Semester Internship Report

A REPORT ON

SEMESTER LONG TERM

INTERNSHIP IN

Harmony Organics Pvt. Ltd. Kurkumbh

Submitted to the Chemical Engineering Dept.

VISHWAKARMA INSTITUTE OF TECHNOLOGY, PUNE

In Partial Fulfilment of the Requirements
For the Award of the Degree of

BACHELOR OF TECHNOLOGY (CHEMICAL)

SUBMITTED BY

NIKHIL NALAWADE
(GR. NO. 151183)

Department of Chemical Engineering

BRACT’S Vishwakarma Institute of Technology,
666, Upper Indiranagar, Bibwewadi, Pune – 411 037
December 2018
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 Semester Internship Report

Bansilal Ramnath Agarwal Charitable Trust’s

VISHWAKARMA INSTITUTE OF TECHNOLOGY
(An Autonomous Institute Affiliated to University of Pune)
666, Upper Indiranagar, Bibwewadi, Pune – 411 037
December 2018

CERTIFICATE
It is certified that the project work entitled
SEMESTER LONG INTERNSHIP REPORT
Submitted by
NIKHIL NALAWADE
(G.R.NO: 151183)

is the original work carried out by them under the supervision of Prof. S.R.Kulkarni is
approved for the partial fulfilment of the requirement of Chemical Engineering Department, VIT
Pune, for the award of the Degree of Bachelor of Engineering (Chemical). This Project Work
has not been earlier submitted to any other Institute or University for the award of any degree or
diploma.

Prof. Dr. S. R. KULKARNI Mr. SANJAY NIKAM Prof. Dr.M.P. DEOSARKAR

Examiner Internal Guide Production Manager Head
Dept. of Chemical Engg. Harmony Organics Pvt.Ltd. Dept. of Chemical Engg.
VIT, Pune VIT, Pune

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ACKNOWLEDGMENTS

I take this opportunity to thank & express our sincere gratitude towards

Mr. Ravi Nangia (Managing Director) Harmony Organics Private Limited, Pune for providing us

an excellent opportunity to gain exposure to professional world. We also express sincere

gratitude towards Prof. Dr. Shrikant Kulkarni to allow us undertaking the training.

Mr. Ravi Nangia from HOPL Pune, Managing director deserves our

deepest gratitude for providing continuous support guidance throughout the training .We would

like to express our gratitude towards all ours teacher Prof. Dr. M.P. Deosarkar (HOD, Chemical

Engg. Dept. VIT, Pune) and Prof. Dr. Shrikant Kulkarni. Last but not the least we would like to

thanks all Harmony Employees to have helped in minor necessities in the process of learning.

Mr. NIKHIL NALAWADE

B-Tech Chem Engg.
G.R.No: 151183
VIT, Pune

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DECLARATION

I declare that this written submission represents my ideas in my own words and where

other ideas or words have been included, I have adequately cited and referenced the original

sources. I also declare that I have adhered to all principles of academic honesty and integrity and

have not misrepresented or fabricated or falsified any idea/data/fact/source in my submission. I

understand that any violation of the above will be cause for disciplinary action by the institute

and can also evoke penal action from the sources which have thus not been properly cited or

from whom proper permissions has not been taken when needed.

Mr. NIKHIL NALAWADE

B-Tech Chem Engg.
G.R.No: 151183
VIT, Pune

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ABSTRACT

Humble beginning with a plant in New Bombay 30 years ago for

manufacture of aroma and specialty chemicals, mainly for the fine chemical industry. The
company has made products like phenyl ethyl alcohol involving use of highly hazardous material
like ethylene oxide.
Harmony has been a regular participant in industry conferences and a
member of key trade organizations. As the Company grew in size and tonnages the original
manufacturing site at Mumbai became constraining in terms of expansion potential and hence in
the year 2006 the company established a new manufacturing location at a Chemicals
Manufacturing Hub located at Kurkumbh near Pune, India. This current manufacturing facility is
located on a 6 acre plot at Kurkumbh MIDC ( 70 km from Pune & 300 km from Mumbai) and
manufactures Phenyl Ethyl Alcohol, Styrene Oxide and Methyl-Pentenone as key products
(combined tonnage of 3000 TPA) in addition to several smaller products including Styrallyl
Acetate, Para Cresyl Methyl Ether, Anisole etc. Large customers include the S H Kelkar group &
Oriental Aromatics and Lupin Industries (Pharma). We have successfully executed export orders
to customers in EU & North America.
The company is committed to future growth in the Aroma Chemical
industry with a focus on large tonnage products. Sustainability, environment friendliness and the
safety of our employees and neighborhoods are non-negotiable goals for Harmony. The company
is invested in the welfare of its employees and has continuing investment in upgrading their
skills. Mr. Nangia is always proud to mention the number of highly skilled & devoted operators
that have been with the company more than 30 years.

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TABLE OF CONTENT

CHAPTER 1 : INTRODUCTION…………………………………………………………...10
1.1 About Phenyl Ethyl Alcohol (PEA)………………………………………………….. 10
1.2 About Methyl Pentanone (MPO)……………………….... ……………………..……10
1.3About Cinnamic Aldehyde (CNMD)……………………………………………………… 11
CHAPTER 2 : PROPRTIES OF MATERIALS……………………………………….……12
2.1 Physical Properties………………………………………………………………..…..12
2.2 Material safety data sheet…………………………………………………………...…13
2.2.1 Material safety data sheet for Phenyl Ethyl Alcohol (PEA)……….…………....13
2.2.2 Material safety data sheet for Methyl Pentanone (MPO)………………………..14
2.3 Under-ground storage tanks……………………………………………………………15
2.3.1 what is UST ?........................................................................................................15
CHAPTER 3 : PROCESS FLOW DIAGRAM……………………………………………………...16
3.1 Phenyl Ethyl Alcohol manufacture process flowsheet……………………………..…16
3.2 Methyl Pentanone manufacture Process flowsheet…………………………………....19
3.3 Cinnamic Aldehyde Manufacture process flosheet……………………………………20
CHAPTER 4 : TRAINING SESSIONS……………………………………………..……….22
4.1 Process of evaporative cooling………………………………………………………...22
4.2 Study of Pumps Types………………………………………………………………...23
4.3 Study of Valves Types ……………………………………………………………......23
4.4 Fire safety……………………………………………………………………………...23
4.5 common fire hazards…………………………………………………………………..24
4.6 What is SOP ?................................................................................................................24
CHAPTER 5 : DETAILED PROCEDURE………………………………………………...25
5.1 Process Description…………………………………………………………………...26

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5.2 Batch Inputs & Outputs……………………………………………………………………….26

5.3 Standard Operating Parameters and Time Cycle……………………………………..27
5.4 Safety Operating procedure…………………………………………………………..31

CHAPTER 6 : ADDITIONAL ASSIGNMENTS…………………………………………..32

6.1 calibration of storage tank……………………………………………………………32
6.1.1 Types of head…………………………………………………………………..32
6.1.2 Calibration of vertical tanks………………………………………………....…32
6.1.3 Calibration of horizontal tanks…………………………………………………32
6.1.5 Physical calibration…………………………………………………………….33
6.2 Pump testing at different operating pressure…………………………………………33
6.3 Piping and instrumentation diagram…………………………………………………33
6.4 Tracing and labelling of pipe lines…………………………………………………..33
6.5 Removal of unused pipes and electrical wires……………………………………….33
6.6 Monitoring……………………………………………………………………………34
6.7 Documentation……………………………………………………………………….34
CHAPTER 7 : HAZARD AND OPERABILITY STUDY (HAZOP)………………….....35
7.1 About HAZOP study………………………………………………………………...35
7.2 Methods……………………………………………………………………………...35
7.3 Guide words and parameters………………………………………………………...37
CHAPTER 8 : PLANT VIEW…………………………………………………………...…38
CHAPTER 9 : CONCLUSION………………………………………………………..……43
CHAPTER 10: REFERENCES …………………………………………………….……..44

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LIST OF FIGURE

Figure 01: Structure of PEA………………………………………………………………1

Figure 02: Structure of MPO………………………………………………………..……2

Figure 03: Structure of CNMD……………………………………………………..…….2

Figure 04: Before GLR Monitoring Graph …………………………………….………29

Figure 05: After GLR Monitoring Graph ……………………………………………..29

Figure 06: GLR P&ID…………………………………………………….….……...….30

Figure 07: Plant 01……………………………………………………………………….38

Figure 08: Dosing pump…………………………………………………………………38

Figure 09: Condensor……………………………………………………………………39

Figure 10:Cooling Tower……………………………………………...………………...39

Figure 11:Styrene batch Tank……………………………………..……………………40

Figure 12: R-3 Cooling Tank…………………………………………………………….41

Figure 13: Storage Tank…………………………………………………………………42

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LIST OF TABLES

Table 01: Properties of Materials………………………………………………………12

Table 02: Input per Batch………………………………………………………….……26

Table 03: Output per Batch…………………………………………………………...….27

Table 04: Standard Operating Parameters and Time Cycle:……………………………….27

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CHAPTER : 01
INTRODUCTION

1.1 Phenyl Ethyl Alcohol :

Phenyl ethyl alcohol is a good flavoring agent and preservative. It is extensively used in
manufacture of synthetic rose perfumes, orange blossom, Jasmine etc. and also in the synthesis
of rose oils. Practically, all rose perfumes are compounded with Phenyl ethyl alcohol. It is used
as perfumery chemical in the cosmetic formulations like detergents, soaps, perfumes, cosmetic
powder and lotions, paste cream etc.

Figure 1:- Structure of PEA

Phenyl ethyl alcohol is largely used in agarbathi, perfumery, cosmetic and soap sector. PEA
does not have any other chemical substitute which can compete with its price structure, though
Linalool is used to mimic PEA to some extent. There are reported to be over 260 agarbathi
producers in Karnataka state itself and around 450 units in the country. Phenyl ethyl alcohol is
used for providing flavor properties to toilet soaps, particularly catering to the requirement of
higher income group Phenyl ethyl alcohol are generally used in the formulation of perfumery
compounds used in product such as face powder, scent, handkerchief perfumes, shaving cream,
cigars etc
.
1.2 Methyl Pentanone :
3-methyl-2-pentanone is aliphatic ketone and isomer of 2-
hexanone.Harmony organics produces methyl pentanone on contract manufacturing bases.
Methyl pentanone is ketone and solvent of minor importance . it is comparable to MEK , but has
lower solvency and is more expensive.

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Figure 2:- Structure of MPO

It is used widely in pharmaceutical as well as aroma chemical companies.

1.3 Cinnamaldehyde (CNMD) :

Cinnamaldehyde is an organic compound with the formula

C6H5CH=CHCHO. Occurring naturally as predominantly the trans (E) isomer, it gives
cinnamon its flavor and odor.It is a flavonoid that is naturally synthesized by the shikimate
pathway.

Figure 3:- Structure of CNMD

This pale yellow, viscous liquid occurs in the bark of cinnamon trees and
other species of the genus Cinnamomum. The essential oil of cinnamon bark is about 50%
cinnamaldehyde.

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CHAPTER : 02

PROPERTIES OF MATERIALS
2.1 Physical Properties :

The list of Physical properties of some materials which Harmony

organics produces and which reactants required for production as :

Table 01:

Molecular Boiling Point Flash Point Sp. Gravity

Name of Material weight (O Celsius) (O Celsius)

Styrene 104.15 145 31.1 0.906

H2O2 34 108 12 1.2
HCl 36.5 110 1.2

SCH 1.2
SO 120 194 80 1.05
Phenyl Ethyl Alcohol 122 220 96 1.02

Methyl Ethyl Ketone 72 79 -09 0.805

H2SO4 98 337 1.84
Acetaldehyde 44 21 -38 1.52

Benzaldehyde 106 179 64 1.04

Methyl Penta none 86 138 34 0.805
Cinnamic Aldehyde 132 252 71 1.05

1,3-Butanediol 90 207 121 1.005

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2.2 MSDS (Material Safety Data Sheet) :

2.2.1 MSDS for Phenyl Ethyl Alcohol :

Potential Acute Health Effects : Very hazardous in case of skin contact (irritant), of eye contact
(irritant), of inhalation. Hazardous in case of skin contact (permeator). Inflammation of the eye is
characterized by redness, watering, and itching. Skin inflammation is characterized by itching,
scaling, reddening, or, occasionally, blistering.

Potential Chronic Health Effects: Very hazardous in case of skin contact (irritant), of eye
contact (irritant), of inhalation. Hazardous in case of skin contact (permeator).
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Not available.
TERATOGENIC EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Not available.
The substance is toxic to lungs, the nervous system, mucous membranes. Repeated or prolonged
exposure to the substance can produce target organs damage. Repeated or prolonged inhalation
of vapours may lead to chronic respiratory irritation.

Eye Contact : Check for and remove any contact lenses. Immediately flush eyes with running
water for at least 15 minutes, keeping eyelids open. Cold water may be used. Do not use an eye
ointment. Seek medical attention.

Skin Contact : After contact with skin, wash immediately with plenty of water. Gently and
thoroughly wash the contaminated skin with running water and non-abrasive soap. Be
particularly careful to clean folds, crevices, creases and groin. Cold water may be used. Cover
the irritated skin with an emollient. If irritation persists, seek medical attention. Wash
contaminated clothing before reusing.

Serious Skin Contact : Wash with a disinfectant soap and cover the contaminated skin with an
anti-bacterial cream. Seek immediate medical attention.

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Inhalation : Allow the victim to rest in a well ventilated area. Seek immediate medical
attention.

Serious Inhalation : Evacuate the victim to a safe area as soon as possible. Loosen tight
clothing such as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the
victim is not breathing, perform mouth-to-mouth resuscitation. Seek medical attention.

Ingestion : Do not induce vomiting. Examine the lips and mouth to ascertain whether the
tissues are damaged, a possible indication that the toxic material was ingested; the absence of
such signs, however, is not conclusive. Loosen tight clothing such as a collar, tie, belt or
waistband. If the victim is not breathing, perform mouth-to-mouth resuscitation. Seek immediate
medical attention.

Serious Ingestion : Not available.

2.2.2 MSDS for Methyl Pentanone :

Eye protection : Face shield and safety glasses Use equipment for eye protection tested and
approved under appropriate government standards such as NIOSH (US) or EN 166(EU).

Skin and body protection : Complete suit protecting against chemicals, Flame retardant
antistatic protective clothing, The type of protective equipment must be selected according to the
concentration and amount of the dangerous substance at the specific workplace.

Hand protection : Handle with gloves. Gloves must be inspected prior to use. Use proper glove
removal technique (without touching glove's outer surface) to avoid skin contact with this
product. Dispose of contaminated gloves after use in accordance with applicable laws and good
laboratory practices. Wash and dry hands.

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General advice : Consult a physician: Show this safety data sheet to the doctor in
attendance.Move out of dangerous area.

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. Consult a physician.

In case of eye contact Rinse thoroughly with plenty of water for at least 15 minutes and consult a
physician.

If swallowed Do NOT induce vomiting. Never give anything by mouth to an unconscious

person. Rinse mouth with water. Consult a physician.

2.3 Under ground storage tanks :

2.3.1 What is UST ?

An underground storage tank system (UST) is a tank and any underground piping connected to
the tank that has at least 10 percent of its combined volume underground. The federal UST
regulations apply only to UST systems storing either petroleum or certain hazardous substances.

When the UST program began, there were approximately 2.1 million regulated UST systems in
the United States. Today there are far fewer since many substandard UST systems have been
closed. For the most current statistics, see UST Performance Measures. Nearly all USTs
regulated by the underground storage tank requirements contain petroleum. UST owners include
marketers who sell gasoline to the public (such as service stations and convenience stores) and
non marketers who use tanks solely for their own needs (such as fleet service operators and local
governments). EPA estimates that less than 10,000 tanks hold hazardous substances covered by
the UST regulations.

Underground storage tank mainly used in petroleum products because they have low flash
point similarly in harmony organics raw materials mainly styrene and methyl ethyl ketone have
low flash point that’s why they used under ground storage tanks.These are some question which
came in my mind while going through underground storage tanks.

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CHAPTER : 03
PROCESS FLOW DIAGRAM

3.1 Phenyl Ethyl Alcohol Manufacture flowsheet :

Receiving of Raw materials (A1)

Sampling of Raw Materials (A2)

Unloading of Raw materials (A3)

Storage of Raw Materials (A4)

Transfer of Raw materials to day Tanks

(A5)

Transfer of RM to dosing Tanks (A6)

Reaction in GLR 1/3/4/5 reactors

(A7)
Neutralization of effluent water
Cooling & Settling in R3 (A8) (A11)

Multiple effect
evaporation (A12) S
Epoxidation reaction in FR/BR reactor (A9) a
lt
(
Biological A
treatment (ETP)
Transfer of SO crude To T-28/T-7 (A10)

Water Recycle to
Cooling Tower
CONT. ON NEXT PAGE

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SO crude in T-28/T-7 (A10)

Total take off of SO crude in JD/HD/GD column (A16)

Transfer of SO TTO to T-23 (A19)

SO residue Drumming
(A17)

Transfer of SO TTO to T-3/4 (A20)

Transfer to Designated Area
(A18)

Hydrogenation of SO in the reactor A3/A5 (A21)

Dispatch of SO residue (A18’) HYDROGEN

PEA crude transfer to T-1 (A22)

Solvent Recovery in BD/FD column (A23)

Recovered Solvent transfer in T-41/T-53 (A24)

PEA 1st RBM transfer in T-24 (A25)

PEA 1st RBM transfer from T-24 to ST-6 (A26)

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CONT. ON NEXT PAGE

PEA 1 RBM in ST-6 (A26)

st

Distillation of PEA RBM in ND-1 column (A27)

Transfer of PEA fraction to T-2 Bottom Material transfer to ND-2 Column

(A28) (A29)

PEA main to Receivers (A30) Transfer of PEA 2nd RBM into ST-17 (A31)

PEA main to blenders (A32)

Distillation of 2nd RBM in Distillation column (A33)

Analysis of FG (A34)

PEA TTO to ND-2 (A35) PEA residue for

drumming
Drumming of FG (A37)
Transfer of PEA Residue
drums in designated area
Packaging of FG (A39)

Dispatch (A41)

Labelling (40)

Dispatch of PEA FG (A42)

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3.2 Methyl Pentanone Manufacturen flowsheet :

Receiving of Raw materials (A1)

Sampling of Raw Materials (A2)

Unloading of Raw materials (A3)

Storage of Raw Materials (A4)

Transfer of Raw materials to Tanks (A5)

Reaction in GLR 6/7 reactors (A7)

MPO Crude to NR (A8)

1st Wash 2nd 3rd
Wash Wash
MEK recovery in LD (A9)
IBC IBC
Tank Tank NF
Filter
Recovered MEK (A10) 1st RBM to KD/HD (A10)

MPO Main (A11) 2nd RBM to ID (A11)

FO tank (A12)

Dispatch Area (A13)

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3.3 Cinnamic Aldehyde manufacture flowsheet:

Receiving raw materials (B1)

Sampling of raw materials (B2)

Unloading of raw materials (B3)

Storage of Raw materials (B4)

Transfer of raw materials to day Tanks (B5)

Aldol Condensation Reaction in JR/KR(B6)

Transfer of CNMD crude to T-59/T-60 (B7) Toluene extraction of Effluent water (B8)

Transfer of effluent water to

MEE (B9)

Distillation of Ext. toluene

(B10) S
Biological treatment (ETP) (B12) a
l
t

Drumming of Rec. toluene (B11)

Water Recycle to Cooling
Tower (B13)

Cont. to next page

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Distillation of CNMD crude in ED/DD (B14)

Transfer of Rec. CNMD TTO to T-56/T-57 (B16)

Bald to T-55 (B15)

Fraction Distillation of CNMD TTO in GD

column (B17)

Transfer of CNMD Transfer of CNMD main to the Transfer of residue into MS

fraction to T- 56/T-57 receiver (B19) drums (B20)
(B18)

Transfer of CNMD main into the

blender (B21) Transfer of Residue in
designated area (B27)

Analysis of FG (B22)

Dispatch of Residue (28)

Drumming of CNMD main (B23)

Labeling of CNMD main (B24)

Packaging (B25)

Dispatch of CNMD (B26)

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CHAPTER 4
TRAINING SESSIONS

4.1 Concept of Evaporative Cooling

The cooling tower in any chemical plant operates by the principle of evaporative
cooling. The water inlet at higher temperature cools the same at a temperature below room
temperature. This happens because one mole of water from inlet evaporating takes away 540
Kcal of energy. This energy in turn reduces the temperature of the water flowing in the
surrounding. Hence the concept Evaporative cooling. The water evaporating from the cooling
tower is lost and needs make up water. Water is added acoordingly for make up of the cooling
tower water. To reduce foam formation special chemicals are added to the cooling tower.

4.2 study of Pump types:

The following are the types of pumps

A pump is a device that moves fluids (liquids or gases), or sometimes slurries, by

mechanical action. Pumps can be classified into three major groups according to the method they
use to move the fluid: direct lift, displacement, and gravity pumps.

Centrifugal Pump
Piston pump

4.3 study of Valves types:

Valves can be categorized into the following basic types:

Ball valve : For on/off control without pressure drop, and ideal for quick shut-off, since a 90°
turn offers complete shut-off angle, compared to multiple turns required on most manual valves.

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Butterfly valve : For flow regulation in large pipe diameters.

Gate valve : Mainly for on/off control, with low pressure drop.

Globe valve : Good for regulating flow.

Needle valve : for accurate flow control.

Flush Bottom Valve : To empty the Reactor

4.4 Fire Safety

Fire safety is the set of practices intended to reduce the destruction caused by
fire. Fire safety measures include those that are intended to prevent ignition of an uncontrolled
fire, and those that are used to limit the development and effects of a fire after it starts.

Fire safety measures include those that are planned during the construction of a
building or implemented in structures that are already standing, and those that are taught to
occupants of the building. Threats to fire safety are commonly referred to as fire hazards. A fire
hazard may include a situation that increases the likelihood of a fire or may impede escape in the
event a fire occurs.

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4.5 Common fire hazards

Electrical systems that are overloaded, poorly maintained or defective

Combustible storage areas with insufficient protection
Combustibles near equipment that generates heat, flame, or sparks
Smoking (Cigarettes, cigars, pipes, lighters, etc.)
Equipment that generates heat and utilizes combustible materials
Flammable liquids and aerosols
Flammable solvents (and rags soaked with solvent) placed in enclosed trash cans
Fireplace chimneys not properly or regularly cleaned
Electrical wiring in poor condition
Leaking Batteries
Personal ignition sources – matches, lighters
Electronic and electrical equipment

4.6. What is SOP?

A standard operating procedure is a set of step-by-step instructions compiled by an organization

to help workers carry out complex routine operations. SOPs aim to achieve efficiency, quality
output and uniformity of performance, while reducing miscommunication and failure to comply
with industry regulations.

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CHAPTER 5
DETAILED PROCEDURE

5.1 Process Description:-

Step 1. Styrene reacts with H2O2 & HCL to form Styrene chlorohydin crude - Reaction

Styrene when reacts with Hydrogen peroxide & hydrochloric acid forms SCH (Styrene
Chlorohydrin). This is an exothermic reaction.

Reaction : Styrene + H2O2 + HCL Styrene chlorohydrin.

Unit Description : Reactor

Equipment : GLR-I/II/III/IV & V

Type of Reactor : MS Glass line Reactor

Capacity : 12.5 KL

Working Volume : 12500 lit.

Minimum Working Volume : 5000 lit.

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5.2 Batch Inputs & Outputs:

Inputs:-

Table 02:

Input Standard Ratio RM / WIP Specifications, Test Results

Acceptance Criteria

Styrene By GLC Styrene.= 98% (as per RM Specifications)

1 kg

H2O2 50% 0.7818 kg 50 % H2O2

H2O2 30% 1.303 kg (As per RM Specifications)

HCL 32% 32 % HCL (As per RM Specifications)

1.052 kg

Initial Water (2.5%HCL) Acidity of water should be 2.0 – 3.0 % & Iron
1.81 kg content below 2 ppm

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Outputs:-

Table 03:

Output Standard Ratio WIP Specifications, Test Results Acceptance Criteria

Slightly yellowish Liquid,

SCH Crude
1.49 kg Styrene by GLC < 1 % , SDC<0.5%

Benzaldehyde < 3 %, SCH - 90%-93%,

HB < 1.5 %, PH= 3-5

Aqu. layer 1.81 lit

N/A.

-- Styrene by GLC < 0.5 %, SDC - < 7 to 9 %,

1st digestion Benzaldehyde < 3 %, SCH – 85-88 %, HB < 1.5 %.

5.3 Standard Operating Parameters and Time Cycle:

Table 04:

Operation Standard
Time Std.Parameters

Water Charging 30 Min. Room Temp

Heating of initial 2% HCL Water 1-4 Hrs. 90°C.

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Regular Time Cycle

Addition of H2O2,HCL & Styrene 6 Hrs. 94°C - 105°C.

Digestion & Lab analysis after addition 2 Hr. 95°C - 100°C.

Heating to raise temperature & pressure for Digestion 1.5-2 Hrs. 118 -120°C & pressure 1.5 – 2.0
kg/cm2

118 -120°C & pressure 1.5 – 2.0

kg/cm2
Lab analysis after 4 Hr. Digestion 1Hr.

Cooling 1Hr. 120 -90°C & pressure

Settling 1Hr 90 °C.

Crude unloading 30 Min. pH – 4 to 5

Aqu. Layer Transfer 30 Min. 90°C to 95 OC

Total 18 Hrs

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Figure 4 :- Before GLR Monitoring

Figure 5 :- After GLR Monitoring

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Figure 6 :- GLR (Glass Line Reactor)

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5.4 Safety operating procedure:-

1) While charging H2O2, HCL, & Styrene proper precautions should be taken. PPE should be worn.

2) If temp increased above the limit stop addition and starts cooling till the temperature comes
below the limit.

3) If the reaction is not completed, i.e. Un-reacted Styrene is more than 0.5 % ,then add H2O2 as
per un-reacted Styrene % in GLC.

4) If cooling water circulation or bottom circulation pump failure is observed during the reaction,
stop addition & wait till it resumes.

5) While removing the sample from 1 inch valve provided below the sight glass of the bottom valve
of GLR, open and close the sample removing valve Slowly to avoid spillage of liquid

CHAPTER : 06

ADDITIONAL ASSIGNMENTS
6.1 Calibration of storage tanks:

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For Vertical storage tank it is easy to calculate volume of liquid per cm. we just
calculate volume by formulae of cylinder. But for horizontal storage tank we have to calibrate of
volume for every centimetre.

6.1.1 Types of Heads:

Flat Head

Semi Ellipsoidal or Elliptical Head

Torispherical Head

6.1.2 Calibration of vertical tanks :

For calibration of vertical tank we used formula of cylinder : pi*r2*h

If heat of vertical cylinder is flat, we don’t need to mention dish volume.

Dish volume : volume of head.

6.1.3 Calibration of horizontal tanks :

Calibration of horizontal storage tank is different from vertical tank as equal amount of liquid
does not get added in tank as level increases.

Foe horizontal storage tank we must consider total amount of liquid getting filled which includes
fluid in cylindrical part plus head.

6.1.6 Physical Calibration :

Physical calibration of an equipment involes keeping one of parameter constant and calculate
amount of liquid getting filled.

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For the physical calibration of tank we used water as fluid and measured increase in the level of
water with the constant flowrate provided by the pump.

6.2 Pump testing at different operating pressure :

Pump testing of reciprocating pump is done by varying the operating pressure of the pump . this
can be done in two ways by varying the area or varying speed of piston, or both.

We did the pump testing by varying the stokes which nothing but varying the volume transferred
at a time.

6.3 Pipe and instrumentation diagram :

Piping and instrumentation diagram can be done equipment wise or for the whole plant which
involves how the connection is.

We did P&ID for distillation columns to illustrate how and where exactly where pipe and valves
are situated which can be further used to increase safety and control system.

6.4 Tracing and labelling of lines :

We traced and labelled pipes from reactors to distillation columns. Making it easier for the
workers in the company to a quick action in case of any accident.

6.5 Removal of unused pipes and electrical wires :

After tracing the pipes we eliminated those pipes which are not in used also brought in attention
which are critically damaged which could lead to a major accident.

6.6 Monitoring :

Monitoring of distillation columns is also necessary as the parameters as in many cases. These
parameters keep on changing which needs to stabilized for a better yield.

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6.7 Documentation :

We were also involved in documentation involving the daily stock as well as amount of
product produced in a week by production department. The maintenance routine data of pumps
and heat exchangers was also documented by us.

CHAPTER : 07
Hazard and operability study (HAZOP)
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7.1 About HAZOP Study :

A hazard and operability study (HAZOP) is a structured and systematic examination
of a complex planned or existing process or operation in order to identify and evaluate problems
that may represent risks to personnel or equipment. The intention of performing a HAZOP is to
review the design to pick up design and engineering issues that may otherwise not have been
found. The technique is based on breaking the overall complex design of the process into a
number of simpler sections called 'nodes' which are then individually reviewed. It is carried out
by a suitably experienced multi-disciplinary team (HAZOP) during a series of meetings.
The HAZOP technique is qualitative, and aims to stimulate the imagination of
participants to identify potential hazards and operability problems. Structure and direction are
given to the review process by applying standardised guide-word prompts to the review of each
node. The relevant international standard calls for team members to display 'intuition and good
judgement' and for the meetings to be held in 'a climate of positive thinking and frank
discussion'.
The HAZOP technique was initially developed in the 1960s to analyze major
chemical process systems but has since been extended to other areas, including mining
operations and other types of process systems and other complex systems such as nuclear power
plant operation and software development. It is also used as the basis for reviewing Batch
processes and operating procedures.

7.2 Method :
The method is applied to complex 'processes' for which sufficient design
information is available, and not likely to change significantly. This range of data should be
explicitly identified and taken as the ‘design intent’ basis for the HAZOP study. For example, a
prudent designer will have allowed for foreseeable variations within the process creating a larger
design envelope than just the basic requirements and the HAZOP will be looking at ways in
which this might not be sufficient. For processes plant, the nodes are chosen so that for each a
meaningful design intent can be specified and they are commonly indicated on piping and
instrumentation diagram (P&IDs) and process flow diagram (PFD).

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The extent of each node should be appropriate to the complexity of the system
and the magnitude of the hazards it might pose. However, it will also need to balance between
"too large and complex" (fewer nodes, but the team members may not be able to consider issues
within the whole node at once) and "too small and simple" (many trivial and repetitive nodes,
each of which has to be reviewed independently and documented). For each node in turn the
HAZOP team uses a list of standardised guide-words and process parameters to identify potential
Deviations from the design intent. For each deviation, the team identifies feasible Causes and
likely Consequences then decides (with confirmation by subsequent risk analysis where
necessary) whether the existing safeguards are sufficient, or whether an Action to install an
additional safeguard is necessary to reduce the risks to an acceptable level.
The degree of preparation for the HAZOP is critical to the overall success of the
review - 'frozen' design information provided to the team members with time for them to
familiarise themselves with the process, an adequate schedule allowed for the performance of the
HAZOP, provision of the best team members for their role. Those scheduling a HAZOP should
take into account the review scope, the number of nodes to be reviewed, the provision of
completed design drawings and documentation and the need to maintain team performance over
an extended time-frame.
The team members may also need to perform some of their normal tasks during this
period and the HAZOP team members can tend to lose focus unless adequate time is allowed for
them to refresh their mental capabilities. The team meetings should be managed by an
independent, trained HAZOP Facilitator who is responsible for the overall quality of the review,
partnered with a dedicated Scribe to minute the meetings.
"The success of the HAZOP study strongly depends on the alertness and
concentration of the team members and it is therefore important that the sessions are of limited
duration and that there are appropriate intervals between sessions. How these requirements are
achieved is ultimately the responsibility of the study leader." For a medium-sized chemical plant
where the total number of items to be considered is 1200 (items of equipment and pipes or other
transfers between them) about 40 such meetings would be needed. Various software programs
are now available to assist in meetings.

7.3 Guide words and parameters:

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In order to identify deviations, the team applies (systematically, in order ) a set of Guide Words
to each node in the process. To prompt discussion, or to ensure completeness, it may also be
helpful to explicitly consider appropriate parameters which apply to the design intent. These are
general words such as Flow, Temperature, Pressure, Composition. The current standardnotes that
Guide words should be chosen which are appropriate to the study and neither too specific
(limiting ideas and discussion) nor too general (allowing loss of focus).

CHAPTER : 08

Plant View
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Figure 7:- Plant 01

Figure 8:- Dosing pump

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Figure 9:- Condensor

Figure 10:- Cooling Tower

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Figure 11:- Styrene batch Tank

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Figure 12:- R-3 Cooling Tank

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Figure 13:- Storage Tank

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Conclusion

The desired purity of the aromatic chemical Phenyl Ethyl Alcohol was achieved which
was (>99.80%) better than the RM (Raw Material) Specifications i.e. 99.87%. This purity
resulted in better olfactive note. The odour panel was satisfied by the tests carried on the PEA
samples of better purity.
I as a student learnt to be a chemical engineer in production department, quality
control department, R & D Department, Maintenance Dept., Dispatch, etc. A series of training
taught the working of Aldol Condensation, Hydrogenation process, Vacuum Distillation process
in Batch as well as Continuous manner. Training developed overall professional aspect of a
chemical engineer.
The main achievement is that the monitoring of addition reaction because of
decreases residue in 2% per batch i.e, the 10000-15000 profit per batch means, 30000-45000
profit per day.

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References
1. Bhatt BI, Thakore SB(2007). “Stoichiometry”, Fifth Edition, 325-400.
2. M.V Joshi,V.V Mahajani(1996), “Process Equipment design”,Third Edition,209-235.
3. Robert E. Treybal(1980). “Mass Transfer Operations”, Third Edition, 565-585.
4. Perry,R.H and Green(2008), D.W. “Perry’s Chemical Engineers Handbook”, 9th Edition
5. Binay .K. Dutta(2009). “principles of Mass tranfer and seperation Processes”,Third
Edition,319-421
6. D. Q. Kern(1983). “Process Equipment Design”,21st Edition,113-700
7. www.nptel.ac.in
8.

https://www.wikipedia.org/

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