Professional Documents
Culture Documents
Project Report
On
Trazodone (Phase I)
And
i
COMPANY TRAINING CERTIFICATE (PHASE -II)
ii
CERTIFICATE
iii
DECLARATION
iv
ACKNOWLEDGEMENT
v
PREFACE
vi
PHASE I
TRAZODONE
vii
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
viii
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
ix
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
x
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 13 BIBLIOGRAPHY..........................................................................108
xi
LIST OF FIGURES
LIST OF TABLES
xii
2.3 Properties of KSM02 24
xiii
ABBRIVATIONS
BD Blank Diameter
SR Slenderness ratio
Kg Weight in Kilograms
mm Length in Millimeter
m Length in Meter
cm Length in Centimeter
J Energy in Joules
xiv
cal Energy in Calories
K Temperature in Kelvin
W Power in Watts
SS Stainless Steel
MS Milled Steel
Hp Horse Power
xv
NOMENCLATURE
τ Reaction Time, hr
M Mass of Solid, kg
Q Amount of Heat, J
T Actual Temperature, ℃ or K
Tr Reduced Temperature, ℃ or K
Tc Critical Temperature, ℃ or K
t Temperature Difference
X Conversion
P Pressure, KPa
xvi
θ Space Time, hr
D Diameter, m
H Height, m
Rc Crown Radius, m
Rk Knuckle Radius, m
W Weight, kg
tf Design Thickness, mm
tn Nozzle Thickness, mm
Dc Diameter of Coil, mm
Dj Diameter of Jacket, mm
bw Width of Blade, mm
σ Stress, kgf/cm2
Np Power Number
P Power, hp
Τc Torque, kgf.m
Rb Radius of Blade, m
xvii
M Bending Moment, kgf.m
δ Maximum Deflection, cm
xviii
CHAPTER 1
INTRODUCTION
1
1.1 History of Product
1.3 Structure
2
1.4 Capacity 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.
1.8 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.
3
1.9 Physical as well as Chemical Properties of Trazodone
Odor Light
4
1.10 Material Safety Data Sheet (MSDS)
5
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.
6
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.
7
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.
8
Section 7: Exposure Control - Personal Protection
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
9
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)
10
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.
11
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)
12
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.
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:
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.
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
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.
UN number
18
Packaging group
Environmental Hazards
Chemical safety assessment: For this product a chemical safety assessment was not
carried out.
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
Raw material comes from Ami Organics Ltd. and Sukhram Pvt. Ltd.
2.1.2 Transportation
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
Odor Irritating
Density NA
Specific Heat NA
Reactivity NA
Solubility NA
Freezing Point NA
23
2.2.2 Properties of KSM-02
Odor Light
Flash Point NA
Instability NA
Reactivity NA
24
2.3 Detailed Process Description
Pressure
Nutsche Filter
NaCl
SSR
Centrifuge
mL
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
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.
Trazodone production seems a single step reaction, but however it takes place in two
steps as shown below.
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
But,
Actual Capacity= Original Capacity*(1.Roll Number) kg/batch
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
31
= 100.6148 kg
Summary Table
32
Now, Let us assume that conversion is 90%
33
(10) Unreacted KSM-02 = 98.6376 - 88.77384 = 9.86376 kg
Summary
34
3.3 Material Balance Across Each Equipment
↓
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
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
37
3.3.3 Material Balance over Centrifuge(CF)
↓
IPA + Unreacted Reactant(ML)
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
38
3.3.4 Material Balance over Vacuum Tray Dryer(VTD)
Moisture
↑
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
3.4 Conclusion
39
CHAPTER 4
ENERGY BALANCE
40
4.1 Introduction
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.
41
4.2 Energy Balance Across Each Equipment
∆T = 80℃ - 30℃ = 50 ℃
QKSM 01 = mCp∆T
=0.73*409.9*50
=14961.35
QKSM 01 = mCp∆T
=0.73*187.7*50
=6851.05
42
Table 4.2 Heat of Formation
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
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℃.
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.
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
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.
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:
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.
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.
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.
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.
5.7 Conclusion
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.
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
6.4 Centrifuge
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
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.
58
= 152.35 / 309.66
= 0.492 Kmol
Now,
τ = 12 hr.
τ / CAO = XA / -rA
-rA = 0.370 mol/lit hr
PA0 = CA0RT
R = 0.082 lit atm/mol K
T = 288 K (inside temperature of reactor)
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
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
60
For Thickness of Shell:
C.A. = 2.6 mm + 2 mm
= 4.6 mm
tf = 5 mm
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
O.D. = I.D. + 2t
= 124.09 + (2 * 0.6)
= 125.2 cm
Man Hole:
Diameter = 1000 mm
Thickness, tm = P * Do / (2 * f * J)
= (4 * 1000) / (2 * 1124.91 * 0.85)
= 2.091 mm
Jacket Design:
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
tc = trc + C
where, C = Corrosion Allowance = 2 mm
tc = 0.4 + 2
= 2.4 mm
So, take thickness of coil tc = 4 mm
63
7.3.2 Agitator and Shaft Design
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
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
66
7.4 Pump Design
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
67
= 0.0407 m
∆Hfp = (f * v2 / D * 2 * g) * L
= (0.0332 * 0.7072 / 0.06 * 2 * 9.81) * (15 + 5)
= 0.28 m
68
(ii) Hs = 0.5 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
⸫ 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,
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
H.P = 2.2 KW
H.P = 1.8 KW
H.P = 5 KW
Flow rate = 18
m3/hr
H.P = 9.5 KW
73
8.2 Details of Valves
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.
Thermocouple
Water
Inlet
Hot Steam
Water
Tank
Sensor
HE Reactor
75
8.4 Conclusion
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.
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.
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
(b) Canister Mask - used while cleaning vessels or reactor inner wall.
(a) Eye Protection - Safety goggles, Chipper goggles, Gas tight goggles, are used.
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 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 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.
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.
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.
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
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.
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.
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.
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 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.
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.
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.
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
88
CHAPTER 10
PLANT LAYOUT AND PLANT LOCATION
89
10.1 Introduction
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:
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
Market
Energy availability
Transportation facilities
Water Supply
Climate
Waste Disposal
Labor Supply
Community Factors
92
10.4 Drawing of 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.
96
Here density of material = 8000 kg/m3
= 0.008 kg/cm3
Now,
Cost of MOC = (material cost per kg × weight of vessel)
= (300 × 198.97)
= Rs. 55,691
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
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
So,
Total weight of 7 flanges = 150 kg
Total cost of flanges = (total weight × cost per kg)
= (150 × 300)
= Rs. 45000
Cost of fabrication
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 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
2 Centrifuge 1 696000
5 Pump 2 22000
2 Insulation Cost 8
3 Installation Cost 39
100
4 Instrumentation & Control 26
5 Piping 31
6 Electrical Installation 10
8 Yard Improvement 12
9 Service Facilities 55
TOTAL 310
1 Construction Expenses 34
2 Contractor Fee 19
3 Contingencies 37
4 Legal Expenses 4
5 Engineering and Supervision 32
TOTAL 126
101
11.3.2 Working Capital Investment (W.C.I)
Now,
W.C.I = T.C.I - F.C.I
⸫ W.C.I = 18922400 - 15137920
⸫ W.C.I = Rs. 3784480
102
11.4 Manufacturing Cost
(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
(3) Insurance
2% of F.C.I = Rs. 302758.4
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
104
11.5 Profitability Analysis
105
11.5.5 Payback Period
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.
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.
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
i
3.2.2 Material Balance over Tray Dryer..........................................................26
3.2.3 Material Balance around the Multi Mill................................................. 27
3.3 Conclusion........................................................................................................27
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
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
LIST OF TABLES
v
3.2 Overview of Material Balance across SSR (X=86%) 24
vi
ABBRIVATIONS
Kg Weight in Kilograms
mm Length in Millimeter
m Length in Meter
cm Length in Centimeter
J Energy in Joules
K Temperature in Kelvin
W Power in Watts
SS Stainless Steel
MS Milled Steel
Hp Horse Power
vii
NOMENCLATURE
τ Reaction Time, hr
M Mass of Solid, kg
Q Amount of Heat, J
T Actual Temperature, ℃ or K
Tr Reduced Temperature, ℃ or K
Tc Critical Temperature, ℃ or K
t Temperature Difference
X Conversion
P Pressure, KPa
viii
θ Space Time, hr
D Diameter, m
H Height, m
bw Width of Blade, mm
σ Stress, kgf/cm2
Np Power Number
P Power, hp
Τc Torque, kgf.m
Rb Radius of Blade, m
δ Maximum Deflection, cm
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.
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
C21H37ClN4O8S
2
1.4 Capacity of Product
3
1.8 Technical Competitors
1.9 Applications
4
1.10 Physical as well as Chemical Properties
Odor Light
5
1.11 Material Safety Data Sheet (MSDS)
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
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
Pictogram:
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.
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.
7
Methods and Materials for containment and cleaning up Absorb spills on sand or
vermiculite and place in closed container for disposal.
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
8
Possible hazardous combustion products: carbon oxides; hydrogen chloride;
nitrogen oxides; sulfur dioxide.
No Data
No Data
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
2.1.2 Transportation
12
2.1.3 Cost of Raw Materials
Table 2.2 Cost of Raw Materials
5. Water H2O 22
8. Toluene C7H8 45
13
2.2 Physical and Chemical Properties of Raw Materials
14
2.3 Detailed Process Description
SSR
CENTRIFUGE
TRAY
DRYER
MULTI
MILL
PACKAGING
15
2.3.2 Process Description
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
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
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
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.
For conversion, the quantity of reactant reacted is identified. The material balance is
governed by Law of Conservation of Mass, viz. Input - Output = Accumulation.
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)
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
CTA-1→ → CTA-pure
HCl→
R-3→ SSR
H2O→
→CH3CH2OCH
20
(1) Moles of CTA-pure to be produced = 150/541.052
= 0.277kmol
21
Summary Table
22
Now, Let us assume that conversion is 86%
= 0.322 kmol
23
(9) Kg of unreacted CTA-1 = 117.97-101.49 = 16.48 kg
Summary Table
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.
↓
Mother Liquor (ML)
Summary
Table 3.3 Overview of Material Balance across CF
25
3.2.2 Material Balance over Tray Dryer
Moisture
↑
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
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
27
CHAPTER 4
ENERGY BALANCE
28
4.1 Introduction
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 ℃
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
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
31
4.3 Conclusion
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.
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:
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
35
5.3 Attachments to the Boiler
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.
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.
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.
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.
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
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.
MOC SS 316
Diameter 1700 mm
Length 2080 mm
40
6.3 Centrifuge
Capacity 300 kg
MOC SS 316
Motor Hp 15 Hp
41
6.5 Multi Mill
42
6.6 Tray Dryer
MODELS TD-48
WDH
External Dimension in mm
1980X1020X1880
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
Insulation
50/75/75
in mm100°C/200°C/300°C
No of Trays 20
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
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.
47
Volume of CTA-1,
V = mass/density
= 117.97 / 1.34
= 0.088 m3
Now,
τ = 15 hr.
τ / CAO = XA / -rA
-rA = 0.0157 mol/lit hr
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
Also,
FXF = DXD + BXB
⸫ (250)(0.35) = D(0.96) + B(0.02) … (2)
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.
50
Rmin / (Rmin + 1) = 0.426
⸫ Rmin = 0.742
R = 1.25*Rmin
⸫ R = 1.25(0.742)
⸫ R = 0.9275
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.
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
52
Heat Load on Heat Exchanger(Q) is a function of Latent heat and Sensible heat.
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.
Q’ = wCp ∆T
⸫ 12256.73 = w*1*4
⸫ w = 3064.18 kg/hr
= 0.8511 kg/s
53
LMTD = [(T1 – t1 ) – (T2 – t2 )] /ln[(T1 – t1 ) / (T2 – t2 )]
= [(75 – 36) - (37 - 32)] / In [(75- 36)/(37- 32)]
= 11.166℃
∆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
54
= 12.087 / (π *0.020* 4)
= 48.11 Nos.
⸫ Nt = 50 Nos.
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
56
Moment of Inertia, I = π d4 / 64
= π * 84 / 64
= 200.96 cm4
57
CHAPTER 8
PUMPS AND VALVES
58
8.1 Various pumps used in the plant
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.
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.
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.
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.
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.
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.
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.
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.
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Error Error Signal
Comparator Reactor/
Heat Controller Steam Valve
Jacket
Thermocouple
8.4 Piping
Material specification
Chemical composition
Mechanical properties
Brittle facture toughness
Carbon equivalent
Inspection time
Easy to repairing
Welding procedure
8.5 Conclusion
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.
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.
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Table 9.1 Classification of fire
9.2.1 Facilities for the handling the material and firefighting equipment
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.
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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.
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.
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.
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
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CHAPTER 10
PLANT LAYOUT AND PLANT LOCATION
72
10.1 Introduction
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:
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
Market
Energy availability
Transportation facilities
Water Supply
Climate
Waste Disposal
Labor Supply
Community Factors
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10.4 Drawing of 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.
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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.
79
Here density of material = 8000 kg/m3
= 0.008 kg/cm3
Now,
Cost of MOC = (material cost per kg × weight of vessel)
= (300 × 243.66)
= Rs. 73100.75
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
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
So,
Total weight of 7 flanges = 150 kg
Total cost of flanges = (total weight × cost per kg)
= (150 × 300)
= Rs. 45000
Cost of fabrication
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 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
83
11.3.1 Fixed Capital Investment (F.C.I)
F. C.I = Direct Cost + Indirect Cost
Table 11.2 Direct Cost Factor
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
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
(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
(3) Insurance
2% of F.C.I = Rs.15,81,118.2
86
11.4.2 Direct Production Cost
87
11.4.4 Total Production Cost
88
Net Profit = Gross Profit - Income Tax
= 79825840.975 - 31930366.39
= Rs. 4,78,95,504.585
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.
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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.
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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.
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.
91