance of Reactor, Centrifuge separator,Tray Dryer


and Multi Mill. Material balance gives us an idea about the quantity of feed entering
and the product leaving along with unreacted material of particular equipment. It also
helps us to determine the composition in the feed and in the product which is
unreacted for given conversion.

For conversion, the quantity of reactant reacted is identified. The material balance is
governed by Law of Conservation of Mass, viz. Input - Output = Accumulation.

3.2 Overall Material Balance

Acotiamide HCl Trihydrate production seems a single step reaction, but however it
takes place in three steps as shown below:

(i) R-1 + SOCl2 P-1 + HCl +SO2 R-2 + TEA CTA-1 + TEA*HCl
(ii) CTA-1 + R-3 + HCl + H2O CTA-crude + CH3CH2OCH
(iii) CTA-crude + 2H2O CTA-pure(Acotiamide HCl Trihydrate)

Thus the overall Reaction is,

CTA-1 + R-3 +HCl +3H2O IPA CTA-Pure + CH3CH2OCH

A+B+C+D IPA
E+F

19
Where,
A = CTA-1
B = R-3; C10H11O4Cl
C = Hydrochloric Acid; HCl
D = Water; H2O
E = CTA-pure; C21H27ClN4O8
F = Methyl Ethyl Ketone; CH3CH2OCH
G = Iso Propyl Alcohol; C3H8O

Since the data of the company is confidential, batch size is assumed.


Let, the batch size = 90 kg
ORIGINAL BASIS: Batch Capacity = 90 kg/batch
But,
Actual Capacity = Original Capacity*(1.Roll Number) kg/batch
⸫ Actual Capacity = 90*(1.66) kg/batch
⸫ Actual Capacity = 150 kg/batch
NEW BASIS: Batch Capacity = 150 kg/batch
Here, we also assume that conversion is 100%

 Material Balance over Stainless Steel Reactor(SSR):

CTA-1→ → CTA-pure
HCl→
R-3→ SSR
H2O→
→CH3CH2OCH

Figure 3.1 Material Balance across SSR

20
(1) Moles of CTA-pure to be produced = 150/541.052
= 0.277kmol

(2) Kg of CTA-1 needed = M.W. of CTA-1*moles of CTA-pure


= 366.39*0.277
= 101.49 kg

(3) Kg of HCl needed= M.W. of HCl*moles of CTA-pure


= 36.46*0.277
= 10.09 kg

(4) Kg of H2O needed = M.W. of H2O*moles of CTA-pure


= 3*18*0.277
= 14.955 kg

(5) Kg of R-3 needed = M.W. of R-3*moles of CTA-pure


= 144.26*0.277
= 39.96 kg

(6) Kg of CH3CH2OCH produced = M.W of CH3CH2OCH*moles of CTA-pure


= 60.1*0.277
= 16.647 kg

21
Summary Table

Table 3.1 Overview of Material Balance across SSR (X=100%)

CHEMICALS INLET (KG) OUTLET (KG)


A 101.49 0
B 39.96 0
C 10.09 0
D 14.955 0
E 0 150
F 0 16.647
Total 166.647 166.647

22
Now, Let us assume that conversion is 86%

(1)1 mol of CTA-1= 0.86 mol of CTA-pure


⸫ Mol of CTA-pure produced for 86% conversion = 0.277/0.86

= 0.322 kmol

(2) Kg of CTA-1 needed = M.W. of CTA-1*moles of CTA-pure


= 366.39*0.322
= 117.97 kg

(3) Kg of HCl needed = M.W. of HCl*moles of CTA-pure


= 36.46*0.322
= 11.74 kg

(4) Kg of H2O needed = M.W. of H2O*moles of CTA-pure


= 3*18*0.322
= 17.388 kg

(7) Kg of R-3 needed = M.W. of R-3*moles of CTA-pure


= 144.26*0.322
= 46.45 kg

(8) Kg of CH3CH2OCH produced = M.W of CH3CH2OCH*moles of CTA-pure


= 60.1*0.322
= 19.35 kg

23
(9) Kg of unreacted CTA-1 = 117.97-101.49 = 16.48 kg

(10) Kg of unreacted R-3 = 46.45-39.96 = 6.49 kg

(11) Kg of HCl not consumed = 11.74 - 10.09 = 1.88 kg

(12) Kg of H2O not consumed = 17.388 - 14.955 = 2.433 kg

Summary Table

Table 3.2 Overview of Material Balance across SSR (X=86%)

CHEMICALS INLET (KG) OUTLET (KG)


A 117.97 16.48
B 46.53 6.49
C 11.74 1.88
D 17.388 2.433
E 0 150
F 0 19.35
Total 193.63 193.63

Note: F=Methyl Ethyl Ether is a highly volatile compound, so on basis of volatility is


separated from the main reactor at the the operating temperature.

24
3.2.1 Material Balance over Centrifuge(CF)

In CF, ML is separated from solid wet cake. Here, the unreacted reactants are
dissolved in IPA and that IPA containing ML is separated out. Some part of IPA
going into the product is known as wet cake.
The final wet cake which is coming out from CF will contain about 4% of IPA part
which is sent to Tray Dryer for drying.

Slurry→ CF →Wet Cake(Product)


Mother Liquor (ML)

Figure 3.2 Mass Balance across CF

Summary
Table 3.3 Overview of Material Balance across CF

CHEMICALS INLET (KG) OUTLET(KG) OUTLET (KG)


WET CAKE ML
A 16.48 0 16.48
B 6.49 0 6.49
C 1.88 0 1.88
D 2.43 0 2.43
E 150 150 0
F 0 0 0
G 550 22 528
Total 727.28 172 555.28

25
3.2.2 Material Balance over Tray Dryer

Moisture

Wet Product → Tray Dryer → Acotiamide


From CF HCl Trihydrate

Figure 3.3 Mass Balance across Tray Dryer

The wet product contains 2% moisture and remaining is pure solid product.
Solid in wet solid = Solid in product.
Moisture in final product = NMT 0.7%
So, in final product moisture content = (150*0.7)/100=1.05 kg
IPA removed with use of Tray Dryer = 22-1.05 = 20.95 kg

Summary

Table 3.4 Overview of Material Balance across Tray Dryer


CHEMICAL INLET(KG) OUTLET(KG) MOISTURE(KG)
E 150 150 0
Moisture 22 1.05 20.95
TOTAL 172 151.05 20.95

3.2.3 Material Balance around the Multi Mill

Around Multi Mill there is no need of material balance as whatever goes in, the same
product comes out with small particle size. However, there may be material loss due
to dry powder product getting stuck on the screens and the blades as well as the walls
of the Multi Mill.

26
3.3 Conclusion

We conclude that the material balance is governed by Law of Conservation of Mass,


viz. Input - Output = Accumulation. The material balance of Reactor, Centrifuge
separator and Vacuum Tray Dryer was carried out which gave us information about
the quantity of feed entering and the product leaving along with unreacted material of
particular equipment.

27
CHAPTER 4
ENERGY BALANCE

28
4.1 Introduction

Energy Balance is done based on Heat of Reaction, Heat Capacities, Expected


Temperatures, and Pressure at various points to calculate amount of heating and
cooling needed at various places and to size equipments.
In this chapter, energy balance of Reactor at various stages and dryer is given. There
us one major conservation law which provides an additional equation called Law of
Conservation of Energy. E denotes the entire amount of energy in system.

Law of Conservation of Energy:


Ein - Eout = Eaccumulated
Kinetic Energy and Potential Energy are generally very small compared to the
enthalpy, except in case of very rapid flow or when there are no significant
temperature changes occurring in the system. Therefore, they are often neglected in
performing energy balances.
Here Cp values are found using Kopp’s Law and Heat of Formation is found using
group contribution method.

Table 4.1 Molar Heat Capacities

CHEMICAL MOLAR HEAT CAPACITY


(KJ/mol K)

CTA-1 395.70

R-3 177.44

HCl 29.20

H2O 75.348

CTA-pure 405.78

CH3CH2OCH3 91.35

29
4.2 Energy Balance Across SSR

∆T = 85℃ - 60℃ = 25 ℃

Heat in with feed,


QCTA-1 = mCp∆T
= 0.322*395.70*25
= 3284.31 kJ

QR-3 = mCp∆T
= 0.322*177.44*25
= 1428.39 kJ

QHCl = mCp∆T
= 0.322*29.20*25
= 235.06 kJ

QH2O = mCp∆T
= 0.322*75.348*25
= 606.55 kJ

Heat out with product,


QAcotiamide HCl Trihydrate = mCp∆T
= 0.322*405.78*25
= 3266.529 kJ

QMethyl Ethyl Ether = mCp∆T


= 0.322*91.35*25
= 735.36 kJ

30
Table 4.2 Heat of Formation
MATERIAL HEAT OF FORMATION (KJ/mol)
CTA-1 273.2
R-3 95.52
HCl -92.3
H2O -285.83
CTA-pure -329.7
CH3CH2OCH3 -184.10

∆Hr = Reactant - Product


= (273.2 + 95.52 + (-166.10) + 3(-285.83)) - ((-329.7) + (-184.10))
= 1168.67 KJ/mol

Qsupply = Qin -Qout - ∆Hr


= 5554.31 - 4001.88 - 1168.67
=383.76 KJ/mol

Water is used as a cooling media.


Temperature of Water in = 15℃
Temperature of Water out = 23℃
Now,
Qsupply = mCp∆T
⸫ 383.76 = m * 4.18 * 8
⸫ m = 11.47 mol
⸫ Kg of Water = m * 18
= 11.47 * 18
= 206.46 kg

Mass Flow = Kg of Water / Batch Time


= 206.46 / 15
= 13.764 kg/hr

31
4.3 Conclusion

We conclude that the energy balance is governed by Law of Conservation of Energy:


Ein - Eout = Eaccumulated. Energy Balance was done based on Heat of Reaction, Heat
Capacities, Expected Temperatures, and Pressure at various points to calculate
amount of heating and cooling needed at various places and to size equipment.

32
CHAPTER 5
PLANT UTILITIES

33
5.1 Introduction

Just as any plant requires raw materials to produce the final product, it equally
requires various other services called Utilities for smoothly carrying out the processes.
Utilities are neither a product nor a reactant, but they are required for maintaining
adequate conditions of manufacturing unit. Thus, Utility area is an important section
of a plant which is house to various boilers, large compressors, cooling towers, water
treatment plants etc. Plant also requires electric power, so Power Plants are also
considered as a part of Utilities.

The bad management of of utilities can make even the most profitable processes
unprofitable. Utilities can be used to maintain processing parameters like pressure,
temperature, etc., without which it is impossible to carry out the process.

Some properties of Utilities are as follows:


 They are generally reusable.
 Their composition doesn’t change.
 They cannot be stocked, so regular supply is must.
 They must be readily available.

The following are the Utilities present in the plant:


 Steam
 Portable Water
 Power Supply
 Chilling Water
 Cooling Tower

34
5.2 Boiler Section

The steam is supplied to the plant from boiler house. This steam is used for heating
purpose and in drying. The boiler used here is Fire Tube Boiler. The specification of
the boiler used in the company is tabulated below:

Table 5.1 Boiler Data

Company Thermax
Type of Boiler Packed Boiler (Fire Tube Boiler)
Type of Heating Gas Fired (3 pass)
Pressure 10.54 kg/cm2
MOC of Shell Mild Steel
MOC of Tube SS
Heating Medium Coal
Capacity 3 ton/hr
Insulating Material (inner wall) Fire Bricks
Insulating Material (outer wall) Glass Wool

Softening
Raw Water Filter Unit Point

Feed
Boiler
Water

Figure 5.1 Block Diagram of Boil

35
5.3 Attachments to the Boiler

1. Main Stop Valve:


Function: it is used to stop the supply of steam to plant if necessary

2. Air Vent Valve:


Function: To avoid the formation of vacuum. It comes in to action when
Condensation of steam occurs & it is an automatic operation.

3. Manhole:
Function: it is used to clean the tubes & shell when the plant is not in operation.
Any defect in the boiler can be easily detected.

4. Water level indicator:


Function: level of water is indicated by means of this indicator.

5. Feed Check Valve:


Function: used to supply the water to the boiler according to need from Tanks.

6. Centrifugal Pump:
Function: it is used to charge water to the boiler.

7. PRV system:
Function: it is used for reducing pressure of the steam generated in the boiler. It is
known as Pressure reducing valve system. PRV system is used at the inlet (for
controlling gas pressure) and outlet (of the boiler to achieve required pressure of
steam).The PRV system is generally having diaphragm valve, strainer, etc. The cost
of PRV system is approximately 2.8 lacks.

8. Softening of Feed Water


Water available to boiler contains carbonates and bicarbonates of heavy metals. Leads
scaling of the tubes. So water must be softened. For this purpose we make the used of

36
water treatment plant having a vessel containing packing of a rash high rings, which
softens the water passing through it. After using it for sometime it is required to wash
the packing. For washing, salt solution is passed in reversed direction, which removes
all the impurities from the packing thus make it reusable.

5.4 Brine Chilling plant

Temperature requirements below -7C cannot be supplied by chilled water, so to fulfill


this requirement of cooling chilled brine is used. Composition of this chilled brine is
generally 40% MEG and 60% water, chilled brine can have temperature up to -20C.
this temperature is achieved by compression and expansion cycle of ammonia
There are five brine chilling units on the site three of them are of 72 TR one is of 80
TR and a newly installed unit is of 100 TR capacity.

5.5 Water chilling plant

There are some unit operations which require chilling water to accomplish their
operations and this chilled water is supplied through 3 units of water chilling plants
two of 80 TR capacity and another is of 150 TR capacity. Chilled water is produced
by the ammonia compression and expansion cycle.

5.6 Cooling Tower

Cooling water is an essential requirement for most of the heat exchangers as cooling
medium and in some unit operations and processes to maintain the temperature
induced draft types of cooling towers are there in the plant. There are total four
number of cooling towers are located on site. Two of them having 800 TR capacity
one is of 1000 TR and the last one is having 1200 TR capacity.

37
5.7 Air Compressor

Air is an essential requirement of the industry because there are many air operated
valves and number of safety equipment such as breathing apparatus requiring an air
supply in large amount. This is supplied by air compression unit having 4
compressors two of them are in standby mode having supply pressure of 5 kg/cm2
whereas most of the control valves are being operated at 3.5 Kg/cm2 pressure and the
process air requirement is also supplied by this compression unit.

5.8 Conclusion

We conclude that Utility area is an important section of a plant which is house to


various boilers, large compressors, cooling towers, water treatment plants etc.
The bad management of of utilities can make even the most profitable processes
unprofitable. Utilities are used to maintain processing parameters like pressure,
temperature, etc., without which it is impossible to carry out the process.

38
CHAPTER 6
DESCRIPTION OF THE EQUIPMENT

39
6.1 Introduction

Numerous equipment are involved in the construction of any plant. After selection
process it becomes inevitable to decide the equipment necessary to accomplish the
process.
Suitable MOC is decided according to the fluid to be handled considering their nature,
properties, corrosion, fouling and reactivity with their material of the equipment. The
MOC should be selected which is capable enough to withstand these conditions and
work efficiently getting damage and at the same time providing maximum conversion
and yield.

6.2 Stainless Steel Reactor

Table 6.1 Detailed Description of SSR


Type of Vessel Closed Jacketed

MOC SS 316

Shell Capacity 1000 L

Volumetric Capacity 1100 L

Agitator Blade Turbine Type

Jacket Pressure 3 to 3.2 kgf/cm2

Diameter 1700 mm

Length 2080 mm

Technology Amod Engineering Work

40
6.3 Centrifuge

Table 6.2 Detailed Description of CF


Type Vertical Basket Centrifuge

Capacity 300 kg

MOC SS 316

RPM Maximum 900

Motor Hp 15 Hp

Technology Joflo India Pvt. Ltd.

6.4 Sparkler Filter

Table 6.3 Detailed Description of Sparkler Filter


MOC Mild Steel

Lining Rubber Lining

Plate Size 48”

Filter Cloth Alkali-cloth

41
6.5 Multi Mill

Table 6.4 Detailed Description of Multi Mill

50 Kg to 200 Kg per hour depending on the product


Output Reduction
and size required

12 nos. with knife and impact edges & 2 scraper


Beater
blades

Motor 3 hp, 2800 RPM, 415 V, 50Hz, 3 PH, AC

Screen Area (mm) 495 x 135 (66825 sq. mm)

(I) Perforated 0.5 to 25 mm


Screen size:
(II) Wire mesh 4 to 100 mesh

Rotor Speed 750, 1500, 2300, 3000 RPM

Dimensions (mm) 1230 (L) x 760 (W) x 1700 (H1)

Rotor Assy. Diameter 250 mm

Net Weight (Kg) 250 Kg

Technology Neelam Industries

42
6.6 Tray Dryer

Table 6.5 Detailed Description of Tray Dryer

MODELS TD-48

Loading capacity 45 Trays(50-500 kg)

WDH
External Dimension in mm
1980X1020X1880

Internal Dimension In mm 1020 X930 X1830

No of Doors One

No of Blowers One
No of motors/H.P.3 PHASE 415
1/1 H.P.3 phase 415 volts
VOLTS.
Electrical Heating Load
9kw/15kw/18kw
for100°C/200°C/300°C

Steam Heater No. of coils. 2

Steam Pressure 3.3 kg/cm2

Steam consumption 60 LBS/hr

Insulation
50/75/75
in mm100°C/200°C/300°C

No of Trays 20

Tray Size 812X 406 X 31

Trolley Dimension 840X960X17

Technology Thermax

43
6.7 Conclusion

From this chapter we conclude that suitable MOC is to decided according to the fluid
to be handled considering their nature, properties, corrosion, fouling and reactivity
with their material of the equipment. The MOC should be selected which is good
enough to withstand these conditions and work efficiently getting damage and at the
same time providing maximum conversion and yield. The important selected
equipment are to be designed in the next chapter.

44
CHAPTER 7
DESIGNING OF EQUIPMENTS

45
7.1 Introduction

The processing, storage, or transportation of any raw material, product or utility


requires specific equipment to serve its purpose. These equipment are to be designed
keeping in mind optimum conditions of the process, its residence time and its
orientation to get maximum yield.

Designing is the most creative work carried out by Chemical Engineer. Equipment
Designing is basically divided in two parts:
(i) Process Design
(ii) Mechanical Design

Process design is a basic design and it is done by Chemical Engineers which includes
calculations of volume and residence time in case of Reactors, Number of Stages,
Feed Location, Design of down comer, weir design in case of a distillation column,
overall heat transfer coefficient, dirt factor, and pressure drop calculations in case of
Heat Exchanger and NPSH calculation in case of pump design.
Mechanical design deals with the calculations of height, daimater, thickness of shell,
thickness of head, thickness of nozzles, flanges, number of bolts and calculation for
supports.

Thus design of any equipment is the one of the main aspect in the industry. Somewhat
over design is provided by the design engineers considering the safety aspect but too
much over design is also unfavorable.

46
7.2 Design of Reactor

Data Given:
XA=0.86 (assumed value)
Density of CTA-1 = 1.34 g/cm3
M.W. of KSM 01 = 366.39 kg/kmol
Mass of KSM 01 = 117.97 kg
Batch Time = 15 hr.

Reaction:
CTA-1 + R-3 +HCl +3H2O IPA
CTA-Pure + CH3CH2OCH

A+B+C+D IPA
E+F

Where,
A = CTA-1
B = R-3; C10H11O4Cl
C = Hydrochloric Acid; HCl
D = Water; H2O
E = CTA-pure; C21H27ClN4O8
F = Methyl Ethyl Ketone; CH3CH2OCH
G = Iso Propyl Alcohol; C3H8O

Order of Reaction = 2
Rate Constant, k = unknown (mol/lit-hr)-1
But we know that batch time in this process = 15 hr.

Initial volume of CTA-1 at time t=0


NAO = mass of CTA-1 / M.W. of CTA-1
= 117.975 / 366.39
= 0.321 Kmol

47
Volume of CTA-1,
V = mass/density
= 117.97 / 1.34
= 0.088 m3

Initial concentration of CTA-1,


CA = NAO / V
= 0.321 / 0.088
= 3.64 mol/lit

Now,
τ = 15 hr.
τ / CAO = XA / -rA
-rA = 0.0157 mol/lit hr

Rate of Reaction -rA = K CA2 (⸪ Second order reaction)


We know, CA = CAO(1-XA)
⸫ -rA = kCAO2(1-XA)2
⸫ 0.0157= k * 3.642 * (1-0.86)2
⸫ k = 6.04*10-4 (mol/lit hr)-1

Summary of Process Design of SSR


Conversion = 86 %

Rate of Reaction = 0.0157 mol/lit hr

Order of Reaction = 2

Rate Constant = 6.04*10-4 (mol/lit hr)-1

48
7.3 Design of Distillation Column

Methanol is highly soluble in water so both are separated by fractional distillation


process. It is a sieve column tray located at SRU Unit.
Here,
We assume that feed rate = 250 kmol/hr
Feed mole fraction, XF = 35 mol% methanol
Distillate mole fraction, XD = 96 mol% methanol
Bottom mole fraction, XB = 2 mol% methanol
Operating Pressure = 1 bar

Overall Material Balance,


F=D+B
⸫ 250 = D + B … (1)

Also,
FXF = DXD + BXB
⸫ (250)(0.35) = D(0.96) + B(0.02) … (2)

Solving (1) and (2) we get,


D = 87.77 kmol/hr
B = 163.23 kmol/hr

Table 7.1 Equilibrium data of Methanol and Water at different temperatures

X 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Y 0 0.42 0.58 0.66 0.73 0.78 0.82 0.87 0.91 0.96 1.0
T(℃) 100 87.7 81.7 78 75.3 73.1 71.2 69.3 67.6 66 64.5

49
Here, assume that feed is at saturated liquid condition. Therefore from q-line equation,
q=1

Figure 7.1 Equilibrium curve of Methanol and Water plotting number of stages

As shown in the graph of Y vs X, q-line, Top Operating Line, Bottom Operating Line
are plotted and number of stages are estimated.
At the minimum reflux ratio maximum number of theoretical stages are observed. So,
the top operating line passes through interception of equilibrium curve and q-line.

Gradient of Top Operating Line = (0.96 - 0.7) / (0.96- 0.35)


= 0.426

50
Rmin / (Rmin + 1) = 0.426
⸫ Rmin = 0.742

R = 1.25*Rmin
⸫ R = 1.25(0.742)
⸫ R = 0.9275

Slope of Top Operating Line = R / (R + 1)


= 0.9275 / (0.9275 + 1)
= 0.481

Top Operating Line Equation: Y = 0.481X + 0.498

As we can see from the graph,


Total number of stages = 13
There is total condensor and a partial reboiler. We know that total condensor doesn’t
act as an equilibrium stage, but partial reboiler act as equilibrium stage.
⸫ Number of theoretical stages = 13-1 = 12

Let us assume that column efficiency = 80%


0.8 = (Number of Ideal Stages) / (Number of Actual Stages)
⸫ 0.8 = 12 / (Number of Actual Stages)
⸫ Number of Actual Stages = 15

Now,
Hs = Tray Spacing = 0.45 m
∆H = 0.5 meter each for liquid hold up and vapor disengagement. Take ∆H = 1 m.
ts = Plate Thickness = 5 mm
Nact = Number of Actual Stages = 15
Hc = Height of the Column

Height of the column(Hc) can be estimated from the below design equation:
Hc = (Nact - 1)Hs + ∆H + ts

51
= (15 - 1)(0.45) + (1) + (0.005)(15) = 7.375 m
XF = 0.35 corresponds to 6th stage on the graph. So the feed tray location is estimated
as below:
Feed Tray Location = (Stage which corresponds to XF) / (Column Efficiency)
= 6/0.8
= 7.5
⸫ The Feed Tray Location = 8th plate.

7.4 Design of Heat Exchanger

Methanol is heated and gets converted into vapour above 67℃, so by help of Heat
Exchanger it is to be condensed. Water is used as a coolant to condense hot Methanol.
Overall Heat Transfer Coefficient (U) for this system is 400 W/m2K

Available Data (For Methanol):

Methanol flow rate = 600 kg/hr


Boiling Point of Methanol = 64.5℃
Mass of Methanol, m= 600 kg
Latent heat of Methanol, λm = 0.2716 kcal/kg
Specific heat of Methanol, Cp = 0.5 kcal/kgK
Methanol(vapour) input temperature, T1 = 75℃
Methanol output temperature, T2 = 37℃

Available Data (For Water):

Water flow rate = 1 kg/hr


Boiling Point of Water = 100℃
Specific Heat of Water = 1 kcal/kgK
Water inlet temperature, t1 = 32℃
Water outlet temperature, t2 = 36℃
Water flow rate = w kg/hr

52
Heat Load on Heat Exchanger(Q) is a function of Latent heat and Sensible heat.

⸫ Q = Latent heat of Methanol + Sensible heat of Methanol


= mλm + mCp∆T
= [((600*0.2716) + (600*0.5 *(75-37))]
= 162.96 +11400
= 11562.96 kcal/hr.

There will be some amount of heat loss from the system. Assume that the heat loss is
around 6%.

⸫ Qloss = 0.06*Q
= 0.06*11562.96
= 693.77 kcal/hr

⸫ Qtotal = Q + Qloss
= 11562.96 + 693.77
= 12256.73 kcal/hr.

Now, Cooling water flow rate required

Q’ = wCp ∆T
⸫ 12256.73 = w*1*4
⸫ w = 3064.18 kg/hr
= 0.8511 kg/s

Logarithmic Mean Temperature Difference(LMTD) calculation:

T1 = Vapor inlet Temperature = 75℃


T2 = Condensate Temperature= 37℃
t1 = Cooling Water Inlet Temperature = 32℃
t2 = Cooling Water outlet Temperature = 36℃

53
LMTD = [(T1 – t1 ) – (T2 – t2 )] /ln[(T1 – t1 ) / (T2 – t2 )]
= [(75 – 36) - (37 - 32)] / In [(75- 36)/(37- 32)]
= 11.166℃

R = (th1 –th2)/ (tc1 - tc2)


= (T1 – T2)/(t1 – t2)
= (75 – 37)/(36 – 32)
= 9.5

S = (tc2 – tc1) / (th1 – tc1)


= (t1 – t2) /(T1 – t2)
= (36 – 32) / (75 – 32)
= 0.0930

From LMTD correction factor graph for R = 9.5 & S= 0.09


Correction factor, F = 0.95

∆Tm = LMTD*F
= 11.166*0.95
= 10.607℃

U = 400 W/m2K
= 95.6 kcal/ hr m2 K

Q” = U A ∆Tm
Area of Heat transfer, A = Q / (U * ∆Tm )
= 12256.73 / (95.6 *10.607)
= 12.087 m2

Assume 20 mm inside diameter and length 4m of the tubes are used.

Area of Heat Exchanger, A = π * d* L*Nt


No. tubes required, Nt= A /π* d* L

54
= 12.087 / (π *0.020* 4)
= 48.11 Nos.
⸫ Nt = 50 Nos.

7.5 Mechanical Design for Agitator

Diameter of agitator, Da = Diameter of reactor/2 = 1.2/2 = 0.6 m = 600 mm


Length of agitator shaft between bearing and agitator, L = 2.1 m = 210 mm
Width of Blade, bw = 120 mm
Number of baffles at tank wall = 4
MOC of Shaft and Agitator blade is IS-2062 Grade ST 42-W

Ultimate tensile stress = 4200 kgf/cm2


Yield Stress = 2300 kgf/cm2
Maximum Allowable Shear Stress in Shaft = 550 kgf/cm2
Modulus of Elasticity, E = 19.5 * 105 kgf/cm2
Power required for motor = 7.5 hp

Continuous average torque is given by,


τc = hp * 75 * 60 / (2 * π * N)
Assume N = 120 rpm
τc = 7.5 * 75 * 60 / (2 * π * 120)
= 46.65 kgf.m

Maximum possible torque in agitation system at start up condition is give by,


τm = 1.5 to 2.5 τc
Let us make m = 2 * τc
= 2 * 46.65
= 93.31 kgf.m

55
Maximum shear stress created in shaft,
fs = τm / Zp
where, Polar sectional modulus for circular shaft, Zp = π d3 / 16
⸫ 550 = (93.31 * 100) / ( π d3 / 16)
⸫ d3 = 86.44 cm3
⸫ d = 4.21 cm

Bending Moment,
M = Fm * L
Fm = m / (0.75 * Rb)
where, Rb = Radius of Blade = (Da/2) = 600/2 = 300 mm
Fm = 93.31 * 1000 / (0.75 * 300)
= 414.71 kgf

M = Fm * L
= 414.71 * 2.1
= 870.89 kgf.m

Me = 0.5 (M + (M2 + τm2)0.5)


= 0.5 (870.89 + (870.892 + 93.312)0.5)
= 873.38 kgf.m

Stress created by equivalent bending moment, f = Me / Z


f > yield stress = 2300 kgf/cm2
f = Me / Z
⸫ 2300 = 873.38 * 100 / ( π d3 / 32)
⸫ d = 7.28 m

Let diameter of shaft, d = 8 cm = 80 mm


f = Me / Z
= 873.89 * 100 / (π * (12)3 / 32) = 1739.43 kgf/cm2
f < yield stress = 2300 kgf/cm2
Hence, we can provide d = 80 mm

56
Moment of Inertia, I = π d4 / 64
= π * 84 / 64
= 200.96 cm4

Maximum Deflection in Shaft,


∆ = F m * L3 / 3 * E * I
= 414.71 * 2103 / 3 * 19.5 * 105 * 200.96
= 13.26 cm

Critical Speed, Nc = 60 * 4.187 / ∆0.5


= 68.98 %
Hence shaft diameter = 80 mm

Blade Thickness calculation:


Endurance limit for Carbon Steel = Ultimate Tensile Stress / Factor of Safety
= 4200 / 2
= 2100 kgf/cm2
Maximum stress created in blade material,
f=m/Z
f = Max. B.M. / Z
⸫ 2100 = m / (bt * bw / 6)
⸫ 2100 = 93.31 * 100 / (bt * 120 / 6)
⸫ bt = 0.218 cm
⸫ bt = 2.18 + 2C
= 2.18 + 2*1.5
= 5.18 mm
Use 8 mm thick agitator Blade

57
CHAPTER 8
PUMPS AND VALVES

58
8.1 Various pumps used in the plant

The different types of pumps used in the plant are:


1. Centrifugal Pump
2. Diaphragm Pump
3. Vacuum pump

8.1.1 Centrifugal Pumps

Centrifugal pumps are used to transport fluids by the conversion of rotational kinetic
energy to the hydrodynamic energy of the fluid flow. The rotational energy typically
comes from an engine or electric motor.
 Characteristics:
Creating a resistance to the flow controls the kinetic energy of a liquid coming out of
an impeller. The first resistance is created by the pump volute (casing), which catches
the liquid and slows it down. When the liquid slows down in the pump casing, some
of the kinetic energy is converted to pressure energy. It is the resistance to the pump’s
flow that is read on a pressure gauge attached to the discharge line. A pump does not
create pressure, it only creates flow. Pressure is a measurement of the resistance to
flow.

8.1.2 Diaphragm Pumps

A diaphragm pump (also known as a Membrane pump) is a positive displacement


pump that uses a combination of the reciprocating action of a rubber, thermoplastic or
Teflon diaphragm and suitable valves on either side of the diaphragm (check valve,
butterfly valves, flap valves, or any other form of shut-off valves) to pump a fluid.

 There are three main types of diaphragm pumps:

Those in which the diaphragm is sealed with one side in the fluid to be pumped, and
the other in air or hydraulic fluid. The diaphragm is flexed, causing the volume of the

59
pump chamber to increase and decrease. A pair of non-return check valves prevent
reverse flow of the fluid.

Those employing volumetric positive displacement where the prime mover of the
diaphragm is electro-mechanical, working through a crank or geared motor drive, or
purely mechanical, such as with a lever or handle. This method flexes the diaphragm
through simple mechanical action, and one side of the diaphragm is open to air.

Those employing one or more unsealed diaphragms with the fluid to be pumped on
both sides. The diaphragm(s) again are flexed, causing the volume to change. When
the volume of a chamber of either type of pump is increased (the diaphragm moving
up), the pressure decreases, and fluid is drawn into the chamber. When the chamber
pressure later increases from decreased volume (the diaphragm moving down), the
fluid previously drawn in is forced out. Finally, the diaphragm moving up once again
draws fluid into the chamber, completing the cycle. This action is similar to that of the
cylinder in an internal combustion engine. Diaphragm Pumps deliver a hermetic seal
between the drive mechanism and the compression chamber, allowing the pump to
transfer, compress, and evacuate the medium without a lubricant.

An elastomeric diaphragm can be used as a versatile dynamic seal that removes many
of the limitations found with other sealing methods. They do not leak, offer little
friction, and can be constructed for low pressure sensitivity. With the right material
consideration, diaphragms can seal over a wide range of pressures and temperatures
without needing lubrication or maintenance.

The centrifugal pumps are made of stainless steel and cast iron. The diaphragm of the
diaphragm pump is made up of poly propylene.

8.1.3 Vacuum pump

OTL Pumps are single stage or double stage rotary sliding vane type designed to
eliminate all problems associated with conventional vacuum systems.

60
A small amount of fresh oil is continuously injected in the internals for lubrication
and sealing by an independent force feed oil pump. This oil is discharged from the
exhaust of the pump along with process vapors /non condensables. Since fresh oil is
continuously injected and contaminated oil is continuously discharged with the vapors,
there is absolutely no drop in vacuum through out the process. This will result in
lowered operating temperatures and substantially reduced batch durations. The oil
consumption varies from 300 ml/hour to 450 ml/hour depending on the model /
capacity of the pump. A Radiator cooling arrangement ensures that the pump
maintains a suitable high operating temperature. This in turn ensures that the vapors
enter and exit in vapor form and do not condense in the internals thus eliminating
corrosion and the resultant maintenance.Viton oil seals are provided for long life.

Oil lubricated mechanical shaft seals are provided on the drive side with both faces in
metal for long and trouble free service. Heat treated Phenolic fiber vanes are proven
to withstand vapors like methanol, EDC, MDC, toluene, Xylene, Benzene, hexane etc.
these also ensure that there is minimum wear on the stator bore. The design of the
pump ensures that vanes / bearings can be replaced in a short time without disturbing
the motors or process pipe lines or electricals .

In other words the OTL series High Vacuum pumps will achieve and maintain
consistent High vacuum through out the process duration in spite of handling vapors /
non condensables. These pumps are capable of handling / corrosive vapors due to that
fact that because of high operating temperatures they do not allow the vapors to
condense in the internals. The maintenance crew will find it extremely easy to do the
routine maintenance jobs.

8.2 Various valves used in the plant

Different types of valves used in the industry are:


1. Ball Valves
2. Globe Valves
3. Plug Valves
4. Non Return Valves

61
8.2.1 Ball Valves

A ball valve is a form of quarter-turn valve which uses a hollow, perforated and
pivoting ball (called a "floating ball") to control flow through it. It is open when the
ball's hole is in line with the flow and closed when it is pivoted 90-degrees by the
valve handle. The handle lies flat in alignment with the flow when open, and is
perpendicular to it when closed, making for easy visual confirmation of the valve's
status.

Ball valves are durable, performing well after many cycles, and reliable, closing
securely even after long periods of disuse. These qualities make them an excellent
choice for shutoff applications, where they are often preferred to gates and globe
valves, but they lack their fine control in throttling applications.

The ball valve's ease of operation, repair, and versatility lend it to extensive industrial
use, supporting pressures up to 1000 bar and temperatures up to 752 °F (500 °C),
depending on design and materials used. Sizes typically range from 0.2 to 48 inches
(0.5 cm to 121 cm). Valve bodies are made of metal, plastic, or metal with a ceramic;
floating balls are often chrome plated for durability. One disadvantage of a ball valve
is that they trap water in the center cavity while in the closedposition. In the event of a
freeze, the sidescan crack due to expansion of ice forming. Some means of insulation
or heat tape in this situation will usually prevent damage. Another option for cold
climates is the "freeze tolerant ball valve". This style of ball valve incorporates a
freeze plug in the side so in the event of a freeze up, the freeze plug ruptures, (acts as
a sacrificial disk), thus making for an easy repair. Now instead of replacing the whole
valve, just screw in a new freeze plug. This is commonly called freeze plug
technology.

8.2.2 Globe valve

A globe valve, different from ball valve, is a type of valve used for regulating flow in
a pipeline, consisting of a movable disk-type element and a stationary ring seat in a
generally spherical body.

62
Globe valves are named for their spherical body shape with the two halves of the
body being separated by an internal baffle. This has an opening that forms a seat onto
which a movable plug can be screwed in to close (or shut) the valve. The plug is also
called a disc or disk.In globe valves, the plug is connected to a stem which is operated
by screw action using a hand wheel in manual valves. Typically, automated globe
valves use smooth stems rather than threaded and are opened and closed by an
actuator assembly.

Globe valves are used for applications requiring throttling and frequent operation. For
example, globe valves or valves with a similar mechanism may be used as sampling
valves, which are normally when liquid samples are being taken. Since the baffle
restricts flow, they are not recommended where full, unobstructed flow is required.

8.2.3 Plug Valves

Plug valves are valves with cylindrical or conically tapered "plugs" which can be
rotated inside the valve body to control flow through the valve. The plugs in plug
valves have one or more hollow passageways goingsideways through the plug, so that
fluid can flow through the plug when the valve is open. Plug valves are simple and
often economical.

When the plug is conically tapered, the stem/handle is typically attached to the larger
diameter end of the plug. Plug valves usually do not have bonnets but often have the
end of the plug with the handle exposed or mostly exposed to the outside. In such
cases, there is usually not much of a stem. The stem and handle often come in one
piece, often a simple, approximately L-shaped handle attached to the end of the plug.
The other end of the plug is often exposed to the outside of the valve too, but with a
mechanism that retains the plug in the body.

The simplest and most common general type of plug valve is a 2-port valve with two
positions: open to allow flow, and shut (closed) to stop flow. Ports are openings in the
valve body through which fluid can enter or leave. The plug in this kind of valve has

63
one passageway going through it. The ports are typically at opposite ends of the body;
therefore, the plug is rotated a fourth of a full turn to change from open to shut
positions. This makes this kind of plug valve a quarter-turn valve. There is often a
mechanism limiting motion of the handle to a quarter turn, but not in glass stopcocks.

8.2.4 Non return Valves


A check valve, clack valve, non-return valve or one-way valve is a valve that
normally allows fluid (liquid or gas) to flow through it in only one direction.

Check valves are two-port valves, meaning they have two openings in the body, one
for fluid to enter and the other for fluid to leave. There are various types of check
valves used in a wide variety of applications.

Check valves are often part of common household items. Although they are available
in a wide range of sizes and costs, check valves generally are very small, simple, or
inexpensive. Check valves work automatically and most are not controlled by a
person or any external control; accordingly, most do not have any valve handle or
stem. The bodies (external shells) of most check valves are made of plastic or
metal.Check valves are often used with some types of pumps. Piston-driven and
diaphragm pumps such as metering pumps and pumps for chromatography commonly
use inlet and outlet ball check valves.

These valves often look like small cylinders attached to the pump head on the inlet
and outlet lines. Many similar pump-like mechanisms for moving volumes of fluids
around use check valves such as ball check valves. The feed pumps or injectors which
supply water to steam boilers are fitted with check valves to prevent back-flow.

8.3 Control Valve

There are no control valves in this plant but one can implement a control valve for
controlling the steam flow rate which in turn controls the temperature of the reactor.
The basic control loop for such a control valve is given below.

64
Error Error Signal
Comparator Reactor/
Heat Controller Steam Valve
Jacket

Thermocouple

Figure 8.1 Block Diagram of Control Valve

8.4 Piping

In Plant piping material is selected on the base of bellow criteria:

 Material specification
 Chemical composition
 Mechanical properties
 Brittle facture toughness
 Carbon equivalent
 Inspection time
 Easy to repairing
 Welding procedure

8.5 Conclusion

Unlike in any Chemical Process Industry, in Pharmaceutical Industries DCS system is


mostly not implemented. However, recent developments show the applications of
DSC system even in Pharmaceutical Industries. Mostly for material handling,
Centrifugal pump was used. Ball valve is preferred owing to the smoothness in
operation.

65
CHAPTER 9
HEALTH, SAFETY AND ENVIRONMENT

66
9.1 Introduction

Safety is the state of being “safe”, the condition of being protected against physical,
social, spiritual, financial, political, emotional, occupational, psychological,
educational or other types or consequences of failure, damage, error, accidents, harm
or any other event which could be considered non-desirable. This can take the form of
being protected from the event or from exposure to something that causes health or
economical losses. It can include protection of people or of possessions.

Accidents are analyzed and developed a separate engineering branch of safety and this
analysis was required due to:
 Rising trend of accidents.
 Increased use of machinery.
 Increased material handling.
 Lack of safety standard.
 Lack of training.
 Better reporting of accidents.

No industry can afford to neglect the fundamentals of safety in design and operation
of its plant and machinery. It is important that all the people responsible for
management and operation of any industry should have a good knowledge of
industrial safety.

9.2. Fire Fighting

There is a rapid combustion resulting of heat and light of flame. Flame is luminous
hot come of the fire. For catch fire required three things
1. Combustible Material
2. Air (oxygen)
3. Heat and local temp.
Remove any one and fire will extinguish.

67
Table 9.1 Classification of fire

FIRE CLASS COMBUSTIBLE FIRE EXTINHGUISHING MEDIUM


MATERIAL
A Fire involving ordinary Water and solution with high water
solid material such as content. Cooling and wetting of material
wood, coal, plastic, paper is main principle
etc…
B fire involving flammable Limiting air or oxygen supply inhibits
liquid such as diesel, fire. DCP, FOAM should be used
kerosene, liquid
Chemicals etc..
C Fire involving live CO2 gas , dry chemicals should be used
electrical equipment in
energized state
D fire involving metals Special chemicals and technique are used
E Fire involving flammable Starvation of fire is most useful
gases and fuels

9.2.1 Facilities for the handling the material and firefighting equipment

 Fire and safety department


 Foam system
 Fire water pump
 Fire Bucket
 Fire alarm
 Water hydrant system
 AFFF(Aquous Film Forming Foam)

68
9.2.2 Safety related equipments

 Face shield
 Nitrile hand gloves
 Surgical hand gloves
 Butyl hand gloves
 Safety goggles
 Nomex fire suit
 Spillage kit
 Full body suit
 Cartridge mask
 3M air mask with hose pipe
 White nose mask
 Barrier cream

Auxiliary Pump is provided as Boiler feed Pump in boiler section to feed water at
failure of main pump.

9.2.3 Hazop of the plant

 In case of an accident one has to blow safety Alarm.


 After blowing the Alarm try to evacuate yourself and reach to the safety point.
 Discuss the problem with the safety engineer and try to follow the instruction
given by the safety engineer.
 In case of fire accident, try to control the fire using the fire extinguishers if it is in
a controllable situation, if not contact the fire brigade.
 In case of electrical fire, stop the electrical supply in the particular section and
then try to control the fire.
 In case of any leakage first go for the PPEs and then start the procedure for
maintenance.
 If any employee is affected then take him to get the first aid.

69
9.2.4 Equipment Location According to the Wind Load Direction

Plant is having four floors. And there is no any tall vertical equipment. So any
equipment of plant is not much affected by wind load.

9.2.5 Safety related Equipments, their Locations and Reasons

At plant there are around 60 to 65 Nos. of fire extinguishers of different classes which
can handle fire hazards that can be possible in the plant.
The safety team of plant is regularly take part in the safety meeting, arranged at every
3 months and the decision taken in the meeting is carry forward to the safety inspector.
This safety committee consists of employees from various parts of the plant as a
member. They are also arranging safety programs for workers. WE were also giving
training on safety and how to operate fire extinguishers in self development and
learning center as a part of GMP training.

9.3 Pollution control measures

9.3.1 Water Pollution Control

 Effluent Treatment Plant

The waste water coming from the all sections of plant is collected in a common tank.
The pH of the effluent is around 2 to 4.The effluent coming from various sources first
goes to the equalization tank where various different types of effluents having
different compositions gets mixed with each other to provide a uniform mixture of
slurry which can be treated further. The effluent from common collection tank goes to
the neutralization tank where it is continuously mixed with CaCO3 powder, at this
level the pH of the effluent reaches around 9. Around 10 tons of CaCO3 is used per
day. Now this effluent having 9 pH is pumped to filter press, which is made of poly
propylene. The solid waste and excess lime is removed from filtration unit and send
to solid waste dumping site. While the filtrate effluent is taken into a mixer tank
where acidic water having 2 pH is added to filtrate to make effluent of 7 to 8 pH.

70
Now the effluent is taken in the primary settling unit (sedimentation tank) where
flocculating agent is added to the effluent stream. The outlet from the primary settling
unit is sent to Central Effluent Treatment Plant (C.E.T.P.).

Here, various parameters like pH , COD, TS, TDS, oil & grease, etc of waste water
coming out of ETP are in their permissible limit (According to norms of G.P.C.B.).
So, secondary treatment unit like aeration tank, carbon filter, etc. are not required.
Around 7 lacs litres of effluent is treated in the ETP. The cost of ETP is around 24 Rs.
/ kg Ef.

9.3.2 Air Pollution Control

 Boiler Section: Electrostatic precipitator and bag filters are used to collect the
small particulate matter emitting from the fire box of the boiler. The outlet of this
equipment contains less than 100 ppm of particles.
 Process Section: Scrubbers are used for scrubbing undesirable gases emitting to
atmosphere. They are operated in counter current fashion where the solvent is fed
from the top and gas mixture is fed from bottom.

9.4 Conclusion

We conclude that no industry can afford to neglect the fundamentals of safety in


design and operation of its plant and machinery. Each Industry has its own policy and
approach towards safety as discussed above. Various safety equipment as used as per
their application and need. Industries need to follow the Environment norms set by the
state and treat the waste accordingly with suitable technology and technique.

71
CHAPTER 10
PLANT LAYOUT AND PLANT LOCATION

72
10.1 Introduction

10.1.1 Plant Layout

After process flow diagram are completed and before detailed piping, structural and
electrical design can begin, the layout of process units in plant and equipment within
these process units must be planned. This layout can play important role in
determining construction and manufacturing costs and thus must be planned carefully,
with attention being given to future problems that may arise.

Proper layout will include arrangement of processing area, storage area, and handling
areas in efficient coordination and with regard to such factors as:

 Type and quality of product to be produced.


 Type of product and process control.
 Type of building needed and building code requirement.
 Operational accessibility and convenience.
 Space available and space needed.
 Health and safety consideration.

10.1.2 Plant Location

The geographic location of final plant can have a strong influence on the success of an
industrial venture. Primarily, the plant should be located where minimum cost of
production and distribution can be obtained, but other factors such as room for
expansion and safe living conditions for plant operation as well as the surrounding
community are also important.

The choice of final site should be based on complete survey of advantages and
disadvantages of various geographic areas and ultimately on available real estate.

73
10.2 Principle of Plant Layout

 Storage Layout
Storage facilities for raw material, intermediates, and finished products may be
located in isolated or adjoining area. This will reduce the internal transportation and
material handling cost. Liquids are commonly stored in cylindrical or rectangular
tanks. While gases are stored in spherical or hemispherical or cylindrical pressurized
tanks. Solids which are not affected by open atmosphere conditions can be stored in
open bins or silos.

 Equipment Layout
During modeling of equipment layout, ample space should be assigned to each piece
of equipment. Identical equipment which are repeated several times in flow of
material should be arranged in group or series and this may reduce operating cost.

 Plant Expansion
During the procedure of plant layout, there must be a specified provision for plant
expansion. As this provision will be helpful for future expansion of existing plant.
There will be sufficient space available during the time of expansion.

 Building
The plant building may be either in-house or open plant. When there is a need of inert
atmosphere one should go for in-house plant or else open plant are constructed. The
plant buildings are provided with ventilation, lighting, electrical supply, labors,
platforms, etc.

74
10.3 Factors for Plant Location

The factors to be considered are as followed:

 Raw Material availability

 Market

 Energy availability

 Transportation facilities

 Water Supply

 Climate

 Waste Disposal

 Labor Supply

 Community Factors

 Taxation and Legal Restriction

75
10.4 Drawing of Plant Layout

Figure 10.1 Overall Plant Layout

76
10.5 Conclusion

We conclude that factors as discussed above are vital for making the final layout of
the plant. The layout presented above is the same as the actual layout of the plant
which not much accurate as per the need of the ideal plant layout. The layout was
prepared as the methods of unit area sizing each blocks based on the size of the
equipment kept inside the unit.

77
CHAPTER 11
COST ESTIMATION

78
11.1 Introduction

Cost estimation is done to calculate the total cost of the plant including fixed cost,
direct cost, production cost, raw material cost, cost for labor, maintenance, powder
and utilities, along with cost for the plant and administrative overhead, distribution of
final products and other miscellaneous items.

As soon as the final process design stage is completed, it becomes possible to make
accurate cost estimation because detailed equipment specification and definite plant
facility information are available. Direct price quotations based on detailed
specifications can then be obtained from various manufacturers. However, no design
project should proceed to the final stages before costs are considered, and cost
estimates should be made throughout all the early stages of design when complete
specifications are not available.

The cost estimation also gives us an idea about the direct charges, indirect charges,
fixed capital investment, working capital, plant overhead expenses, etc.

11.2 Purchased Equipment Cost

11.2.1 Based on MOC

Reactor installed is jacketed vessel operating at atmospheric condition having


adequate openings for inlet and outlet and for measuring device. MOC used for vessel
is SS 316 plate of dimension 150 × 120 mm.

Cost of SS 316 is Rs. 300/kg

Volume of vessel = π/4 × (Do2 –Di2) × Height


= π/4 × (1352 – 133.892) × 130
= 30458.64cm3

79
Here density of material = 8000 kg/m3
= 0.008 kg/cm3

So weight of vessel = (volume × density of material)


= (30458.64 × 0.008)
= 243.66 kg

Now,
Cost of MOC = (material cost per kg × weight of vessel)
= (300 × 243.66)
= Rs. 73100.75

Weight of Jacket = π/4 × (Do2 –Di2) × Height × Density


= π/4 × (183.622 –182.022) × 130 × 0.008
= 477.61 kg

Cost of Jacket = (material cost per kg × weight of vessel)


= 300 × 477.61
= Rs. 1,43,283

Weight of torispherical head = π/4 × BD2 × thickness of head × Density of MOC


= π/4 × 154.32 × 0.6 × 0.008
= 89.71 kg

Cost of torispherical head = (material cost per kg × weight of head) = 33936 INR
= 300 × 89.71
= Rs. 26,913.11
⸫ Total cost of head = 2 × 26913.11 = Rs. 53,826.22

Weight of nozzles = π/4 × (Dno2 – Dni2) × (Hi + Ho) × Density of MOC


⸫ Weight of manhole nozzle = π/4 × (60.822 – 602) × (3.476) × 0.008
= 2.1 kg

80
So,
Total weight of 7 Nozzles = 7 × 2.1
= 14.76 kg
⸫ Total cost of 7 nozzles = weight of 7 nozzles × material cost per kg
= 14.76 × 300
= Rs. 4428

Cost of Flange and bolt

Weight of flange = π/4 × (Dfo2 – Dfi2) × Flange thickness × Density of MOC


⸫ Weight of manhole flange = π/4 × (70.4622 – 60.822) × 6.20 × 0.008
= 49.37 kg

So,
Total weight of 7 flanges = 150 kg
Total cost of flanges = (total weight × cost per kg)
= (150 × 300)
= Rs. 45000

Cost of bolts = Number of bolts × Cost per unit


= 92 × 10 INR per 3/8 UNC 56 bolt
= Rs. 920

Cost of fabrication

Perimeter = 3.14 × 133.89 = 420.41 cm


Length = 130 cm

Now if we select (150×120) cm plates


Then,
Plates required of 150 cm = 3
Plates required of 120 cm = 2

Total no of plates required = 6

81
So total area of plates = 6*1.8
= 10.8 m2
= 166.25 ft2

Now total cost of fabrication = Total area × cost per unit area
= 166.25 × 100
= Rs. 16625

Cost of welding
Length = 150 cm
Width = 120 cm
No. of plates = 6

Total length of welding = 2(length + width) ×no of plates


= 2× (150 + 120) × 3
= 1620 cm
= 16.20 m

Cost of welding = (Total length of welding × 10 Rs/m)


= 16.20*10
= Rs. 162

Cost of agitator = Rs. 35,300 (assumed value)

Total cost of Reactor = (cost of MOC+ cost of jacket + Cost of heads + cost of
nozzles + cost of flanges + cost of fabrication + cost of welding + cost of agitator)
=(73100.75+143283+23600+53826.22+4428+4500+920+16625+162+35300)
= Rs. 355769.7
Therefore,
Cost of reactor = Rs. 3,55,769.7
⸫ Cost of 2 reactors = 2 * 355769.7
= Rs. 7,11,539.5

82
Table 11.1 Purchased Equipment Cost

Sr. No. Equipment Quantity Cost/piece Total cost


(Rs.)
1 Milling Equ. 1 300000 300000
2 Reactor 2 355769.7 711539.5
3 Pressure Reactor 1 1200000 1200000
4 Storage Tank 1 90000 90000
5 Crystallizer 1 1100000 1100000
6 Centrifuge 1 400000 400000
7 Reactor 1 1600000 1600000
8 Crystallizer 1 1100000 1100000
9 Vessel 3 800000 2400000
10 Heat exchanger 3 200000 600000
11 Flaker 1 300000 300000
12 Distillation Reactor 2 800000 1600000
13 Distillation Column 2 1200000 2400000
14 Condenser 4 300000 1200000
15 Ejector system with HE 2 600000 1200000

So, Total Purchased Equipment Cost = Rs. 16101000

11.3 Capital Cost

Purchased Equipment Cost (PEC) = Rs. 16101000


But we know that,
Total Capital Investment = Fixed Capital Investment + Working Capital Investment
T.C.I = F.C.I + W.C.I

83
11.3.1 Fixed Capital Investment (F.C.I)
F. C.I = Direct Cost + Indirect Cost
Table 11.2 Direct Cost Factor

Sr. No. Item % of PEC

1 Purchased Equipment Cost 100


2 Insulation Cost 10
3 Installation Cost 45
4 Instrumentation & Control 26
5 Piping 40
6 Electrical Installation 15
7 Building including services 36
8 Yard Improvement 8
9 Service Facilities 58
TOTAL 338

Total Direct Cost = 16101000* 338/100


= Rs. 5,44,21,380

Table 11.3 Indirect Cost Factor

Sr. No. Item % of PEC

1 Construction Expenses 40
2 Contractor Fee 24
3 Contingencies 35
4 Legal Expenses 8
5 Engineering and Supervision 46
TOTAL 153

84
Total Indirect Cost = 16101000 * 153/100
= Rs. 2,46,34,530

Total Fixed Capital Investment (FC)


= Total Direct Cost + Total Indirect Cost
= Rs. 5,44,21,380 + Rs. 2,46,34,530
= Rs. 7,90,55,910

11.3.2 Working Capital Investment (W.C.I)

It includes the total cost invested in:


 Raw Material and supplies carried in stocks.
 Finished product in stocks and semi finished products in process of being
manufactured.
 Accounts receivable
 Cash kept on hand for monthly payment of operation expenses.
 Account Payable
 Taxes Payable

It is in the range of 20% of Total Capital Investment (T.C.I)


T.C.I = F.C.I - W.C.I
⸫ T.C.I = F.C.I + (0.2) T.C.I
⸫ (0.8) T.C.I = F.C.I
⸫ T.C.I = F.C.I / (0.8)
⸫ T.C.I = 79055910 / 0.8
⸫ T.C.I = Rs.9,88,19,887.5

Now,
W.C.I = T.C.I - F.C.I
⸫ W.C.I = 98819887.5 - 79055910
⸫ W.C.I = Rs.1,97,63,977.5

85
Capital Investment Cost (Rs.)
F.C.I 79055910
W.C.I 19763977.5
T.C.I 98819887.5

11.4 Manufacturing Cost

11.4.1 Fixed Charges

(1) Depreciation
For Machinery, 10% of F.C.I = Rs. 79,05,591
For Building, 2.5% of F.C.I = Rs. 19,76,317.75
Total = 7905591 + 1976317.75
= Rs. 98,81,988.75

(2) Local Taxes


1% of F.C.I = Rs. 7,90,559.1

(3) Insurance
2% of F.C.I = Rs.15,81,118.2

Total fixed charges = 9881988.75 + 790559.1 + 1581118.2


= Rs. 1,22,53,666.05

Plant overhead cost is 10% of total fixed charges.


Plant overhead cost = 10 % of 12253666.05
= Rs. 12,25,366.605

86
11.4.2 Direct Production Cost

Table 11.4 Direct Production Cost


Sr. No. Item % Cost Cost (Rs.)
1 Operating Labour 10% of Total Equipment Cost 1610100
2 Direct Supervision 10% of Operating Labour 161010
3 Utilities 12% of Total Equipment Cost 193212
4 Maintenance and Repairs 7% of F.C.I 5533913.7
5 Operating Supplies 10% of Maintenance and Repair 553391.37
6 Laboratory Charges 12% of Operating Labour 193212
7 Patent and Royalties 5% of Total Equipment Cost 805050
8 Plant Overhead Cost 10% of Total Equipment Cost 1610100
9 Raw Material Cost 60% of F.C.I 47433546

So, Total Direct Production Cost = Rs. 5,80,93,535.07

Manufacturing Cost = Direct Production Cost + Plant Overhead Cost +


Fixed Charges
= 58093535.07 + 1225366.605 + 12253666.05
= Rs. 7,15,72,567.725

11.4.3 General Expenses

Table 11.5 General Expenses


Item %Cost Cost(Rs.)
Administration Cost 9% of F.C.I 7115031.9
Distribution and Selling Cost 15% of F.C.I 11858386.5
R&D Cost 8% of F.C.I 6324472.8
Sales and Services 11% of F.C.I 8696150.1

So, Total General Expenses = Rs.3,39,94,041.3

87
11.4.4 Total Production Cost

Total Production Cost = Manufacturing Cost + General Expenses


= 71572567.725 + 33994041.3
= Rs. 10,55,66,609.025

11.5 Profitability Analysis

11.5.1 Yearly Production

Total 9000 Kg of Acotiamide HCl Trihydrate is expected to be made per year.


Along with that 1519 Kg of Methyl Ethyl Ether is obtained as a useful by product.
The average selling value of Acoriamide HCl Trihydrate is Rs. 20000/kg
The average selling value of Methyl Ethyl Ketone is Rs. 3550/kg
Thus, the Total Income = (20000 * 9000) + (3550 * 1519)
= Rs. 18,53,92,450

11.5.2 Gross Profit

Gross Profit = Total Income - Total Production Cost


= 185392450 - 105566609.025
= Rs. 7,98,25,840.975

11.5.3 Net Profit

Income Tax (IT)


It is in range of 30-50% of Income
Assume 40% of Income
So,
Income Tax (IT) = 0.40*79825840.975
= Rs. 3,19,30,366.39

88
Net Profit = Gross Profit - Income Tax
= 79825840.975 - 31930366.39
= Rs. 4,78,95,504.585

11.5.4 Rate of Return

Rate of return = (Net Profit / TCI) * 100


= 47895504.585 / 98819887.5
= 48.46%

11.5.5 Payback Period

Payback Period = F.C.I / Net Profit


= 79055910 / 47895504.585
= 1.65 i.e. 2 year

11.6 Conclusion

All calculations are based on percentage of purchased equipment cost method. From
the product value we found annual production cost which actually is raw material
inventory saving cost. From that we concludes that average 1 crore rupees net profit is
obtained by running of the plant. Also we calculated direct cost, indirect cost,
depreciation, local taxes, plant overhead cost, insurance policy, manufacturing cost,
general expenses, etc.

89
CHAPTER 12
CONCLUSION

After completing this four month industrial training at two different companies, I
come on a conclusion that such a type of training feels access between theoretical
aspects of technical thing and how that is implemented in practice. Also this training
has helped me learn a lot in terms of technical along with social things. I got an
opportunity to understand the practical functioning of various equipments with their
basic design and application along with running processes. I also tried to observe
important aspects of industrial management, discipline, and safety precautions. What I
studied here is some general information about product, process description, salient
features of the plant, diagrams, mass balance, energy balance, Functioning of major &
minor process equipments, safety rules, utilities, ETP along with cost estimation of
the plant.

90
CHAPTER 13
BIBLIOGRAPHY

Joshi M.V.; Mahajani V.V. Process Equipment Design, 3rd ed.; Macmillan India Ltd:
New Delhi, 1976; p.96, 106,115,126 to 131,201,202,334,340,368,369.

Peters Max S.; Timmerhaus Klaus D. Plant Design and Economics for Chemical
Engineers, 4th ed.; McGraw-Hill, Inc.: New York, 1991; p.300.

Robert E. Treybal; MASS TRANSFER OPERATION; 3rd edition; McGraw Hill:


1980.

Thakore S.B.; Bhatt B.I. Stoichiometry, 5th ed.; TMHEPL: New Delhi, 2010; p.
11,111,187,193,382,397.

Thakore S.B.; Bhatt B.I. Introduction to Process Engineering and Design, 1st ed.;
TMHEPL: New Delhi, 2007; p. 55, 60,135 - 82,663,664.

Warren L. Mc-Cabe, Julian C. Smith, Peer Harriolt; Unit Operations of Chemical


Engineering , 5th edition; McGraw Hill: 1993

91

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