Application for Prior Environmental Clearance Pre-Feasibility Report · 2019-05-09 · Application for Prior Environmental Clearance Pre-Feasibility Report For Proposed Expansion

Prefeasibility Report Deepak Nitrite Limited, MIDC Roha

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Application for Prior Environmental Clearance

Pre-Feasibility Report

For

Proposed Expansion of Agrochemical, Pharma Product & Synthetic Organic Chemical Manufacturing

Category 5 (b) and 5(f)

Prepared By

M/s Deepak Nitrite Limited

Plot No 1-8 & 26-34, MIDC Roha, Dist Raigad, Maharashtra- 402116


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Table of Contents

1 EXECUTIVE SUMMARY ............................................................................................................................................ 4

2 INTRODUCTION OF THE PROJECT ...................................................................................................................... 6

IDENTIFICATION OF THE PROJECT AND PROJECT PROPONENT ......................................................................................... 6 BRIEF DESCRIPTION OF NATURE OF THE PROJECT .............................................................................................................. 7 NEED OF THE PROJECT AND ITS IMPORTANCE TO THE COUNTRY AND/OR REGION ...................................................... 7 DEMAND – SUPPLY GAP ........................................................................................................................................................... 7 IMPORTS VS INDIGENOUS PRODUCTION ................................................................................................................................. 8 EXPORT POSSIBILITY ................................................................................................................................................................ 8 DOMESTIC / EXPORT MARKET ................................................................................................................................................ 8 EMPLOYMENT GENERATION (DIRECT AND INDIRECT) DUE TO THE PROJECT ................................................................ 8

3 PROJECT DESCRIPTION .......................................................................................................................................... 9

TYPE OF PROJECT ...................................................................................................................................................................... 9 LOCATION ................................................................................................................................................................................... 9 DETAILS OF ALTERNATIVE SITES......................................................................................................................................... 10 SIZE OR MAGNITUDE OF OPERATION ................................................................................................................................... 10 PROJECT DESCRIPTION WITH PROJECT DETAILS ............................................................................................................... 13

Project layout ............................................................................................................................................................ 13 Product chemistry, Process description, Process Block Diagram ......................................................... 13

RAW MATERIAL REQUIRED ................................................................................................................................................... 13 Details of Machineries and Utilities required ............................................................................................... 13 Solvent Management plan ................................................................................................................................... 17

WATER, ENERGY / POWER AVAILABILITY AND SOURCE ................................................................................................. 18 Water ........................................................................................................................................................................... 18 Power ........................................................................................................................................................................... 20 Fuel ................................................................................................................................................................................ 20 Manpower .................................................................................................................................................................. 21

WASTE GENERATION, MANAGEMENT AND DISPOSAL ...................................................................................................... 21 Water Pollution ........................................................................................................................................................ 21 Non-Hazardous and Hazardous waste ........................................................................................................... 26 Air Pollution .............................................................................................................................................................. 28

SCHEMATIC OF EIA PURPOSE .............................................................................................................................................. 30

4 SITE ANALYSIS ......................................................................................................................................................... 31

CONNECTIVITY ........................................................................................................................................................................ 31 LAND FORM, LAND USE AND LAND OWNERSHIP ................................................................................................................ 31 TOPOGRAPHY (ALONG WITH MAP) ...................................................................................................................................... 31 EXISTING LAND USE PATTERN .............................................................................................................................................. 31 EXISTING INFRASTRUCTURE ................................................................................................................................................. 31 SOIL CLASSIFICATION ............................................................................................................................................................. 31 CLIMATE DATA FROM SECONDARY SOURCES ..................................................................................................................... 32 SOCIAL INFRASTRUCTURE AVAILABLE ................................................................................................................................ 32

5 PLANNING BRIEF ..................................................................................................................................................... 33

PLANNING CONCEPT .............................................................................................................................................................. 33 POPULATION PROJECTION .................................................................................................................................................... 33 LAND USE PLANNING ............................................................................................................................................................. 33 ASSESSMENT OF INFRASTRUCTURE DEMAND (PHYSICAL AND SOCIAL) ....................................................................... 33 AMENITIES / FACILITIES....................................................................................................................................................... 33

6 PROPOSED INFRASTRUCTURE ........................................................................................................................... 34

INDUSTRIAL AREA (PROCESSING AREA) ............................................................................................................................ 34 SOCIAL INFRASTRUCTURE..................................................................................................................................................... 34 CONNECTIVITY ........................................................................................................................................................................ 34


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DRINKING WATER MANAGEMENT ........................................................................................................................................ 34 SEWAGE SYSTEM .................................................................................................................................................................... 34 EFFLUENT PLANT TREATMENT SYSTEM ............................................................................................................................ 34 INDUSTRIAL WASTE MANAGEMENT..................................................................................................................................... 35 SOLID WASTE MANAGEMENT................................................................................................................................................ 35 POWER REQUIREMENT AND SUPPLY / SOURCE ................................................................................................................. 35

7 REHABILITATION & RESETTLEMENT PLAN ................................................................................................. 36

8 PROJECT SCHEDULE AND COST ESTIMATES ................................................................................................. 37

LIKELY DATE OF START OF CONSTRUCTION AND LIKELY DATE OF COMPLETION ......................................................... 37 ESTIMATED PROJECT COST ................................................................................................................................................... 37

9 ANALYSIS OF THE PROPOSAL (FINAL RECOMMENDATION) ................................................................... 38

List of Annexures Annexure No Description I Google image of study area II Land agreement, Layout plan, Existing land use status III Proposed Water Balance IV Product, Process chemistry and Process description


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1 E XEC UT IVE S UM MA RY

The Deepak Group, with around 50 years of rich heritage and legacy, has been one of the earliest adopters of the ‘Make in India’ philosophy.

Over the years, they have made significant efforts to diversify group’s offerings. Refining our processes; fostering stronger relationships, adopting sustainable practices, we do our best to help shareholders, investors, partners, customers, employees and this planet to flourish.

It has manufacturing sites at Nandesari, Roha, Taloja, Hyderabad and Dahej.

This proposed expansion project is for manufacture of pesticide specific intermediates & synthetic organic chemicals at Company’s existing Plot no 1 to 7 and 26 to 31 and adjacent acquired plot no 8 and 32 to 34, MIDC Roha Industrial area, Tal Roha, Dist Raigad.

The proposed establishment is covered under Category 5(b) and 5(f) as per EIA Notification of Ministry of Environment & Forest (MoEF & CC), dated 14/09/2006 and subsequent amendments.

Therefore, unit requires obtaining prior Environmental Clearance from Ministry of Environment & Forest (MoEF&CC),

The project brief is summarized in the table below, Project summary at a glance,

Table Brief Project summary

Sr No

Particulars Details

1 Name of Company Deepak Nitrite Limited 2 Corporate Office address 1st Floor, Aaditya – II, Chhani Road, Vadodara –

390024. Gujarat, India. 3 Project Location Plot No.1-8, 26-34, MIDC Dhatav, Tal Roha, Dist.

Raigad. 4 Total land area of the plot 34,816 sq m 5 Built up area after expansion 19,943 Sq m 6 Name of the project Proposed manufacture of Agrochemical, Pharma

Product & Synthetic Organic Chemical Manufacturing

7 Estimated project cost Rs. 156 Cores 8 Products Refer section 3.4 9 Raw material Refer section 3.6 10 Water Existing water requirement 524 cmd.

Additional water requirement 1123 cmd. Total 1647 cmd. It will be sourced from MIDC.

11 Power Existing power requirement - 2500 KVA, Proposed for expansion 2500 KVA,


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Total 5000 KVA, which will be sourced from MSEDCL. Existing 3 Nos (750, 750, 500 KVA) of DG sets installed and it is proposed to install 2 No of DG sets each of 1000 KVA for emergency power requirement.

12 Manpower Proposed additional manpower requirement for operational phase will be 50 Nos. (Permanent 25 + Contract 25 = Total 50)

Pollution Potential and mitigation measures 13 Water Pollution Refer section 3.8 14 Air pollution Refer section 3.8

16 Hazardous waste Refer section 3.8 17 Green belt development (1) The unit will develop 3,676 sq m green belt

within plot premises, and (2) within MIDC at plot survey No. 17, 21 and 206

about 8,605 sq m. Total Green belt area= 12,281sq m.


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2 IN T ROD UCTIO N O F T HE P RO JECT

Identification of the Project and Project Proponent

Deepak Nitrite Ltd. is a public limited firm. Details of the directors are given in table below. No Name of Director Designation Qualification Experience,

Years

1 Mr. Deepak C. Mehta

Chairman & Managing Director

B.Sc 41

2 Mr. Umesh Asaikar Executive Director & Chief Executive Officer

B.E., Mechanical Engineering Masters in Management Science, AICWA

40

3 Mr. Ajay C. Mehta Non-Executive Director

B.SC, M.S, in Chemical Engineering

35

4 Mr. Maulik D. Mehta

Whole Time Director

Bachelor in Business Administration & Masters in Industrial and Organizational Psychology

8

5 Ms. Nimesh Kampani

Independent Director

Chartered Accountant 41

6 Mr. Sudhin Choksey


Chartered Accountant 42

7 Mr. Sudhir Mankad


Masters’ degree in History 40

8 Dr. R. H. Rupp Independent Director

Ph.D in Chemistry 38

9 Dr. Swaminathan Sivaram


Ph.D in Chemistry 42

10 Dr. Indira J. Parikh Independent Director

M.A., Ph.D 31

11 Mr. S. K. Anand Independent Director

B.E. Chemical Engineering 47

12 Mr. Sanjay Upadhyay Director-Finance & Chief Financial Officer

M.COM, AICWA, FCS, AMP(Wharton USA)

36

13 Shri Sanjay Asher Additional Director C.A., LLB 27 14 Ms. Purvi Sheth Additional Director Bachelor Degree in Arts,

Economics and Political science

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Regulatory Framework The proposed expansion project is covered under Category 5(b) and 5(f) as per the EIA Notification of Ministry of Environment Forest & Climate Change (MoEF&CC), dated 14/09/2006 and subsequent amendments. Therefore, unit requires obtaining Environmental Clearance from Ministry of Environment & Forest (MoEF&CC).


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As a part of application for obtaining Environmental Clearance, the unit requires to submit Form-1 and Pre-Feasibility Report of the proposed expansion project. The objectives of the report are, a) To assess the feasibility of the proposed project. b) To identify various sources of pollution and anticipate the impacts of the proposed

project on the environment. c) To suggest preventive and mitigation measures to minimize the adverse impacts and

to prepare Environmental Management Plan (EMP). d) Propose the Terms of Reference to carry out EIA Study for the proposed project.

Brief Description of nature of the Project

The proposed expansion project is a brownfield project and is to be executed within the plot. The proposed products are Pesticide specific intermediates & synthetic organic chemicals covered under Category 5(b) and 5(f) as per new EIA notification. The unit believes in sustainable development and equally concern about environment preservation and pollution control. The unit has and will provide an adequate Environmental Management System to meet desired norms of effluent discharge (Water + Air + Solid) as per the statutory requirements for their proposed project and will continue its endeavor for the pollution prevention and betterment of environment.

Need of the Project and Its Importance to the country and/or Region

Deepak Nitrite Ltd. (Deepak Nitrite), the Flagship Company of Deepak Group, is one of India's leading manufacturers of organic, inorganic, fine and specialty chemicals. The company is diversified into manufacturing of Organic intermediates through its in-house expertise, strategic acquisitions and technological collaborations with world leaders. Deepak Nitrite is in operation since more than 3 decades and presently it is a multi-product and multi-location company. DNL has plan to enter into pesticide /agro chemical intermediate segment and expand its product portfolio and capacities of existing products to cater rising demand of the chemicals at national and international market.

Demand – Supply gap

Based on our informal survey of the market with potential customers and various traders, we have found that there is a big demand in the domestic as well as international market for the range of the products we are planning. Also, some of our products will be used captively in manufacturing of various chemicals at our other units located across India.


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Imports vs indigenous production

Continual R & D initiatives have strengthened niche and complex product in in-house development / manufacturing at highly cost-effective processes v/s import of these molecules. This will make us very competitive against imported finished products.

Export Possibility

There is great potential for export.

Domestic / Export market

The finished goods will be sold in domestic market and would be largely exported to the Regulated International Market as per demand all over the world.

Employment Generation (Direct and indirect) due to the project

Proposed unit will give direct employment to local people based on qualification and requirement. In addition to direct employment, indirect employment shall generate ancillary business to some extent for the local population


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3 P RO JECT D ES C RIP T ION

Type of Project

It is project of expansion of the unit for manufacture of Pesticide specific intermediates & synthetic organic chemicals. There is no interlinking of any project.

Location

The proposed expansion will be established in notified MIDC area.

Location of proposed project within MIDC

Brief location details are as follows: No Destination Approx. distance from project

site (km) 1 Nearest town – Roha 4

2 Nearest state highway (NH-66) 5.4 3 Nearest airport – Mumbai 130

4 Nearest railway station - Roha 4

The geographical Location of this Industry is at coordinates, 18°25'37.96"N and 73° 9'33.87"E at elevation above Mean sea level of 12 meters.

Geographical plant site coordinates are as below: Direction Latitude Longitude

North east corner 18°25'39.31"N 73° 9'40.00"E

North west corner 18°25'42.64"N 73° 9'31.24"E

Proposed Project Location(Plot No 1-8, 26-34)


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South east corner 18°25'32.35"N 73° 9'38.74"E

South west corner 18°25'36.37"N 73° 9'28.65"E

Details of Alternative sites

No alternate site examined.

Size or magnitude of operation

The unit proposes to expand manufacturing facility of following products. Existing products/ by products as per Environmental Clearance and Consent to operate is as follows,

Existing Product & By product quantities Sr No

Product / By products Existing

*TPM

1 Para cumidine (PC) OR 3 Amino Benzotri Fluoride (3 ATBF) 200

2 Ortho Anisidine (OA) OR Tri methyl hydro Quinine (TMHQ) 50

3 2,4 Xylidine and 2,6 Xylidine OR 2,3 Xylidine and 3,4 Xylidine OR 2,5 Xylidine OR 2,3 Xylenol OR 2, 4 Xylenol and 2,5 Xylenol

250

4 Diphenyl amine derivatives 50

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Crystal diethyl Meta Amono Phenol ( Cryst. DEMAP) OR Dibutyl Para Phenylene Di amine (DBPPDA) OR 3 NAP (3 Nitro Acetophenone) OR 3 AAP ( 3 Amono Acetophenone) OR 3 HAP ( 3 Hydroxy Acetophenone)

40

6 TFMAP (3 Trifloromethyl acetophenone) 80

7 2 MePPDA Sulphate (2 Methyl p-Phenylene Diamine Sulphate) OR 1,3 CHD (1,3 Cyclohexanedione)

60

8 Pilot plant products (Synthetic orgaqnic chemicals) 10 9 Ortho nitro cumine (from p-Cumidiene) (By product) 150

10 2 NBTF (2 Nitro BTF) / 2 ATBF (2 Amino BTF) / 4 ATBF (4 Amino BTF) from 3 Amino BTF (By product)

41

11 PPO (Poly phenylene oxide / (By product) 135 12 OHBTF/OA BTF From TFMAP (By product) 20 13 Ortho Toludine (OT) (By product) 25

Grant Total 1,111 *Ref : EC letter F No J-11011/363/2016-IA-II(I) dated 2nd January 2018 and 12th April 2018 and Consent order number Format 1.0/BOAST/UAN No. 0000031393/O/CC-1803000099 dated 01.03.2018 valid till 30.06.2019. The unit proposes to expand manufacturing facility at site including existing one (shown above) and add pesticide specific intermediates manufacturing (5(b) activity) as per EC notification). Post expansion total production capacity will be 3,534 TPM. (as against existing 1,111 TPM) i.e. expansion by 2,423 TPM. Post expansion product wise break up after rearranging above will be as follows,


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Post expansion Product quantities Sr No

Product Activity Total Quantity MT/M (after expansion)

1 Para Nitro cumene (PNC) / Para cumidine (PC) OR Ortho Nitro cumene (ONC) /Ortho cumidine (OC)

5(f) & 5(b) 300

2 2 Amino Benzotri Flouride (2ABTF) OR 3 Amino Benzotri Flouride (3ABTF) OR 2 Nitro Benzotri Flouride (2 NBTF) OR 3 Nitro Benzotri Flouride (3NBTF) OR 4 Nitro Benzotri Flouride (4NBTF)

5(f) & 5(b) 400

3 Ortho Anisidine (OA) OR Tri methyl hydro Quinine (TMHQ)

5(f) & 5(b) 100

4 2,3 Nitro-Xylene OR 2,4-Nitro-Xylene OR 3,4 Nitro-Xylene OR 2,6 Nitro-Xylene

5(f) & 5(b) 1330

5 2,3 Xylenol OR 2,4 Xylenol OR 2,5 Xylenol 5(f) & 5(b) 120 6 Phenyl hydrazine OR 4 -Methoxy 2 - Methyl Diphenyl

Amine (MMDPA) 5(f) & 5(b) 100

7 Aniline 5(f) 10 8 3 NAP (3 Nitro Aceto Phenone) 5(f) 60 9 3 AAP (3 Amino Aceto Phenone) 5(f) 48

10 3 HAP (3 Hydroxy Aceto Phenone) 5(f) 30 11 2 MePPDA Sulphate (2 Methyl p-Phenylene Diamine

Sulphate) OR Di-Butyl Para Phenylene Di-amine (DBPPDA) OR 1,3 CHD (1,3 Cyclohexane dione )

5(f) 100

12 Ortho Toludine(OT) 5(f) 46 13 SMIA (syn Methoximino(2 furanyl)acetic acid 5(f) 25 14 Adenine OR PMPA OR S - Alcohol OR DBTZ OR Trimethyl

phenol OR Chlorphenesin OR MethoxyMePPDA OR 2-Acetylfuran OR MTA OR NMTA

5(f) 30

15 Sodium Acetate 5(f) 150 16 Pilot Plant 5(f) 10 17 1,2,4-Triazinone 5(b) 100 18 Thiocarbohydrazide (TCH) 5(b) 19 Dichloropnacolone (DCP) 5(b) 20 2-Cyanophenol 5(b) 150 21 4-Chloro-6-methylanthramide 5(b) 50 22 PPO (Poly Phenylene Oxide) 5(b) 150 23 TFMAP (3-(Trifloromethyl) acetophenone) 5(b) 200 24 CL-BTF / OHBTF / OA BTF from TFMAP 5(b) 25

GRAND TOTAL 3534 Product wise CAS Number and its application in various industries is tabulated below, Sr No

Product CAS No. Product application in

industry type

1 Para Nitro cumene (PNC) / Para cumidine ( PC)

1817-47-6 Agrochemicals intermediate and Pharmaceuticals

2 Ortho Nitro cumene (ONC) / Ortho cumidine ( OC)

6526-72-3

3 3 Amino Benzotri Flouride (3ABTF) 98-16-8

Agrochemicals intermediate and Pharmaceuticals

4 3 Nitro Benzotri Flouride (3NBTF) 98-46-4 5 2 Nitro Benzotri Flouride (2NBTF) 384-22-5 6 4 Nitro Benzotri Flouride (4NBTF) 402-54-0 7 2 Amino Benzotri Flouride (2ABTF) 88-17-5


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8 Ortho Anisidine (OA) 90-04-0 Pharmaceuticals and Agrochemicals intermediate 9 Tri Methyl Hydro Quinine (TMHQ) 700-13-0

10 2,4-Nitro-Xylene 89-87-2


11 2,6 Nitro-Xylene 81-20-9 12 2,3 Nitro-Xylene 83-41-0 13 3,4 Nitro-Xylene 99-51-4 14 2,3 Xylenol 526-75-0


15 2,4 Xylenol 105-67-9 16 2,5 Xylenol 95-87-4 17 Phenyl hydrazine, or 100-63-0 Agrochemical intermediate

18 4 -Methoxy 2 - Methyl Diphenyl Amine (MMDPA)

41317-15-1 Color formers

19 Aniline 62-53-3 Synthetic chemicals 20 3 NAP (3 Nitro Aceto Phenone) 121-89-1

Pharmaceutical intermediate

21 3 AAP (3 Amino Aceto Phenone) 99-03-6 22 3 HAP (3 Hydroxy Aceto Phenone) 121-71-1 23 TFMAP ( 3-(Trifloromethyl) acetophenone) 349-76-8

Agrochemical intermediate 24 CL-BTF / OHBTF / OA BTF from TFMAP

384-22-5/ 88-17-5/ 98-17-9/ 88-

17-5

25 2 MePPDA Sulphate ( 2 Methyl p-Phenylene Diamine Sulphate)

615-50-9 Dyes

26 Di-Butyl Para Phenylene Di-amine (DBPPDA) 101-96-2 Synthetic chemicals 27 1,3 CHD ( 1,3 Cyclohexane dione ) 504-02-9 Agrochemical intermediate 28 Ortho Toludine(OT) 95-53-4 Basic chemical

29 SMIA(syn Methoximino(2 furanyl)acetic acid 97148-39-5 Pharmaceutical intermediate

30 Adenine 73-24-5

Pharma Product & Specialty chemicals

31 PMPA 107021-12-5

32 S-alcohol 132335-44-5

33 N-methyl Duloxetine oxalate

136434-34-9 (HCl salt)

132335-47-8 (N-methyl duloxetine

oxalate) 34 DBTZ 460029 35 Trimethyl phenol 2416-94-6 36 Chlorphenesin 104-29-0 37 MethoxyMePPDA 337906-36-2

38 2-Acetylfuran 1192-62-7 39 MTA 54396-44-0 40 NMTA 5437-38-7 41 Sodium Acetate 127-09-3 Textile industry 42 Pilot Plant - - 43 1,2,4-Triazinone 33509-43-2

Pesticides and agrochemical intermediates.

44 Thiocarbohydrazide (TCH) 2231-57-4 45 Dichloropnacolone (DCP) 22591-21-5 46 2-Cyanophenol 611-20-1 47 4-Chloro-6-methylanthramide 890707-28-5 48 PPO (Poly phenylene Oxide) 25134-01-4

http://www.commonchemistry.org/ChemicalDetail.aspx?ref=337906-36-2


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Project description with Project details

Project layout

Refer Annexure II

Product chemistry, Process description, Process Block Diagram

Process block diagram and material required is mentioned at Annexure IV.

Raw material required

Various raw materials will be required for manufacturing of proposed products. Details of raw material requirement for proposed project are given below: Raw Materials: The detailed raw material list for product, mixed products as per selected capacity is tabulated in Annexure IV. Source for Raw Material Procurement: Raw Materials are easily available in the local market, from Mumbai and Gujarat. Part of the raw materials are generated In-house and used internally and some raw material will be imported. Mode of Transport of Raw Materials: Raw Materials will be transported through Trucks/ Tankers from supplier’s factories or traders go-downs. Those which are in house will be transported through internal pipelines as per the requirements. Storage at the site: Raw Materials will be stored in storage yard at the project site. Location of storage yard is demarcated in Layout Plan.

Details of Machineries and Utilities required

As the proposed expansion project will have different production plants for the manufacturing of various products, large number of plant machineries, equipment and utilities will be required. Also, existing plant will facilitate requirement of some of the machineries and utilities. The lists of plant machineries for the proposed project are given in following Table. However, the actual requirements of machineries and equipment are not limited to the basic list below as some minor requirements can also be cited depending up on necessity noticed during installation & operations.


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Details of Proposed Equipment and Machineries Sr. No

Reactor/ vessel/ equipment MOC/Type Qty Size/Capacity

1 Reactors Glass lined 2 12.5 KL, 25 KL

2 Reactors MS 2 8 KL, 10 KL 3 Reactors SS 14 5 KL- 11 KL, 16KL, 22 KL 4 Distillation set SS/MS 5 6 KL, 7 KL, 8 KL, 16L 5 Centrifuge/Decanter SS/MS 2 10 m3/hr 6 Nutsche Filter SS/MS 2 3.5 KL, 5 KL

7 Condensers SS/MS 8 5 m2, 15 m2, 20 m2,

25 m2, 38 m2 8 Chillers -- 5 1000TR

9 Blowers -- 6 500 CFM, 1,000 CFM,

1,500 CFM 10 Cooling Tower -- 2 1000 TR 11 Air compressor -- 1

12 RO -- 1

13 MEE -- 1 14 Boiler (20 TPH) -- 1 15 Thermopack (10 Kackcal/hr) -- 1

BULK LIQUID STORAGE TANK DETAILS

Detailing of Storage tanks along with their required capacities is tabulated below:


15

18 100 3.57 0.59 2.12 2.12

34 50 1.79 1.56 2.79 2.79

2 BTF 6 400 14.29 1.21 17.29 17.29 17.29 1190 44

3 Cumene 1,2 300 10.71 1.34 14.36 14.36 14.36 862 50

4 m-Xylene 10,11 500 17.86 0.95 16.96 16.96 16.96 860 59

5 o-Xylene 12,13 1330 47.50 1.78 84.55 84.55 84.55 880 288

6 3-ABTF 23 200 7.14 1.26 9.00 9.00 9.00 1290 21

37 30 1.07 3.34 3.58 3.58

34 50 1.79 1.30 2.32 2.32

Class B tank farm

7 DMF 5.90 944 19

Quantity

required

(MT/day)

Group wise

quantity

required

(MT/day)

Total quantiy

required

(MT/day)

density

(kg/cubic

meter)

Required

holdup

Capacity

(kL)

1 DMS 4.91 840 18

Sr No. Name of CompoundProduct

Number

Product

(MT/month)

Product

(MT/Day)

Quantity

(MT/MT

product)


16

34 50 1.8 18.02 32.2

46 30 3.6 6.76 24.1

10,11 500 17.9 0.58 10.4

12,13 1330 47.5 1.17 25.1

1,2 300 10.7 1.09 11.7

6 400 14.3 0.76 10.9

8 50 1.8 0.68 1.2 1.2

18 100 3.6 1.00 3.6 3.6

20 60 2.1 0.83 1.8 1.8

45 30 1.1 0.86 0.9

46 30 1.1 0.93 1.0

34 50 1.8 2.39 4.3 4.3

1,2 300 10.7 1.73 18.6

6 400 14.3 2.52 36.0

8 50 1.8 0.68 1.2 1.2

10,11 500 17.9 0.49 8.8

12,13 1330 47.5 1.21 57.5

14 120 4.3 1.06 4.5

15 120 4.3 1.47 6.3

16 120 4.3 1.05 4.5

18 100 3.6 0.05 0.2 0.2

20 60 2.1 0.84 1.8

22 30 1.1 3.92 4.2

23 200 7.1 1.39 9.9 9.9

25 100 3.6 0.61 2.2 2.2

30 100 3.6 0.72 2.6 2.6

36 30 1.1 2.30 2.5

43 30 1.1 10.34 11.1

45 30 1.1 4.92 5.3

33 150 5.4 0.41 2.2 2.2

3 HBr 18 100 3.6 0.18 0.7 0.7 0.65 1490 1

21 48 1.7 0.059 0.1 0.1

23 200 7.1 0.16 1.1 1.1

5 AAO 23 200 7.1 0.56 4.0 4.0 3.96 969 12

14 120 4.3 1.19 5.1

15 120 4.3 1.20 5.1

16 120 4.3 1.17 5.0

41 30 1.1 1.00 1.1 1.1

7 Formamide 36 30 1.1 2.67 2.9 2.9 2.86 1130 8

17 100 3.6 8.01 28.6 28.6

23 200 7.1 1.57 11.2 11.2

27 100 3.6 1.38 4.9 4.9

29 25 0.9 7.52 6.7 6.7

9 Dichloro Pinacolone 30 100 3.6 1.016 3.6 3.6 3.6 801 14

10 Aniline 36 30 1.1 1.45 1.6 1.6 1.6 1020 5

18 100 3.6 0.81 2.90 2.90

23 200 7.1 1.56 11.14 11.14

27 100 3.6 1.10 3.93 3.93

29 25 0.9 1.17 1.04 1.04

30 100 3.6 1.80 6.43

31 100 3.6 0.09 0.31

36 30 1.1 2.74 2.94

37 30 1.1 1.32 1.41

38 30 1.1 2.96 3.17

39 30 1.1 0.60 0.64

40 30 1.1 0.59 0.63

42 30 1.1 0.76 0.81

45 30 1.1 0.98 1.05

17 100 3.6 2.31 8.25 8.25

33 150 5.4 0.47 2.52 2.52

Class C tank farm

Quantity

required

(MT/day)

Group wise

quantity

required

(MT/day)

Total quantiy

required

(MT/day)

density

(kg/cubic

meter)

Required

holdup

Capacity

(kL)

1 98% Nitric Acid

32.2

57.25 1510


Number

Product

(MT/month)

Product

(MT/Day)

Quantity

(MT/MT

product)

114

25.1

1 72% Nitric Acid

22.6

34.4 1350.0 76

1.0

2 98% Sulphuric acid

36.0

133.30 1840.00 217

57.5

6.3

4.2

11.1

4 Acetic acid 1.24 1050 4

6 Xylidines5.1

6.21 993

11 48% Caustic Soln 39.38 1510 78

6.43

3.17

19

8 30% HCl 51.45 1150 134


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Solvent Management plan

Unit will require various solvents for manufacturing of proposed products. There will be generation of spent / mix solvent during the manufacturing process. It will be separated and sent to offsite distillation units who are authorized recyclers, or recovered in-house and reused in process or sold to authorized end-users having permission under rule 9 of “Hazardous and Other Wastes (Management & Trans-boundary Movement) Rules, 2016. Details of solvent requirement and spent/mix solvent generation are given in following table:

9 0.56 1.8 23.5 23.5 19.04

18 0.03 3.6 9.8 9.8 6.56

22 0.23 1.1 7.4 7.4 0.00

25 0.08 3.6 14.1 14.1 5.47

29 0.67 0.9 23.3 23.3 5.35

37 4.44 1.1 142.7 0.00

40 0.13 1.1 5.5 1.29

41 1.10 1.1 36.0 0.64

43 14.11 1.1 460.0 6.48

33 0.64 5.4 123.0 20.10

34 3.40 1.8 198.7 16.59

9 0.22 1.8 9.3 9.3 7.53

15 0.22 4.3 47.6 19.33

17 0.33 3.6 43.7 8.36

22 0.08 1.1 6.7 6.7 4.10

23 0.13 7.1 46.1 46.1 18.21

37 1.07 1.1 34.3 0.00

38 1.19 1.1 40.6 2.36

39 0.07 1.1 7.0 4.69

40 0.61 1.1 23.7 4.13

42 0.96 1.1 33.3 2.40

43 12.21 1.1 393.9 1.45

3 MEK 26 0.74 3.6 79.9 79.9 79.9 0.16

4 Methylene Dichloride 37 4.38 1.1 140.8 140.8 140.8 0.00

14 0.10 4.3 21.3 8.83

16 3.45 4.3 454.3 10.71

37 4.44 1.1 142.7 0.00

38 15.44 1.1 500.5 4.19

39 4.62 1.1 153.4 4.95

7 Carbon Disulphide 31 0.83 3.6 88.9 88.9 88.9 0.00

27 0.11 3.6 19.0 19.0 19.0 7.21

39 0.52 1.1 16.7 16.7 16.7 0.00

34 1 1.8 64.1 64.1 64.1 10.58

9 Acetone 37 0.98 1.1 31.5 31.5 31.5 0.00

10 EDC 44 0.447 1.1 17.64 17.64 17.6 3.27

11 1-propanol 43 10.37 1.1 337.0 337.0 337.0 3.71

Generation

as Spent

Solvent,

TPM

736.9

503.6

454.3

500.5

Total,

TPM

8 Ethyl Acetate

Quantity

(MT/MT

product)

Product

(MT/Day)Product

Wise TPM

Group

Max,

TPM

Requirement

460.0

198.7

47.6

393.9

454.3

500.5

2 Toluene

5Methyl Isobutyl Ketone

(MIBK)

6 Isopropyl Alcohol


Number

1 Methanol


18

Resource optimization-

To conserve the water, various recycle/ reuse schemes will be implemented. Most energy efficient technology will be selected.

Water, Energy / Power availability and source

Water

Total amount of required process water is tabulated below:


19

Product Max. Qty Max. QtyWater

consumptionWater requirement

Water

requirement (Max.)

(MT/M) (MT/Day) MT/MT MT/Day

1Para Nitro cumene ( PNC ) / Para

cumidine ( PC)10.71 14.41 154.4

2Ortho Nitro cumene ( ONC ) /

Ortho cumidine ( OC) 0.00 0 0.0

33 Amino Benzotri Flouride (3ABTF)

14.29 2.87 41

4 3 Nitro Benzotri Flouride (3NBTF) 0.00 0 0.0



72 Amino Benzotri Flouride (3ABTF)

0.00 0 0.0

8 Ortho Anis idine (OA) 50 1.79 3.41 6.1 `

9 Tri Methyl Hydro Quinine (TMHQ) 50 1.79 8.86 15.8 16

10 2,4-Nitro-Xylene 17.86 8.12 145.0

11 2,6 Nitro-Xylene 4.46 0 0.0

12 2,3 Nitro-Xylene 4.35 206.6

13 3,4 Nitro-Xylene 0 0.0

14 2,3 Xylenol 4.29 6.39 27.4

15 2,4 Xylenol 4.29 7.33 31.4

16 2,5 Xylenol 4.29 5.24 22.5

17 Phenyl hydrazine 100 3.57 11.63 41.5

184 -Methoxy 2 - Methyl Diphenyl

Amine (MMDPA)100 3.57 5.87 21.0 21.0

19 Ani l ine 10 0.00 0 0.0 0

20 3 NAP (3 Nitro Aceto Phenone) 60 2.14 7.71 16.5

21 3 AAP (3 Amino Aceto Phenone) 48 1.71 6.47 11.1

22 3 HAP (3 Hydroxy Aceto Phenone) 30 1.07 13.52 14.5

23TFMAP ( 3-(Tri floromethyl )

acetophenone) 200 7.14 10.68 76.3

24CL-BTF / OHBTF / OA BTF from

TFMAP25 0.89 0 0.0

252 MePPDA Sulphate ( 2 Methyl p-

Phenylene Diamine Sulphate)3.57 7.91 28.3

26Di-Butyl Para Phenylene Di -amine

(DBPPDA) 3.57 0.00 0.0

27 1,3 CHD ( 1,3 Cyclohexane dione ) 3.57 1.55 5.5

28 Ortho Toludine(OT) 46 1.64 0.00 0.0 0

29SMIA(syn Methoximino(2

furanyl )acetic acid25 0.89 7.84 7.0 7

30 1,2,4-Triazinone 3.57 11.68 41.7

31 Thiocarbohydrazide (TCH) 3.57 1.11 4.0

32 Dichloropnacolone (DCP) 3.57 0.00 0.0

33 2-Cyanophenol 150 5.36 6.87 36.8

34 4-Chloro-6-methylanthramide 50 1.79 35.00 62.5

35 PPO (Poly phenylene Oxide) 150 0.00 0.00 0.0 0

36 Adenine 1.07 47.72 51.1

37 PMPA 1.07 12.00 12.9

38 S-a lcohol 1.07 1.00 1.1

39 N-methyl Duloxetine oxa late 1.07 3.00 3.2

40 DBTZ 1.07 26.88 28.8

41 Trimethyl phenol 1.07 0.76 0.8

42 Chlorphenes in 1.07 5.00 5.4

43 MethoxyMePPDA 1.07 55.69 59.7

44 2-Acetyl furan 1.07 5.70 6.1

45 MTA 1.07 3.63 3.9

46 NMTA 1.07 10.31 11.0

772

120

Product No.

300

400

154

41

1330

47.50

60

63

207

42

17

76

28

42

100

Total Water Consumption per day, CMD

30.00

100


20

(Note: Water consumption arrived based on worst case scenario for group of products)

Details of existing and proposed water requirement is as follows, Sr. No.

Consumption details Existing Quantity, cmd

Proposed Quantity, cmd

Total Quantity, cmd

1 Domestic 35 5 40 2 Industrial process 333 439 772

3.1 Industrial cooling 80 500 580 3.2 Boiler 76 144 220 4 Gardening 0 35 35 Total 524 1123 1647

Water will be sourced from MIDC. About 483 CMD treated waste water recycled and fresh water requirement will be up to 1164 CMD.

Power

Existing requirement 2500 KVA, proposed for expansion 2500 KVA, Total 5000 KVA, which will be procured from MSEDCL.

Fuel

Existing 3 Nos (750, 700, 500 KVA) of DG sets installed and it is proposed to install 2 No of DG sets each of 1000 KVA for emergency power requirement. Total D.G. Set capacity is 3950 KVA.

Table: Details of Stack

S. No

Particulars

Capacity Stack

Ht., mtr. Fuel

Fuel consumption

Stack Dia(mm)

Stack gas

temp(˚C)

Existing

1 *Boiler 8 TPH 34 Coal 32.83 TPD 1200 145

2 Thermo pack

6 Lakh Kcal/Hr

3 *Boiler 8 TPH 24.5

FO 11.25 KLD 1000 145

4 Hot Oil Unit 4 Lakh

Kcal/Hr Coal 4 TPD

5 Hot Oil Unit 4 Lakh

Kcal/Hr 20 FO 20.83 kg/hr 600 145

6 DG Set 750 KVA

3.5**

HSD 200 Lit/hr

400 165 7 DG Set 750 KVA HSD 200 Lit/hr

8 DG Set 500 KVA HSD 162 Lit/hr

9 Scrubber- NOx

-- 8.5** -- -- 300 --


21

S. No

Particulars

Capacity Stack

Ht., mtr. Fuel

Fuel consumption

Stack Dia(mm)

Stack gas

temp(˚C)

Proposed

10 Boiler 20 TPH 36 Coal

70 TPD 1250 140

11 Thermo pack 10 Lakh Kcal/Hr

5 TPD

12 D.G. Set 1000 KVA

3.5** HSD 250 Lit/hr

400 165 13 D.G. Set

1000 KVA

HSD 250 Lit/hr

14 Scrubber- SOx -- 8.5** -- -- 300 --

15 Scrubber- HCl -- 8.5** -- -- 300 --

Note: * Boiler Sr. No. 1 or Sr. No. 3 either of one will be run at a time and other will be remain as standby. ** Stack height above roof level.

Manpower

Expected manpower requirement for operational phase of the project will be

Description Permanent, No Contracts, No Total, No

Existing 195 225 420

Proposed additional 25 25 50

Total 220 250 470

Waste generation, Management and disposal

Water Pollution

Total Quantity of effluent generated from different processes is tabulated below:


22

Max. Qty Max. QtyEffluent

QuantityEffluent Gen.

(MT/M) (MT/Day) MT/MT (MT/Day)

1Para Nitro cumene (

PNC ) / Para 10.71 9.75 104.5

2Ortho Nitro cumene

( ONC ) / Ortho 0.00 0 0.0

33 Amino Benzotri

Flouride (3ABTF) 14.29 2.72 38.9

43 Nitro Benzotri

Flouride (3NBTF) 0.00 0 0.0

52 Nitro Benzotri


64 Nitro Benzotri


72 Amino Benzotri

Flouride (3ABTF) 0.00 0 0.0

8 Ortho Anisidine (OA) 50 1.79 3.76 6.7 7

9Tri Methyl Hydro

Quinine (TMHQ) 50 1.79 9.19 16.4 16

10 2,4-Nitro-Xylene 17.86 2.99 53.4

11 2,6 Nitro-Xylene 4.46 0 0.0

12 2,3 Nitro-Xylene 2.19 104.0

13 3,4 Nitro-Xylene 0 0.0

14 2,3 Xylenol 4.29 8.76 37.5

15 2,4 Xylenol 4.29 7.51 32.2

16 2,5 Xylenol 4.29 8.43 36.1

17 Phenyl hydrazine 100 3.57 25.40 90.7

18

4 -Methoxy 2 -

Methyl Diphenyl

Amine (MMDPA)

100 3.57 6.84 24.4 21.00

19 Aniline 10 0.00 0 0.0 0

203 NAP (3 Nitro

Aceto Phenone)60 2.14 3.06 6.6

213 AAP (3 Amino

Aceto Phenone) 48 1.71 6.73 11.5

223 HAP (3 Hydroxy

Aceto Phenone) 30 1.07 5.61 6.0

12091

Product

No.Product

300

400

Max Effluent

product

1330

47.50

104

Comparative Statement of Effluent Load

104

39

12


23

Max. Qty Max. QtyEffluent

QuantityEffluent Gen.

(MT/M) (MT/Day) MT/MT (MT/Day)

23

TFMAP ( 3-

(Trifloromethyl)

acetophenone)

200 7.14 14.82 105.8

24CL-BTF / OHBTF /

OA BTF from TFMAP25 0.89 0 0.0

25

2 MePPDA Sulphate

( 2 Methyl p-

Phenylene Diamine

Sulphate)

3.57 5.00 17.9

26Di-Butyl Para

Phenylene Di-amine 3.57 0.39 1.4

271,3 CHD ( 1,3

Cyclohexane dione ) 3.57 4.01 14.3

28 Ortho Toludine(OT) 46 1.64 0.00 0.0 0.00

29

SMIA(syn

Methoximino(2

furanyl)acetic acid

25 0.89 25.64 22.9 23

30 1,2,4-Triazinone 3.57 17.91 64.0

31Thiocarbohydrazide

(TCH)3.57 2.70 9.6

32Dichloropnacolone

(DCP)3.57 0.40 1.4

33 2-Cyanophenol 150 5.36 7.01 37.6

344-Chloro-6-

methylanthramide50 1.79 30.12 53.8

35PPO (Poly phenylene

Oxide)150 0.00 0.00 0.0 0.00

36 Adenine 1.07 48.15 51.6

37 PMPA 1.07 17.49 18.7

38 S-alcohol 1.07 16.63 17.8

39N-methyl Duloxetine

oxalate 1.07 4.46 4.8

40 DBTZ 1.07 38.51 41.3

41 Trimethyl phenol 1.07 0.42 0.5

42 Chlorphenesin 1.07 3.90 4.2

43 MethoxyMePPDA 1.07 39.40 42.2

44 2-Acetylfuran 1.07 8.55 9.2

45 MTA 1.07 6.42 6.9

46 NMTA 1.07 25.66 27.5

710

Product

No.Product

Max Effluent

product

Effluent Generation per day

100

30 52

100 64

54

105.83

18


24

(Note: Effluent load arrived based on worst case scenario for group of products) Summarized quantity of effluent generated is tabulated below:

Sr. No.

Type of effluent Existing quantity

CMD

Proposed additional quantity,

CMD

Total

Treatment / Disposal

1 Domestic 31 4 35 It will be treated in independent STP plant. Treated water will be used for gardening.

2 Trade effluent

2.1 From Process 240 470 710

It will be treated at ETP consisting of Stripper MEE, Primary, secondary and tertiary treatment, RO and MEE. About 247 CMD Treated waste water will be sent to CETP.

2.2 From utilities 7 25 32 Total 278 499 777

Details of total water consumed is as follows,

Particular Consumption (cmd) Loss (cmd) Effluent (cmd) Water

requirement Existing Proposed Total Existing Proposed Total Existing Proposed Total

Domestic 35 5 40 4 1 5 31 4 35 Industrial

process 333 439 772 93 -31 62 240 470 710

Cooling tower/ Boiler

156 644 800 149 619 768 7 25 32

Gardening 0 35 35 0 35 35 0 0 0 Total 524 1123 1647 246 624 870 278 499 777

Domestic effluent will be treated separately in proposed STP. Treated domestic waste water will be reused for gardening, floor washing flushing, spraying on coal etc. Treatment Scheme for Trade Effluent The total effluent generation will be 777 cmd. Effluent generation from manufacturing process 710 cmd, utilities (Boiler and Cooling Tower) 32 cmd and domestic 35 cmd. Low concentrated effluent 32 cmd from utilities (boiler and cooling tower) and manufacturing processes 368 cmd will be directly sent to ETP for further treatment and around 247 CMD low concentrated effluent sent to RO along with 153 CMD ETP treated effluent. RO reject will be sent to MEE for further treatment. RO permeate and MEE Condensate will be recycled into process or utility. MEE sludge disposed to CHWTSDF. High concentrated effluent generated from manufacturing process 95 cmd will be collected and treated in Stripper & MEE. Condensate will be recycled in process/utility.


25

The treated water 247 CMD will be sent to CETP. ETP treatment scheme-

1. Primary Treatment

The system will be designed to treat 400 cmd of waste water. Wastewater from Different process, which has gone through MEE treatment along with wastewater from cooling tower, boiler blow down and low concentrated process wastewater. etc. will be collected in the Equalization Tank and air stripped. This effluent will be then be pumped to the Flash Mixer where it is dosed with alum for coagulation. Flash Mixer is followed by a flocculator where poly will be dosed for bigger flock formation. This effluent is overflowed into the settling tank where the solids will be settled down and removed.

2. Secondary (Aerobic) Treatment:

The system will be designed to treat 400 cmd waste water. The neutralized effluent will enter the bioreactor. In the bio reactor, dissolved organic material is degraded by the micro–organisms present in the bio reactor. Oxygen required for the oxidation of organic matter will be provided by means of proposed diffuser aeration system which will mix the contents of the bioreactor. The mixed liquor will overflow into Secondary Settling Tank (SST). In the secondary settling tank, solid-liquid separation takes place and solids i.e. biomass will settle at the bottom of the tank. Settled biomass will be recycled to the bio reactor for maintaining the MLVSS concentration by using proposed sludge recycle pumps and excess biomass will be wasted periodically to the sludge sump. Two stage treatments are proposed where the overflow from the 1st stage clarifier will enter the 2nd stage bioreactor where the non-degraded organics from the 1st stage bioreactor will be treated. The clear overflow from the 2nd stage Secondary Settling Tank will be Collection in the intermediate sump. 3. Tertiary Treatment: The system will be designed to treat 400 KLD of waste water. The clear effluent from the intermediate sump will be pumped by tertiary Feed pumps through the pressure sand filter (PSF) & activated carbon filters. The final treated effluent will be Collected in the final Collection tank from where it is discharge to CETP (247 CMD). 4. RO & MEE (Proposed) Balance treated effluent from ETP and low COD effluent from process is send to RO plant (400 CMD). RO permeate is recycled back to utility and reject send to MEE Plant (80 CMD) for treatment. MEE condensate recycled back into utility and Sludge (Salt) disposed to CHWTSDF. 5. Sludge Handling: Primary sludge, excess biomass from the secondary treatment and backwash water from PSF will be collected in the sludge sump. From the sludge sump the sludge will be


26

pumped to the decanter/valuate for dewatering. The solid cake from the decanter/valuate will be sent for disposal to Hazardous waste disposal site. The filtrate from the decanter/valuate will be drained to the collection tank. Design details and Performance Projection of ETP are tabulated below: Sr. No

Parameters Units Inlet effluent Characteristics

Outlet Effluent Characteristics

Effluent Discharge Standards(MPCB)

1 Designed quantity

Cubic m/ day

1000 1000 ---

2 pH --- 4-9 6.9-7.3 6.5-9 3 BOD (at 27

deg. C) mg/L 400-650 50-95 <100

4 COD mg/L 1500-3000 175-230 <250 5 TSS mg/L 350-450 35-75 <100 6 TDS mg/L 3000-4000 1900 <2100 7 Oil and

Grease mg/L 10-20 5-6 <10

Non-Hazardous and Hazardous waste

The quantification of nonhazardous and hazardous waste generated from present and proposed activities is tabulated as below:

Non-Hazardous waste details & disposal

Sr. No.

Type of Waste Existing Proposed Total UOM Disposal

1 Insulation Material 2 2 4 MT/A Sale to Authorized party

2 MS/SS scrap 0 7 7 MT/M Sale to Authorized party

3

Wood, Paper, decontaminated plastic, Rubber material, PVC material, Tarpaulin, Filter Bags etc.

2 5 7 MT/A Sale to Authorized party

4 Glass ware/ broken/discarded glass

1 1 2 MT/A Sale to Authorized party

5 Boiler ash 2.5 8.5 11.0 MT/Day Sale to brick manufacturing /Landfill

6 Thermo pack Ash 0 2 2 MT/M Sale to brick manufacturing /Landfill

7 Canteen waste 0 0.7 0.7 MT/M Send to viniculture


27

Action plan for disposal of Fly ash generated from Boiler Coal will be used as fuel in boiler and generated ash shall be collected and sold out to nearest brick manufacturer and land filling. Details are shown in table as above.

The main source of hazardous waste generation from proposed plant is dried sludge from ETP and various process wastes. The ancillary source of hazardous waste is used oil from plant & machinery and discarded containers/bags/liners from storage and handling of raw materials. Unit will obtain membership from various CHWIF/TSDF facilities for additional quantity of hazardous waste generated. The details of hazardous waste generation and handling/ Management are given in following table.

Apart from effluent, generated amount of hazardous solid waste is categorized below:

Hazardous waste details & disposal

Sr. No.

Type of waste Categ

ory

Generation Total UOM

Source of Generation

Disposal Existing Proposed

1 Used/spent oil Sch.-1

5.1 91 25 116 MT/A

From plant and machinery

Collection, Storage, Transportation and disposal by selling

to registered recyclers

OR Reused as Lubricant within

premises

2

Wastes or residues containing oil (cotton/gaskets/ insulation materials)

Sch.-1 5.2

0 1 1 MT/M From plant and

machinery

Sale to actual users having

permissions/ CHWTSDF

3 Dilute Sulfuric Acid

Sch. 2 C2

836 2135 2971 MT/M From Manf.

Process 1, 3, 10, 11, 12, 13, 22, 45

Sale to actual users

4 Spent Chemicals Sch.-1 32.1

91 0 91 MT/M

From Manufacturing

process 1, 3, 10, 11, 12, 13, 22, 45

Sale to actual users /CHWTSDF

5 Sludge from treatment of waste water

Sch.-1 34.2

1778 2510 4288 MT/A From Process Stripper-MEE-

ATFD

CHWTSDF/Co-processing /Sale to

actual users

6 Discarded containers/ barrels/ liners

Sch.-1 33.3

25 125 150 Nos./

M Raw Material

Handling

Collection, Storage, and Disposal by

selling to registered scrap

vendors

7 Waste from waste water

treatment

Sch.-1 35.3

50 50 100 MT/M From ETP

Collection, Storage, Transportation and

Disposal by landfilling at TSDF

/ Co-processing


28

8 Spent Catalyst Sch.-1 29.5

0.07 14.23 14.3 MT/M

From Manufacturing

Process 3, 9, 18, 26, 30, 34, 36, 45

Collection. Storage, Regeneration & Re-

use

9

Distillation Residues from contaminated organic solvent

Sch.-1 38.1

28 298.8 326.8 MT/M

From Manufacturing

Process 1, 3, 10, 13, 14, 15, 16, 22, 23, 25, 38, 39, 40,

41, 42, 43, 44

CHWTSDF/co-processing

10 MEE salts Sch.-1 36.1

0 47 47 MT/M From MEE

process

Collection, Storage, Transportation and

Disposal by landfilling at TSDF

/ Co-processing

11 Iron Sludge/ Iron Oxide

Sch.-1 35.3

0 124 124 MT/M From

Manufacturing Process 21,40

Sale to actual users /TSDF

12 Charcoal Sludge Sch.-1 36.2

0 21.7 21.7 MT/M From

Manufacturing Process 9, 22,36


13 Spent / Mix Solvent

Sch - 1 28.6

0 208 208 MT/M

Mfg. of various Products

Collection, Storage and sent for off-site

distillation OR Recovered in-

house and re-use OR Sell to

authorized end-users

14 Filter pads/Bags Sch.-1 36.2

0 2 2 MT/M From Filtration and centrifuge

operation


E-Waste and Lead Acid Batteries

Sr. No.

Type of waste Categor

y

Generation Total UOM

Source of Generation

Disposal Existing Proposed

1 E-Waste -- 0 50 50 Kg/M Electronics

and electrical waste items

Sale to authorized

party

2 Lead acid batteries

-- 0 20 20 Nos./A Power Back

Up /UPS

Sale to authorized

party

Air Pollution

Main source of air pollution is flue gas and process gas generation from existing plant. There are chances of fugitive emission due to manufacturing activities and raw material handling and transportation. There will not be any flue gas generation from proposed expansion project. There will be any process gas generation from proposed expansion project. There will be chances of fugitive emission due to manufacturing activities and raw material handling and transportation. Various sources of air pollution are described hereunder:

(A) Process Gas Generation

There is process gas generation in the form of NOx, SO2, HCl. Unit will provide adequate scrubbing system (water / acid / alkali scrubbers) to control emission of process gas


29

into atmosphere. Details of proposed process gas stack are given in Table section 3.7.3. Schematic diagram of air pollution control measures are given in subsequent figure.

(B) FUGITIVE EMMISION

There will be a chance of fugitive emission and odor nuisance during manufacturing process as well as due to storage & handling of fuel, raw materials and products. Unit has provided multi cyclone and bag filter to control the fugitive dust emission from coal crushing and handling which is connected with common stack of Coal Fired Boiler (16 TPH). The unit takes following precaution for the control of fugitive emission and will implement the same for the proposed expansion.

Probable Sources Control Measures Manufacturing activities during charging into reactors

• Liquid raw materials are charged by pumping & closed loops.

• Dosing is done by metering system to avoid fugitive emissions.

• Dedicated measuring tanks are provided to each reactor. • Usage of closed handling system for odorous chemicals

/ solvents as far as possible. Solvent handling during filling and withdrawal from tanks and vessels

• Breather valves, PSVs, Rupture discs are installed for process/storage tank vents.

• Vapor recovery systems are provided at required locations. • Proper Control of the operating parameters,

mainly temperature, vacuums, cooling media circulation, during plant operation and solvent recovery.

Chemical vapor from wet cake in filtration and drying area

• Covered transfer systems will be adopted, workers shall be provided PPE.

• Fume extraction systems will be provided, wherever required

Emission from bulk storage tanks during storage, loading, unloading

• Breather valves, PSVs, Rupture disc, Vapor recovery system are installed for process/storage tank vents.

• Unit adopts bulk handling of odorous chemicals and avoid usage of drums/carboys for such materials

Coal storage & handling area • Pneumatic feeding system is provided with closed conveyor belt.

• Multicyclone with bag filters are provided in coal handling area

• Water sprinkling system in coal storage yard is provided. Hazardous chemical storage area

• Dedicated storage area is provided • Adequate ventilation systems are provided • All the containers are kept tightly closed • Trolley/Forklift is used for transfer of drums and

containers • Transfers of odorous waste are preferably during day time.

Transfers during odd hours are avoided. Pump and compressor missions

• Mechanical seals are provided in pumps and agitators • Standby arrangement for critical equipment and parts is

ensured. • Drip trays will be placed for each pump to collect leakages


30

-

and spillages.

Pressure relief valve emission from pipelines

• For highly pressurized lines, vent pipes of PRVs are connected in case of toxic gases.

Valves, Flanges, plugs and instrument connections

• Welded pipes are used wherever feasible. • Suitable gasket materials are used. • Suitable glad packing is used in valves. • Periodic inspection and maintenance of pipes and pipe

fittings is carried out. Release from sampling lines • Closed loop system is used.

Schematic of EIA Purpose

Figure below indicates schematic representation of the feasibility drawing which gives EIA purpose


31

4 S IT E ANALYS IS

Connectivity

Industrial area where the plant is to be located, comes in Taluka Roha of Raigad district in Konkan, near west coast of Maharashtra. Site is well connected by rail and road. Nearest railway station is Roha 4 km NW of site and Kolad-Roha road is 300 m to North from site which meets National Highway-66 (Panvel- Edappalli). Site is at a distance of 100 km from Mumbai. The plant facility is to be located in well-developed notified industrial estate and there is no human habitation in immediate vicinity of the plant.

Land form, Land use and land ownership

Land Form: Land is on plain contour; it is flat terrain.

Land Ownership: Land ownership is with project proponent (Deepak Nitrite Limited). Refer Annexure II.

Topography (along with map)

The Raigad district is divided into three parts on the basis of its topography.

The rock of the district is trap. In the plains it is found in tabular masses a few feet below the soil and sometimes standing out from the surface. In the hills it is tabular and

is also found in irregular masses and shapeless boulders varying from a few inches to several feet in diameter. In many places the surface of the trap has a rusty hue showing the presence of iron. River on North of the plant site is the main line of drainage which on going further meets Sea near village Korlai. This river flows east to west and helps in replenishment of ground water table.

Existing land use pattern

The land (Plot no 8, 32 to 34) are vacant at present and is for industrial use. Deepak Nitrite Limited will start activity on the said plot only after obtaining Environment clearance & Consent to establish from competent authorities. Hence, there was no activity carried out on this plot till now & existing EC/ CTE is not applicable.

Existing infrastructure

The Plot is located in well-developed notified MIDC area. Existing infrastructure is well developed.

Soil classification

There are four chief varieties of soil in Raigad district: ailuvial and alluvia, powdered laterite and trap, clay mould resting on trap, and soil containing marine deposits with, much sand and other matter in concretion.


32

The soil in the Roha tahsil is sandy loam and clay-slit. Sandy loam is ideal for plants that need more soil drainage than usual. Chronic incurable "overwater" will appreciate the drainage benefits sandy loam soil provides, since good drainage in soil decreases the chance of plant disease. The large soil particles of sand in sandy loam soil increase the soil's capacity to let water flow through, making it easier for fresh water to move through the planting media.

Climate data from secondary sources

Overall climate of this region is equable with high rainfall in monsoon season and very few days of extreme temperatures. The mean annual temperature ranges from 300C to 330C. The maximum temperature of the hottest month in this area varies from 350C –

400C in April-May while minimum temperature of coldest month varies from 15oC to 20oC. Extremes of temperatures, like 46-48oC in summer and 10-120C in winter, may be experienced for a day or two in respective season. The area has humid climate. Relative humidity varies from 25% to 85%. Driest days being in summer and wettest ones experienced in July. The rainy season is mostly confined to southwest monsoon & is

responsible for fresh water supply.

Social infrastructure available

Nearest town is Roha which is about 4 km from site. Social infrastructures such as schools, Hospitals, market place and other amenities are available. Transport facilities by rail and road are available.


33

5 PLANNING BRIEF

Planning Concept

• Plot is at well-established in Roha MIDC area.

• Purified Water supply from MIDC.

• Well-developed roads and connectivity.

• Infrastructure facilities available at established MIDC site.

• Integration with the existing manufacturing facility.

Population Projection

An official Census 2011 detail of Raigad, a district of Maharashtra has been released by Directorate of Census Operations in Maharashtra. In 2011, Raigad had population of 1,07,562 of which male and female were 55,553 and 52,009 respectively. The proportion of urban & rural population of study area stood at 32.34 (34786) and 67.66 (72776) percent respectively.

There was change of 3.20% in the population compared to population as per 2001. In the previous census of India 2001, study area recorded increase of 18.78 percent to its population compared to 1991.

Land use planning

The existing land use is industrial as it is within MIDC area. Refer Annexure II for details

Assessment of Infrastructure Demand (Physical and social)

There will be no major demand of physical and social infrastructure.

Amenities / Facilities

No major amenities / facilities demand is envisaged as the proposed site is in well-developed MIDC area.


34

6 P RO PO SED IN F RASTRUCT URE

Industrial Area (Processing area)

Deepak Nitrite Ltd. Plot No. 1-8, 26-34, MIDC Roha, Dist. Raigad-402 116, proposes to expand manufacture of synthetic organic chemicals and establish Pharma Product & Specialty chemicals, Agrochemical Products based on demand and market projection.

Social Infrastructure

The project shall have a positive impact on the employment pattern of the region. Economic status of the local population will improve due to increased ancillary/ business opportunities, thereby making positive impact. Educational, medical & housing facilities will improve due to the proposed project.

Connectivity

This proposed project facility is to be located at MIDC Roha Industrial area, in Raigad district, Maharashtra. The Site is 4 km from Roha town. The land and infrastructure is made available by MIDC and the raw material is easily available through the easy transport via road connectivity.

Drinking water management

The source of water is already availability from existing water works of MIDC and the same is adequate and satisfactory. The water supply will be through the good offices of MIDC.

Sewage System

The domestic effluent will be treated in proposed sewage treatment plant.

Effluent Plant Treatment System

The Effluent Stream obtained from the process is subjected to Pre-treatment followed by RO & MEE. The Scheme is as mentioned below. Pre-treatment prior to RO & MEE ➢ The effluent is collected in Equalization Tank, where pH is adjusted to 7- 7.5.

➢ The equalized effluent is taken in to Aeration Tank where the same is subjected to aeration.

➢ The Effluent from Aeration Tank is taken in to clarifier from which the de-canted is taken to collection tank.

➢ Effluent from collection tank is subjected to filtration through multi-media filter followed

by R.O.


35

2. RO plant & MEE

➢ The RO rejected Effluent is taken in to receiving tank for MEE. Permeate from RO will be

recycled.

➢ The effluent from the receiving tank is subjected to triple effect evaporation.

➢ The distillate from MEE is recycled in utility & gardening purpose & Sludge disposed to

CHWTSDF.

Industrial waste management

Refer 3.9 above

Solid waste management

Refer 3.9 above

Power requirement and supply / source

Additional power requirement is 2500 KVA which shall be sourced from MSEDCL.


36

7 RE HAB IL ITAT IO N & RE S E TT LE ME NT P LA N

Not Applicable as the project is to be located in notified MIDC area.


37

8 P RO JECT S CHE D ULE A ND COST E ST IM AT ES

Likely date of start of construction and likely date of completion

The proposed establishment project has been planned for the manufacturing of Pesticide specific intermediates & synthetic organic chemicals (pharmaceutical bulk drugs & intermediates). The proposed development will take about 1.5 year for the operative phase of new production. The construction activities and installation of plant & machineries for expansion will start after obtaining necessary approval from SEIAA and MPCB.

Estimated project cost

Estimated project cost and its break up is as follows,

Sr. No Description Estimated investment,

Rs. Crores

1 Land and site development 3

2 Buildings 1

3 Plant and Machineries 136

4 Environmental protection measures 15

5 Others 2

Total 156


38

9 A NALYS IS OF T HE P RO P O SAL (F INAL RECO MM ENDAT ION )

The unit will provide adequate measures for the prevention and control of pollution. With the execution and operation of such control measures along with proper Environmental Management System, there will not be any major potential for negative impact on the environment due to proposed project. However, there will be positive impact on the socio-economic environment since proposed project will generate some permanent and secondary employment. The unit will also establish cordial relation with the nearby area and villagers and will carry out social welfare activities according to their needs as part of activities carried out by Industrial Association. The proposed project will also boost up ancillary industrial and commercial activity. Thus, it will improve the economic condition of the area.


39

ANNEXURE I Google image of study area Site with 10 km radius area

Site with 1 km radius area


40

ANNEXURE II Plot transfer order

Plot No. 8 attached, Plot No. 32-34 Lease document under approval at MIDC.


41


42


43

Layout plant of the proposed establishment with area statement

AREA STATEMENT

1-8 & 26-34 Total Plot Area: 34816 Sq.m

Sr. No. Details of Land Existing land

Area (in sq.m)

Proposed land Area (in

Sq.m) Total

1 BUILTUP AREA 15432 4511 19943

2 GREEN BELT AREA (Inside) 2968 708 3676

3 PARKING AREA 2662 675 3337

4 ROAD & OPEN SPACE AREA 5562 2298 7860

Total 26624 8192 34816

Plot Survey No. 17,21,206 (Outside Premises inside MIDC)

No Details of Land Proposed

land Area (in Sq.m)

1 GREEN BELT AREA (Outside) 8605

Total Green Belt= 3676 sq.m (inside premises) + 8605 sq.m (outside premises)=12281 sq.m


44

Plot Survey No. 17,21,206 (Outside Premises inside MIDC- Green belt)

Existing land use status

Deepak Nitrite Limited will start activity on the said plot only after obtaining Environment clearance & Consent to establish from competent authorities. Hence, existing EC/ CTE is not applicable.


45

ANNEXURE III

Proposed Water Balance

WATER BALANCE

Domestic Gardening

Total water requirement: 1647 cmd(F –1164, R – 483)

Industrial Processing

All figures in CMDF – FRESH waterR – RECYCLE water

Sewage Treatment

Plant

Boiler and cooling

Evaporation and Losses

Processing and Losses

Consumption and and Losses

40

355

35

772 800 0

Effluent Treatment Plant-

400 CMD

710

32

247

Low volatiles form stripper(Recycle/Reuse/Disposal)

23 MEE Salts to CHWTSDF

12

Treated waste water

to CETP

62

688

Stripper

MEE-72 CMD

95368

7260

RO-400 CMD

MEE-80 CMD

Blow down

Recycle

MEE Salts to CHWTSDF

12

153

247

Recycle to utility

6880

Recycle to utility

320


46

Capacity

17.38 M3

ETP- 400 CMD

108.8 M3

x 2 no.

44 M3

3 x 3 x 2.5 x 2 no.

3.7 M3

1.5 x 1.5 x 1.6

96.2 M3

7.0 D x 2.5

800 M3

10 x 22 x 3.7

96.2 M3

7.0 D x 2.5

Capacity - 64 M3

216 M3

12 x 6 x 3

49.1 M3

5.6 D x 2

20 M3/ Hr

20 M3/ Hr

247 CMD Outlet to MIDC CETP

50 Kl

Low COD Effluent

from process

Permeate recycled to Utility

MEE (80 KLD)

Sludge disposed to CHWTSDF Condensate recycled to Utility

Effluent Treatment Plant Flow diagram

Waste water ( Effluent)

4.8 x 4.2 x 2.7

Oil & Grease Trap

Collection & Equilization Tank

Neutralization Tank

Flash Mixer (Flocculation

Tank)

Aeration Tank

Extended Bio reactor

RO- 400 CMD

Sludge to Sludge

Drying Bed

Acid/Caustic

Alum/

Blower(1000 M3)

Blower(250 M3 x 2 no)

Primary Thickner

Secondary Clarifier

MGF

ACF

Final Clarifier

First Stage

Second Stage

Third Stage

Treated Effluent Collection Tank


47

ANNEXURE IV

Product details Process Reactions and Process description

1) Para Cumidine

Production of Para Cumidine 300 MT/Month

Stage-1Nitration of Cumene to Para Nitro Cumene and Ortho Nitro Cumene

Stage -2Seperation/Distillation of Cumene to Para Nitro Cumene and Ortho Nitro Cumene

Stage-3Reduction of Para Nitro Cumene.

CH

CH3

NO2

H3C

+ HNO3

H2SO4

CH

CH3H3C

+ H2O

( 120 )

Cumene

( 63 )

Nitrating Mixture ( 165 )Nitro-Cumene

( 18 )

Water

CH

CH3

NH2

H3C

+ 3H2

Catalyst

CH

CH3H3C

+ 2H2O

( 165 )PNC

( 3 x 2 )Hydrogen

( 135 )Para-Cumidine ( 2 x 18 )

Water

NO2


48

Process Discription :- Nitration of Cumene to Para Nitro Cumene and Ortho Nitro Cumene

Hydrogenation Process :-

Effluent Details:

Sr.No. MT/MT KLD

1 14.41 154

2 Liquid Effluent 9.75 104

3 0.0035 0.0371

4 2.2165 23.7

RM :

Sr. no. Quantity(MT/MT)

1 1.73

2 1.09

3 1.34

4 0.02

5 0.00084

6 0.01

1. Nitration is carried out using a mixed acid. This mixed acid, which a mixture of nitric and sulphuric acid is to be prepared separately.

2. Add sulfuric Acid in the Reactor. Start addition of nitric acid so that the temperature remains within specified limits.

3. Charge the compound to be Nitrated in the Reactor. Then add mixed acid gradually under controlled conditions in the compound to be

nitrated. The temperature of the reaction is maintained within specified limits. A sample is drawn at the end of the addition of a defined

quantity to verify that the reaction is complete.

4. From the nitrated mixture, organic layer is separated and washed with water till free of acid. The final nitromass is to be transferred for

Distillation.

Description

Water Consumption

1 Hydrogenation is carried out in presence of a catalyst. The compound to be hydrogenated is charged into a Hydrogenation reactor.

2 Hydrogen addition is started at specified temperature. The reaction is conducted under controlled conditions. The temperature and pressure

are maintained within specified limits.

3 After complete reaction, catalyst filtered. And transferred it for Distillation.

Hydrogen

Distillation residue

98% H2SO4

RM

72% HNO3

Cumene

5% Soda soln

Catalyst

Spent layer


49

DEEPAK NITRITE LIMITED

APL DIVISION

STAGEWISE MASS BALANCE

PRODUCT : NITROCUMENE

INPUT QTY UNIT

H2SO4(98%) 2500 Kg

HNO3 (72%) 1580 Kg

TOTAL 4080 Kg

10% soda Solution 213.33 Kg

MIXED

ACID

8.0 NOX to Scrubber

INPUT QTY UNIT 221.33 Kg

CUMENE 1935 Kg

NCU

QTY UNIT + SPENT ACID

6007 Kg

OUTPUT QTY, Kg

(BI PRODUCT) SPENT ACID 3200.00 SPENT ACID

Organics 0.28 SEPARATION

TOTAL 3200.28

QTY,kg

NCU 2807

QTY,kg

NCU 5614

WATER FOR WASHING Total Effluent to ETP

INPUT QTY, Kg OUTPUT QTY, Kg

1 St WATER 14000 1 St WATER Wash 14070

2 nd WATER 15000 2 Nd WATER Wash 15100

%5 SODA SOLN 500 Soda wash 600

3 rd WATER 15000

TOTAL 44500 3 rd WATER Wash 15094

TOTAL 44864

UNIT

Kg 3087

MIXED ACID

PREPARATION

WASHING

NCU + SPENT

CUMENE

NITRATION

Scrubber Water To Effluent

OUTPUT

5250

QTY

NITROCUMENE

UNWASHED

NCU

NITROCUMENE

Scrubber


50


APL DIVISION


PRODUCT : PARA-NITROCUMENE (PNC)

TOP OUTPUT QTY UNIT

ONC 309 Kg

(BIPRODUCT)

INPUT QTY UNIT

NCU 750 Kg

COMP. %

ONC 24.90

MNC 4.77

PNC 69.62

IMP 0.71

TOTAL 100

OUTPUT QTY UNIT

PNC 441 Kg

PRODUCT

Distill,n

Column


51

2) 3 ABTF


APL DIVISION


PRODUCT : PARA CUMIDINE

INPUT QTY UNIT

PNC 441 Kg

Catalyst 1.2 Kg

Hydrogen 17 Kg

TOTAL 460 Kg

460 Kg

OUTPUT QTY UNIT

WATER 37 Kg

CATALYST 1.2 Kg

PC (To recy.) 7 kg

TOTAL 45.3 kg

OUTPUT QTY UNIT

INPUT QTY UNIT WATER CUT 6.04 Kg

RECY.CRUDE 14 Kg PC (To recy.) 6.92 Kg

TOTAL 12.95 Kg

OUTPUT QTY UNIT

DIST.RESIDUE 2.6 Kg

(Disposal to MWML)

OUTPUT QTY UNIT

SETTLING

HYDROGENATION

DISTILLATION

PARA-CUMIDINE

Para

Cumidine

(PC)

412 Kg

CRUDE Para cumidine


52


APL DIVISION

Production of 3ABTF 400 MT/Month

Stage: 1Preparation of 3-Nitrobenzotrifluoride( 3-Nitro BTF)

Stage: 2Preparation of 3-Aminobenzotrifluoride (3-Amino BTF)

Process Description:

1 The 3ABTF manufacturing is a four stage process Nitration, Nitromass Sepration, Hydrogenation & Hydromass Sepration.

2 The BTF nitration is done to convert NBTF (Nitromass)

3 The Nitromass sepration in to 2NBTF & 3NBTF.

4 The 3NBTF Hydrogenation to form ABTF Hydromass.

5 The 3ABTF hydromass sepration to 3ABTF & 4ABTF. RM :

Sr. no. Quantity(MT/MT)

Effluent Details: 1 2.52

Sr.No. MT/MT KLD 2 1.21

1 2.87 41 3 0.76

2 Liquid Effluent 2.72 27 5 0.01

3 0.07 0.93 6 0.03

4 3.34 47.73 7 0.03

5 0.01 0.08

6 0.17 2.46

Water Consumption


Description

Spent acid layer

RM

98% H2SO4

BTF

Soda ash

70% Nitric acid

Catalyst

Hydrogen

Discarded catalyst

2 NBTF

CF3 CF

3

NO2

BTF 3-NBTF

NitrationHNO3

146.11 191.11

+H2SO4

H2O+

CF3

NO2

CF3

NH2

191.11

5% Pd/C

Methanol

+ 3 H2 + 2 H2O

2.02 18.02

3-NBTF

191.11

3-ABTF

161.13


53


APL DIVISION

BLOCK DIAGRAM

(Equivalent to Single batch of BTF)

A) Prepratation of Nitrobenzotrifluoride

98% Sulfuric Acid 3132

BTF 1500

70% Nitric Acid 942

Water 515 Reaction Mass 6089

Spent Acid Layer 4151 To Disposal

Reaction Mass 1938

Plain Water Wash-I 1000 Aq. Layer-I 1006 To Disposal

Reaction Mass 1932

5% Soda Ash Wash 1050 Aq. Layer-II 1058 To Disposal

Reaction Mass 1924

Plain Water Wash-II 1000 Aq. Layer-III 1000

Nitro Mass (Organic) 1918

Water Fraction 12

3 NBTF 1550

Mixed Cut (2 NBTF + 3 NBTF) 97

2NBTF 214 By product

Residue 45

B) Prepratation of 3 Amino benzotrifluoride

Pd on C Catalyst 16

Hydrogen 41

Reaction Mass 1607

Rec. Catalyst 7 To Recycle

Reaction Mass 1600

Water Generated in Reaction 321 To Disposal

Reaction Mass 1279

3 ABTF 1243 To TFMAP Process

Residue 36

1243 Kg

Hydrogenation

Catalyst Filtration

Layer Sepration

(Water Generated in Reaction)

3 ABTF Flash Distillation

Eq. 3 ABTF Output based on BTF / Batch

Nitration

(Semi Batch Process)

Layer Sepration

(Spent Acid Separation)

Washing & Layer Sepration

(Plain Water Wash-I)

Layer Sepration

(Spent Acid Separation)

Washing & Layer Sepration

(Plain Water Wash-I)

Distillation

(Nitro Separation Column)


54

3) Ortho Anicidine


APL DIVISION

Production of Ortho Anicidine 50 MT

Reaction Schem

Stage I

Nitration of Anisole to Ortho Nitro Aniline

Stage II

Reduction of Ortho Nitro Anisole to Orhto Anicidine

Process Discription :-Nitration of Anisole to Ortho Nitro Aniline

1 Mix Acid is prepared by Nitric and Sulfuric Acid.

2 Mix Acid is added to Anisole gradually.

3 Then Spent Acid is seperated from ONA.

4 After washing ONA is send for reduction.

Reduction of Ortho Nitro Anisole to Orhto Anicidine

1 Ortho Nitro Anisole is reduced to Ortho Anicidine by hydrogene.

2 Then the crude OA is Distilled to have pure Ortho Anicidine.

Effluent Details:

Sr.No. MT/MT KLD

1 3.41 6


3 0.001 0.002

4 0.001 0.002

5 0.020 0.036

Description

Water Consumption


Discarded catalyst

Spent Acid

Anisole

+ HNO3H2SO4

OMe

+ H2O

108

OMe

NO2

Ortho Nitro Anisole

153

Water

18

Nitric

63

OMe

NO2

Ortho Nitro

153

+ 3 H2

OMe

NH2

Ortho Anicidine

123

+ 2 H2O

Hydrogene

3x2

Water

2x18


55


APL DIVISION


PRODUCT : ORTHO NITRO ANISOLE

INPUT QTY UNIT

H2SO4(98%) 97 Kg

HNO3 (72%) 97 Kg

TOTAL 195 Kg

10% soda Solution 8 Kg

MIXED

ACID

0.3 Nox

to ETP 8.3 Kg

INPUT QTY UNIT

ANISOLE 139 Kg

QTY UNIT

333 Kg

OUTPUT QTY, Kg

EXCESS ACID 143 SPENT ACID

Organics 0 SEPARATION

TOTAL 144

Reused

QTY,kg

ONA 187

Spent 3

TOTAL 189.6

WATER FOR WASHING Total Effluent to ETP

INPUT QTY, L OUTPUT QTY, Kg

WATER 469 WATER Wash 486

SODA SOLN 14 10% Soln. TOTAL 486

TOTAL 483

UNIT

Kg

sr. No Name of Raw Material Quantity (MT/MT product)

1 H2SO4 (98%) 0.68

2 HNO3 (72%) 0.68

3 Anisole 0.97

4 10% soda solution 0.01

5 Hydrogen 0.05

6 Catalyst 0.00

7 Soda ash 0.11

MIXED ACID

PREPARATION

ONA + SPENT

ANISOLE

UNWASHED

ONA

WASHING

NITRATION

ORTHO NITRO ANISOLE

OUTPUT QTY

ONA 187

Scrubber


56

4) TMHQ


APL DIVISION


PRODUCT : ORTHO ANISIDINE

ONA 187

Organic Layer 195

Raney Nickel 0.2

Hydrogen 7.6

195 195

Organic Layer 195 Crude OA Water Cut 150

Catalyst 0.2 Recycled

Water 44

195 195

Organic Layer 150 OA 143

Azeatrop Cut 6 Recycled

Residue 0.2

Loss 0.8

150 150

Hydrogenation

Separation

Methanol Recovery

Hydrogenation

Separation

Distillation


57


APL DIVISION

Production of TMHQ 50 MT/Month

Reaction:

Stage-I Preparation of TMHQ


58

5) 2,4 Nitro Xylene


STEP 1 – Oxidation of TMP to TMQ

STEP 2 – Hydrogenation of TMQ to TMHQ

STEP 3 – Solvent recovery

STEP 4 – Purification

STEP 2 – Drying

Effluent Details:

Sr.No. MT/MT KLD

1 8.86 15.82

2 Liquid Effluent 9.19 16.42

3 0.00 0.00

4 0.16743 0.299

5 0.02484 0.0443

Discarded catalyst

Charcoal sludge


In this step, TBQ is prepared by oxidation of TMP with Hydrogen peroxide with catalyst in presence of Methanol . The resultant reaction

mass is filtered for recovery of catalyst which is recycle back.

In this step TBQ prepared in the earlier step is hydrohenated using catalyst . The hydromass is then separated from catalyst which is

recycled back into system .The filtered mass is then sent for solvent recovery

Description

Water Consumption

The wet cake obtained from previous step is then dryed in sutable dryer to get finished product.

The reaction mass free from methanol is purified , using Toluene , precipitated ,filtered t get crude TMHQ. The crude is treated

with charcoal & then again purified with solvent & reprecipitated . The final mass is again filtered through centrifuge to get wet

cake & the solvent is recovered & recycled back

Methanol is recovered in this step & methanol free reaction mass is sent for purification


59


APL DIVISION

Production of 2,4-Nitro-Xylene & 2,6-Nitro-Xylene 500 MT/Month

Stage 1Nitration of Meta-Xylene to 2,4-Nitro Xylene & 2,6-Nitro Xylene

Rxn Schem

Stage -2Seperation/Distillation of Nitro-Xylene to 2,6-Nitro Xylene and 2,4-Nitro Xylene

Effluent Details:

Sr.No. MT/MT KLD

1 8.12 145

2 2.99 53

3 0.09 1.58

4 0.72 12.90

Nitration of Meta-Xylene to 2,4-Nitro Xylene & 2,6 Nitro xylene

1. Nitration is carried out using spent acid, sulfuric acid & Nitric acid. Along with these compounds, the compound to be nitrated is continuously charged in to the reactors.

2. Reaction is conducted under controled conditions as mentioned.

3. After completion of Nitration, Spent acid is seperated.

Process Discription :-

Liquid Effluent

Description

Water Consumption


4. After Serperation Nitro mass is washed in washer to remove acidity.

Spent Acid

5. The washed Nitro mass is then send for further Distillation.

CH3 NO2

+ HNO3

H2SO4+ H2O

( 106 )M-Xylene

( 63 )Nitrating Mixture

( 151 )Nitro-Xylene

( 18 )Water

CH3

CH3

CH3

2NO + O2 NaNO3 + NaNO2 + H2O+ 2NaOH


60


APL DIVISION


PRODUCT : NITROXYLENE

Nox TO SCRUBBER scrubber 21.14 Kg

1 kg Nox To ETP

INPUT QTY UNIT

M-XYLENE 242 Kg

HNO3 (98%) 147 Kg

H2SO4 (98%) 126 Kg SPENT

SPENT ACID 575 Kg ACID OUTPUT QTY, Kg % COMP.

TOTAL 1090 Kg SPENT ACID 746 99.99 S.A.GENERATION -

Organics 0.0383 0.01 171.201 Kg

TOTAL 746 100

UNWASHED QTY,kg % COMP

NITROXYLENE NXL 344 99.45

344 Kg/Hr Spent 2 0.55

TOTAL 346 100

WATER FOR WASHING WATER WASHES

INPUT QTY, Lt OUTPUT QTY, Kg/Hr % COMP

WATER 613 3 Washes WATER Wash 708 100.00

SODA Soln 96 10% Soln. 0.00

TOTAL 709

TOTAL 708 100

Actual Effluent Load = 555 kg

INPUT QTY UNIT

NXL+M-XYLENE 346 kg

NXL WITH

M-XYLENE

TOP OUTPUT QTY UNIT

M-XYLENE 24 kg

QTY UNIT

322 kg

20.38

10% NaNO2 Soln kg

OUTPUT

NITROXYLENE

SEPARATION

PRODUCT

WASHING

NXL WITH M-XYLENE

M-XYLENE &

MOISTURE

CONTINEOUS

NITRATION

CONTINUOUS


61

6) 3,4 Nitro Xylene


APL DIVISION


PRODUCT : 2,4 NITROXYLENE & 2,6 NITROXYLENE

OUTPUT QTY UNIT

2,4 NXL 237 Kg

OUTPUT QTY UNIT

2,6 NXL 64 Kg

INPUT QTY UNIT A B

NXL 322 Kg

OUTPUT QTY UNIT

BOTTOM Residue 21.00 Kg

OUTPUT QTY UNIT

2,4 NXL mix 258 Kg

PRODUCT

PRODUCT

BOTTOM


62

Deepak Nitrite Ltd.

APL-DIVISION

Production of 2,3-Nitro Xylene and 3,4-Nitro Xylene 1330 MT/Month

Stage 1

Rxn Schem

Stage -2

6. In the Distillation 2,3-Nitro Xylene and 3,4-Nitro Xylene is Seperated as pure Product.

Effluent Details:

Sr.No. MT/MT KLD

1 4.35 207


3 0.047 2.23

4 0.714 33.92


2. Reaction is conducted under controled conditions as mentioned.

3. After completion of Nitration, Spent acid is seperated.

Nitration of Ortho-Xylene to 2,3-Nitro Xylene and 3,4-Nitro Xylene1. Nitration is carried out using spent acid, sulfuric acid & Nitric acid. Along with these compounds, the compound to be nitrated

is continuously charged in to the reactors.

Spent Acid

Nitration of Ortho-Xylene to 2,3-Nitro Xylene and 3,4-Nitro Xylene

4. After Serperation Nitro mass is washed in washer to remove acidity.

5. The washed Nitro mass is then send for further Distillation.

Seperation/Distillation of Nitro-Xylene to 2,3-Nitro Xylene and 3,4-Nitro Xylene

Description

Water Consumption

( 63 )Nitric Acid

CH3

NO2

+ HNO3

H2SO4+ H2O

( 106 ) O-Xylene

( 151 )Nitro-Xylene

( 18 )Water

CH3

CH3CH3


63

7) 2,3 Xylenol

DEEPAK NITRITE LIMITED 700 1350

APL DIVISION 850 1639.286

1.928571


PRODUCT : NITROXYLENE scrubber 27.60 Kg

To ETP

Nox TO SCRUBBER

1 Kg/Hr

INPUT QTY UNIT

O-XYLENE 850.0 Kg/Hr

HNO3 (98%) 508 Kg/Hr

H2SO4 (98%) 522 Kg/Hr SPENT

SPENT ACID 1639 Kg/Hr ACID OUTPUT QTY, Kg/Hr % COMP.

TOTAL 3519 Kg/Hr SPENT ACID Recycle 1639 69.33 S.A.GENERATION -

Organics 0.0 0.00 725 Kg/Hr

TOTAL 2364 69

UNWASHED

NITROXYLENE

1154 Kg/Hr

WATER FOR WASHING WATER WASHES

INPUT QTY, L/Hr OUTPUT QTY, Kg/Hr

1 ST WATER 1500 1st WATER Wash 1500

Ammo Soln,Kg/Hr 601 10% Soln. Salts 601

2 nd WATER 2125

2 nd WATER Wash 2125

1154

TOP OUTPUT QTY UNIT

O-XYLENE 93 Kg/Hr

QTY UNIT

1061 Kg/Hr

O-XYLENE &

MOISTURE

SEPARATION

PRODUCT

NITRATION

NITROXYLENE

CONTINUOUS

WASHING

OUTPUT

CONTINEOUS

10% NaNO2 Soln kg

26.60

Reaction:

Stage-I Preparation of 2,3 Xylenol

NH2

CH3

+ NaNO2 1/2 H2SO4+Water

MIBK

OH

CH3

+ N2 + 1/2 Na2SO4 + H2O

2,3 Xylidine 2,3 Xylenol

CH3 CH3


64


STEP 1 – Diazotization & Hydrolysis Reaction

STEP 2 – Distillation

In this step, we simultaneously take the required qty of water, 98% sulphuric acid, 2,3 Xylidine & MIBK into the reactor. Then we added

the NaNO2 Solution slowly into same mass by maintaining the reaction temperature. After completion of reaction, aqueous layer

seperated out & organic mass then washed with 5 % soda soln. Then we transfer oraganic mass for further distillation Process.

In this step we recovered MIBK, which is recycled back to Next dizotization Process & Pure 2,3 Xylenol as a finished product.BLOCK DIAGRAM

Process Water 3777.11

98% H2SO4 755.43

2,3 Xylidine 847.00 N2 196.00

MIBK 1533.76

31.8% SNI Solution 1577.25

Hydrolysis Mass 8294.55

Org. Layer 2418.20

Aq. Layer 5876.35

5% Soda Sol. Wash 347.13

Org. Layer 2411.26

Aq. Layer 354.07

MIBK Rec. (Atm) 1180.99

MIBK Rec. (Vac) 283.74

Mixed Cut 148.11

2,3 Xylenol 711.48

Residue 86.93

Diazotization & Hydrolysis

(One Pot Process)

Hydrolysis Mass Cooling and Layer Separation

Soda Washing to Organic Layer

Solvent Recovery and Fractional Distillation

Section


65

8) 2,4 Xylenol

2,4-Xylenol reaction scheme

Production of 2,4-Xylenol 120 MT/Month

Stage: 1 Preparation of 2,4-Xylenol

1

CH3

NH2

CH3

OH

CH3

CH3

N2+ NaNO2

1/2 H2SO4

Toluene++ +

Water

+ H2O1/2 Na2SO4

2,4-Xylenol -Brief process

Process description

Stage: 1 Preparation of 2,4-Xylenol

1 Charge water and 2,4-Xylidine in RBF

2 Add slowly sulfuric acid

3 Charge toluene and heat it

4 Prepare solution of sodium nitrite in water

5 Add slowly sodium nitrite solution into above reaction mass within 5hrs maintaining temperature

6 The reaction mass is further maintain. Check for unreacted 2,4-Xylidine.

7 Cool the reaction mass to RT and allow settling

8 Separate out bottom aqueous layer and wash it with toluene

9 Sent aqueous layer (pH=acidic) to ETP for treatment

10 Wash organic layer with soda solution and take organic layer in RBF and add triethanolamine

11 Distilled out toluene

12 Cool the bottom mass and distilled out remaining toluene under vacuum

13 Distill out product under vacuum (Used 2 feet SS packed column for distillation)

14 1st fraction containing toluene to be recycled in next batch

15 Main fraction as finish good

16 Redistillation Main cut for second time fractional distillation for moisture content within limit

17 Bottom mass of second distillation recycle in next batch


66

9) 2,5 Xylenol

H2SO4 1800

Water 4800

2,4-Xylidine 1464

Toluene 5190

Xylidine salt mass 13254

NaNO2 900

Water 3600 Aqueous layer 11435 Effluent

Toluene wash 600

Organic layer 6919

Soda wash 600

Soda wash 605 Recycle

Organic layer 6914

Rec. Toluene 5521 recovery in house and reuse

TEA 12 Residue 169 waste

Vapour loss 12

2,4 Xylenol 1224

MATERIALS BALANCE- 2,4-Xylenol

REACTION-1

REACTION - 2

DISTILLATION

REACTION - 2

REACTION - 2Washing


67

Reaction:

Stage-I Preparation of 2,5 Xylenol

NH2

CH3

CH3

OH

CH3

CH3

1) NaNO2 + H2SO4

2 ) MIBK

3) 55- 60 o c


STEP 1 – Diazotization & Hydrolysis Reaction

STEP 2 – Distillation

In this step, we simultaneously take the required qty of water, 98% sulphuric acid, 2,5 Xylidine & MIBK into the reactor. Then we added

the NaNO2 Solution slowly into same mass by maintaining the reaction temperature. After completion of reaction, aqueous layer

seperated out Then we transfer oraganic mass for further distillation Process.

In this step we recovered MIBK, which is recycled back to Next dizotization Process & Pure 2,5 Xylenol as a finished product.


68

10) Phenyl Hydrazine

BLOCK DIAGRAM

Process Water 1352.00

98% H2SO4 270.00

2,5 Xylidine 303.00

MIBK 1533.76

33% SNI Solution 575.00

Hydrolysis Mass 4033.76

Aq. Layer 2833.76 Extraction

-889.76

Org. Layer 1200.00 230.0634105 -659.69

MIBK Rec. (Atm) 552.00

MIBK Rec. (Vac) 92.00

1St Cut 18.50

Mixed Cut 260.00

Residue 19.50

2,5 Xylenol 258.00

Diazotization & Hydrolysis

(One Pot Process)

Hydrolysis Mass Cooling and Layer Separation

Solvent Recovery and Fractional Distillation

Section


69

11) MMDPA

Product :- Phenyl Hydrazine 100

Quantity Item Quantity

kg UOM kg

200

600

200

152

222

5

20 Diazo mass 1399

1399

947

1340

340 Rxn mass 4026

408

1560

4026

1200

Rxn mass 4934

2188 Recycle

220

71

4934

PHHCl(w/w) 70.13% Main filtrate 4523

LOD 23.10% 2

PHHCl wet cake 409

2.045

Mix Organic 808

408

820

180

600

1185

14

525

808

212

212

13 225

Item

MATERIAL BALANCE

INPUT OUTPUT

UOM

Aniline Diazotization

30% Hydrochloric acid

Water for 30% HCl

Sodium Nitrite

Water for SNI

Sulfamic acid

Water

Diazo mass Reduction

Sodium bisulfiteRxn temp 0-5°C

Water for NaHSO3

NaOH lye for PH

NaOH lye 48%

Water

Hydrolysis Scrubber

30% Hydrochloric acid

Scrubber solution

As SO2

Rxn massTemp 20-25°C

Loss

Filteration

Rxn mass

Loss

Neutralization

PHHCl wet cake

Water

NaOH lye

Toluene for extr.

Aqeous layer

Crude PHH Base

Toluene Distillation

Mix Organic

Rec. Toluene

MT/M

Crude PHH Base Water addition

Final PHH Basewater

Loss


70

MMDPA Production per Month 100 MT/Month

Reaction Schem

Methylation

Bromination

Condensation

Hydrolysis

OH ONa

CH3

OCH3

CH3

ONa

CH3 CH3

+ NaOH + H2O

( 108 )M-Cresol

( 40 )Caustic Lye

( 130.12 )Sodium salt of

M-Cresol

( 18 )Water

( 130.12 )Sodium salt of M-Cresol

+ (CH3)2SO4

( 126 )Dimethyl

Sulphate

( 122.16 )3 - Methyl Anisole

+ CH3NaSO4

( 134.08 )Sodium Methyl

Sulphate

OCH3

CH3

( 122.16 )3 - Methyl Anisole

+ HNO3 + NaBr

OCH3

CH3

Br

( 63) ( 108 ) ( 18)( 201.06 )4-Br 3 - Me

Anisole

+ H2O + 1/2NaNO2 + 1/2NaNO3

OCH3

CH3Br

NHCOCH3

( 135.16 )Acetanilide

+ + 1/2 K2CO3

(1/2 x138.20)

OCH3

CH3

NCOCH3

( 255.31 )Methoxy Methyl Aceto Diphenyl Amine

( N-Acetate )

+ KBr + 1/2 CO2 + 1/2 H2O

(119) (1/2x44) (1/218)( 201.06 )4-Br 3 - Me

Anisole

OCH3

CH3

NCOCH3

( 255.31 )Methoxy Methyl Aceto Diphenyl Amine( N-Acetate )

+ KOH

OCH3

CH3

NH

( 213.1 )4 -Methoxy 2 - Methyl Diphenyl Amine( MMDPA )

+ CH3COOK

( 98.14 )Potassium Acetate

( 56.1 )

(34.5) (42.5)


71

Detailed Process :-

12 Separated out the Solid MMDPA & Mother liquor from centrifuge.

13 Wet MMDPA dried out in RCVD.

7. Charge measured quantity of 4-Br-3-Me Anisole into the reactor. Subsequently charge measured quantity of Soda Ash, acetanilide, cuprous chloride & iodine. Heat

gradually to the temperatures and maintain subsequently.

8. Charge measured quantity of potassium hydroxide, Caustic & water into condesation mass. Hydrolysed the mass till specified temperature approaches.

9. Filter the mass & Separate the aqueous and organic layer.

10. Charge Crude MMDPA and Distill out.

11. Charge methanol followed by a measured quantity of semi pure MMDPA into the crystalliser.

6. Charge HBr of specified strength then charge measured quantity of 3-Me-Anisole in to the reactor gradually. Start addition of Nitric Acid. Neutralize the mass and

then allow the mass to settle. Drain out the aqueous layer and collect the organic layer.

1. MMDPA is produced by carrying out reaction stages called Methylation, Bromination, Condensation & Hydrolysis followed by purification stages.2. Charge a measured quantity of water in to the methylation reactor. Then charge caustic lye with specified strength from metering tank. Charge M-Cresol into the

reactor.

3. Add DMS gradually.

4. Charge water in to reaction mass and then charge sulphuric acid Separate aq. and organic Layer.

5. Separate organic from the previous aq. layer , Collect the both organic layer.


72

12) 3NAP

BLOCK DIAGRAM

Stage 1:-Methylation

M-cresol 1760.00

Water 1333 Recycled

NaOH 47% 1801 1st Cut 1000 Product recovery at Temp. 100 to 102 oc

DMS 1370

Rec. M- Cresol 200.0 Recover Org. 1960

Aqueous 3504

1st Cut 1000.00

Water 2300.0 Aq. Layer 6714

98% H2SO4 110 Rec. M-cresol 200 Recycle to Next Batch

Caustic 5 % 330 Aq. Layer 335.00 Recycle to Next Batch

3-Methyl anisol 1955 Equiv. MMDPA 2303

Stage 2:- Bromination

NaBr(36%) 2452

HBr 250 1st Aq. Layer 3172

3-Me-Anisol 1162 Nox 172 Scrubbed

HNO3(72%) 1370 Organic 1890

Organic 1890.0 1st Aq. Layer 264.01

Water 225.0

C. Lye 30.0 Organic Layer 1881.00 Equiv. MMDPA 1369

Stage 3:- Condensation :

4 Bromo 3Me Anisole 2130 Water 85

Soda Ash 600 CO2 207

Acetanilide 1300 30% NaBr Soln 3175

Cuprous Chloride 42 Emultion 100

Iodine 4

1st Lot Butanol 1120

Water 2200

Organic Mass 3829

Organic Mass 3829 Dist. Butanol 1058

KOH 550 Butanol loss 62

NaOH 100 Aq. Layer 3025 Recycle to Next Batch

Water 2000

Organic Mass 2334

Stage 4:- Distillation :

Bromo cut 338

Organic Mass 2334 Mix cut 100

Mix Cut 100 MMPDA cut 1804 Equiv. MMDPA 1550

Residue 192

Stage 5:- Crystallisation

MeOH 2742

MMPDA cut 1804 Methanol Ml 3096

MeOH washing 150

MMDPA 1600

Stage 6:- Drying

MMDPA 1600 Vapors 50

Dry MMDPA 1550 Equiv. MMDPA 1550

Stage 7:- MeOH Distillation

Mother Liqure 3096 Rec. MeOH 2845 Recycle to Next Batch

Methanol loss 126

2nd Crop 125 MMDPA Recovery

Methanol Recovery

Methylation

M-cresol recovry

3-Methyl anisol Washing

Bromination

Bromination

Condensation

Hydrolysis

Distillation

Crystallisation

Drying


73

Production 3-Nitro Acetophenone 60 MT/Month

Reaction: Preparation of 3-Nitro acetophenone (3 NAP)

O CH3

HNO3

H2SO

4

O CH3

NO2

+

Acetophenone

120.15

3-NAP

165.15

+ H2O

Nitric acid

6318


In this step, we simultaneously take the required qty of Acetophenone, 98% sulphuric acid into the reactor at certain

temperature. Then we added the Pre-cooled Mixed Acid ( H2SO4 + HNO3) slowly into same mass by maintaining the

reaction temperature. After completion of reaction, we quenched out the reaction mass by adding crushed ice. Then we

filtered out the NAP by using Centrifuge. Wet NAP then dried into the dryer under certain vacuum & we got finished NAP

as a product.


74

13) 3AAP

BLOCK DIAGRAM

Stage 1 - Preparation of 3 Nitro Acetophenone (3 NAP)

98% Sulfuric Acid 243.0

70% Nitric Acid 238.0

Mixed Acid 481

98% Sulfuric Acid 1450.0

Acetophenone 300.0

Nitrated mass 2231

Ice Water 1400.0

Drowning mass 3631

Excess Acid 3191 REUSE

Crude Wet Cake 440

Water wash 467.0 To ETP

DM Water Wash 440

Crude Wet Cake 413

10% NaHCO3 Wash 88.0 Soda Wash water 415 To ETP

Water wash 300 Loss in process 0.0

Crude Wet Cake 386

Filtrate 447 To Methanol

Methanol 386 Recovery

Wet Cake 325

Loss 37.0

3 NAP Product 288

Purification & Filtration

Drying

Mixed Acid Preparation

Nitration

Quenching /Drowning

Crude Filtration

Washing & filtration-1

Washing & filtration-2


75

Production 3-Amino Acetophenone 48 MT/Month

Reaction: Preparation of 3-Amino acetophenone (3-AAP)

O CH3

NO2

O CH3

NH2

3-NAP 3-AAP

540

+ 3 Fe3O4+ 9 Fe4 + 4 H2O 4

696504 72660


In this step, we simultaneously take the required qty of water, 10% sulphuric acid, Iron powder &

Ammonium chloride into the reactor. Then we added the lot wise Iron powder & AAP slowly into same

mass by maintaining the reaction temperature. After completion of reaction, we filtered out the reaction

mass & removed the Iron powder, which recyled to the next batch. Then we added the sod. dithionate &

chiiled the reaction mass, after that we filtered out the AAP by using Centrifuge. Wet AAP then dried

into the dryer & we got finished AAP as a product.

BLOCK DIAGRAM

Stage 2- Preparation of 3 Amino Acetophenone (3 AAP)

Water 900.0

Acetic Acid 13.0

Iron Powder 25.0

3-NAP 325.0

10% Sodium Bicarbonate Sol. 247.0

Water wash 200.0

Reaction Mass 1697.0

Water for washing 0.0 Iron sludge 41.7 Recyle


Sodium Diothionite 0.9


Water Wash 100.0 ML 1481.2 To Disposal

ETP

Wet - 3AAP Cake 275.0

Moisture 55.0

Dry 3AAP Product 220

220 kg/batch3 AAP Product Eq.to 3 NAP Batch

Reaction

(Reduction at 85-90 °C)

Nutsch Filter

(Filtration at 85-90°C)

Crystallization

(at RT)

Centrifuge

(at RT)

Drying


76

14) 3 HAP

Reaction: Preparation of 3-Hydroxy acetophenone (3-HAP)

O CH3

NH2

O CH3

OH

3-AAP

135.16

+

3-HAP

136.2

++1/2 H2SO4NaNO2

Diazotization

Hydrolysis+ N21/2 Na2SO4 + H2O

49 69 71 28 18

Process Description:STEP-1 Dizotization & Hydrolysis

STEP-2 Purification

In this step, we simultaneously take the required qty of water, Methanol, wet cake (3HAP) & charcoal into the reactor.

Then heated the mass up to 60-65°C & maintained it for 1 hrs. Then filtered out the reaction mass through sparkler filter.

The clarity of the reaction mass is checked & the clear solution is taken into another reactor. Then filtered out the slurry

mass through centrifuge. The wet cake (3HAP) is being filled into the bags & Filtered ML transferred to storage tank for

recycling to next batch. Wet 3-HAP then dried into the dryer & we got finished 3-HAP as a product.

In this step, we simultaneously take the required qty of water, 98% sulphuric acid, 3-Aminoacetophenone & toluene into

the reactor. Then we added the NaNO2 Solution slowly into same mass by maintaining the reaction temperature. After

completion of reaction, the reaction mass cooled down up to 5°C & filtered out through Centrifuge. Wet 3-HAP then dried

into the dryer & we got crude 3-HAP.


77

15) TFMAP

BLOCK DIAGRAM

40% SNI Solution 463

Water 1100

98% Sulphuric Acid 861 DIAZOTIZATION & HYDROLYSIS

3-AAP 300 GLR

Toluene 857 6.3KL

Hydrose Powder 0.309

Hydrolyse Mass 3581

5% Soda Sol. Wash 200

CENTRIFUGE

SS-316

48"

ML (Excess acid + Toluene) 3472

309

SEPARATOR

GLR

6.3 KL REUSED

Excess Acid 2615

Toluene 857

REUSED

Distil Toluene 840

TOLUENE DISTILLATION

SS316

2 KL

Residue 17

Water 1400

Methanol 50 PURIFICATION

Charcoal 9 SS316

5 KL

Hyflow Supercell 3

SPARKLER FILTER

SS316

15" X 8 PLATES

Hyflow + Charcoal 15

Organic Mass 1756

Hydrose 0.857

SS316

10 KL For 3-HAP Recovery

Oily Layer 261

Organic Mass 1495

CENTRIFUGE

SS-316

48" ETP

ML 1230

3-HAP Pure Wet Cake 265

Water Vapors 46

DRYING (FBD)

SS-316

350 KG

3-HAP Pure Dry 219

SEPARATION &

CRYSTALLIZATION

Crude 3-HAP Wet Cake


78

3'-(Trifluoromethyl) - acetophenone Production 200 MT per Month

Reaction Schem of TFMAP

Stage :- I Dizodization

Stage :- II Hydrolysis

H2SO4 + NaNO2 +

CuSO4

+ HCl

CF3

NH2

+

CF3

N

OH

CF3

N

OH

CF3

O

Sulfuric Acid 98

Sodium Nitrite 69

+ N2 + 1/2 Na2SO4 + 2 H2O

AAO59.07

3-ABTF161.13

+ NH2OH.HCl

TFMPOL203.16

Sodium Sulfate142

Water2x18

TFMPOL203.16

Hydro Chloric Acid 36.5

TFMAP188.15

Hydroxylamine hydrochloride

69.5

CH3

CH3

N-OH

H

CH3

Nitrogen14

Process Description :-

1. 3'-(Trifluoromethyl)- acetophenone oxime is prepared by 3-amino-benzotrifluoride diazotization and with acetaldoxime.

Stage-II

2. 3'-(Trifluoromethyl) - acetophenone is prepared by hydrolysis of 3- (Trifluoromethyl)- acetophenone-oxime.

3. In Distillation 3'-(Trifluoromethyle)-Acetophenone is separated as finished product.


79

16) Me PPDA Sulphate

BLOCK DIAGRAM

Stage I 3'-(Trifluoromethyl) - Acetophenone Oxim.

INPUT kg OUTPUT kg

3-AMINO BTF 550

WATER 3000

NaNO2 253 Diazo Mass 4427

Cons. H2SO4 608

Sulfamic acid 15

4427 4427

TOTAL MASS 4427 Recycle 890

Organic Layer 1890

Water 890

CuSO4 51.2

Toluene 1175 ETP

Acetic acid 69 Aquess Layer 6250 5360.5

Acetaldoxime 483

30 % NaOH 1045

8140 8140

Stage II 3'-(Trifluoromethyle)-Acetophenone

Organic layer 1890 Organic Layer 1678

Aqueous Layer 688

30 % HCl 688 Loss 212 200

2577 2577

Organic Layer 1678 Organic Layer 1678 Aq Layer to ETP

3 % Caustic Soln 426 Aqueous Layer 426 588

2104 2104 38

Toluene 1116 Pure OH BTF

Toluene Layer 1678 Crude Mass 561 52.4

1678 1678

Residue

62

1 st Fraction 36.3

Crude Mass 561 2 nd Fraction 79.6

Last Cut 76

Residue 32.0

561 561

Pure CL BTF

5

TFMAP 337 Kg / Batch

TFMAP Recovery from 2nd & Last Cut 100.4 Kg / Batch Last Cut Recycle

31.3

TFMAP Total 437 Kg / Batch

STAGES

Multiple Effect

Evaporator

Acidification

Distillation

Distillation

Diazo Mass Preparation

Coupling

Hydrolysis

Washing and Layer Separation

Distillation

Solvent Recovery


80

2 Methyl P- Phenylene Diamine Sulphate 100 MT per Month( 2 MePPDA Sulfate )

Reaction Scheme

Step 1 - 2-Methyl-p-Phenelene diamine

Step 2 - 2-Methyl-p-Phenelene diamine sulfate

Azo Amino

M Wt - 225 M Wt - 4

Hydrogen2-Methyl-p-

Phenelene diamine

M Wt - 122

Ortho

M Wt - 107

2-Methyl-p-Phenelene diamine

M Wt - 122

Sulphuric Acid

M Wt - 98


Sulphate

M Wt - 220

Azo Amino

M Wt - 225 M Wt - 4

Hydrogen2-Methyl-p-

Phenelene diamine

M Wt - 122

Ortho Toluedine

M Wt - 107


M Wt - 122

Sulphuric Acid

M Wt - 98


Sulphate

M Wt - 220

CH3

N NH2

CH3

N

CH3

NH2

CH3

NH2

NH2

H2/ R-Ni

+100°C

CH3

NH2

NH2

NH2

NH2

CH3

H2SO

4

H2SO

4

Methanol + Rec. OT

Process Description :- Stage-I

1. 2-Methyl-p-Phenelene diamine is prepared by Hydrogenation in the presence of methanol + Rec. OT as a solvent.

Stage-II

2. 2-Methyl-p-Phenelene diamine Sulphate is prepared by reacting with sulfuric acid.

3. In filtration the solid 2-Methyl-p-Phenelene diamine sulphate is separated from mother liquor.


81

17) DBPPDA

BLOCK DIAGRAM

Stage I

INPUT kg OUTPUT kg

Azo Amino Toluene 1300

Azo dye Mass 2817

Methanol 1517

2817 2817

TOTAL MASS 2817

Organic Layer 2821

Raney Nickel 1.22

Hydrogen 3.0

2821 2821

Organic layer 2821 Organic Layer 2820

Catalyst 1.22

2821 2821

Organic Layer 2820 Crude MePPDA 1303

Methanol 1441

Losss 75.9

2820 2820

Methanol + OT 108

Crude MePPDA 1303 Pure OT Cut 431

Mixed Cut 69

Main cut 570

Residue 125

1303 1303

Stage II

Pure MePPDA 570 MEPPDA Sulfate 3419

Water 2279

H2SO4 570

3419 3419

MEPPDA Sulfate 3419 Wet Cake 1128

1 st Wash Water 2708 M.L.-1 2291

2 nd Wash Water 2925 M.L.-2 2708

M.L.-3 2925 Recycle

9052 9052

Wet Cake 1128 Moisture Evaporated 188

1128 1128

MEPPDA SULFATE 940 Kg

STAGES

ETP

Methanol +Azo dye

Preparation

Hydrogenation

Separation

Methanol Recovery

2MePPDA Sulphate

Preparation

MEPPDA Distillation

Filtration

Drying

Methanol +Azo dye

Preparation

Hydrogenation

Separation

Methanol Recovery

2MePPDA Sulphate

Preparation

MEPPDA Distillation

Filtration

Drying


82

Production of DBPPDA 100 MT

RXN Scheme :-

Stage :- Hydrogenation of PNA

PNA Methyle Ethyle Ketone Hydrogen DBPPDA Water

138x1 72x2 2x4 218x1 18x4

NO2

NH2

O

2

NH

NH

+ + 4 H2 + 4 H2O

PROCESS DESCRIPTION :-1 Para Nitro Aniline is mixed with Methyle Ethyle Ketone.

2 The Mixture is then Reduced by Hydrogen gas in presence of Catalyst.

3 The Aquess layer from Reduced Mixture is Seperated and transferred to ETP.

4 The Organic Mass is transferred to Distillation Kettle for Methyle Ethyle Ketone Recovery.

5 The Final Product Di Secondary Butyle Para Phenyle Di Amine is the Packed in Drums.


83

18) 1,3 CHD

INPUT MT KL PROCESS OUTPUT MT KL

MEK 1800 1800 Reaction mass 2800 2800

PNA 1000 1000

Reaction mass 2800 2800

OPA 2.05 1.95Hydrogenated

mass2803.69 2803.22

3% Pt on C 0.75 0.38

Hydrogen M3 0.890 0.89

Hydrogenated mass 2803.69 2803.22Recovered

catalyst0.75 0.375

Filtrate 2803 2803

Filtrate 2802.9 2802.8 Org. layer 2207 2207

Aq. Layer 596 595

Org. layer 2207.44 2207.44 Recovered MEK 670.0 670.0

Loss of MEK 18 18

DBPPDA MT

1519

MATERIAL BALANCE of DBPPDA

MIXING

HYDROGENATION

FILTRATION

SEPERATION

DISTILLATION


84

1,3-CHD Production 100 MT/Month

REACTIONS FOR 1,3 - CHD

Step 1

Resorcinol + C.Soda Lye + hydrogen Sodium salt of CHD + water

M 110 40 2 134 18

Step 2 (Precepitation)

Sodium salt of CHD + HCl 1,3 CHD + NaCl

M 134 36.5 112 58.5

OH

OH

+ NaOH + H2

ONa

O

+ H2O

ONa

O

+ HCl

O

O

+ NaCl


STEP 1 - Hydrogenation.

STEP 2 – Acidification

In this Step, Hydrogenation is carried out in the presence of caustic lye. The Resorcinol

is charged into hydrogenation reactor. Hydrogenation addition is started at specified

Temperature & pressure. The temperature & pressure are maintained within specified

limits during reaction. After completion of reaction, Sodium salt of 1 3 cyclohexanedione

formed & which is used for further acidification process.

In this step, the required quantity of Sodium salt of 1 3 Cyclohexanedione is taken into

the reactor & then added the required quantity of 30 % HCL into the same. After

complete addition, 1 3 Cyclohexanedione formed which is filtered & dried in the dryer.


85

19) SMIA

BLOCK DIAGRAM

QTY(MT) QTY(MT)

Resorcinol 1407

Water 1578

48% Caustic soda lye 1122.0825 Catalyst recycle

Catalyst 54.52125

Total 4161

catalyst

Hydrogenated mass 4161Filtered

Hydro. Mass

ISOLATION

Hydrogenated mass 4161

HCl 30% 1401.5

Total 5563

Slurry for centrifuging 5563 Wet Cake 1475

Filtrate 4088 3716.4

(Dilute effluent)

Wet cake 1474.626136 Dry Ca ke (1,3 CHD) 1179.7LOD 294.93

Recycle Ethyl Acetate

Ethyl Acetate 2171

Dry Cake (1,3 CHD) 1180

TOTAL 3350

Reaction mass 3350

Reaction mass for

crystalisation 3350

Wet cake 1132.4

ML 2218

Dry

1,3 - CHD

(product) 1019

1,3,CHD

CRYSTALLISATION

ISOLATION

FILTRATION

DRYING

HYDROGENATION

FILTERATION

DISSOLUTION

FILTRTION

CRYSTALISATION

CENTRIFUGE

Dryer


86

Production of SMIA 25 MT/Month


87

Brief Process

A Stage : Oxidation.

1 Set up assembly of 5 lit Resin Kettle.

2 Charge water start stirring and Heating to 60°C.

3 add HCl (30%) heat to 60°C.

4 Add 2-Acetyl furan in 20-30 min.

5 Add SNI (lot-1 60%) solution(40%) in 6 hr at 60°C.

6 Add catalyst-A in 15-20 min at 60°C.

7 Add SNI solution (40%) (Lot 02 40%) at 60°C.

8 Cool the reaction mass to 20°C

9 Extract the reaction mass with Methelene dichloride

10 Recover 2-acetyl furan by distillation o the MDC by atm.distillation.

11 adjust pH 4.5 by CS lye solution.

B Stage : Oximation.

1 In the reaction mass add MA HCl solution in 1 hr at 20°C.

2 Maintain the reaction mass at 20°C pH 4.0-4.5 for 2 hr.

3 Cool the reaction mass to 5-10°C ,add Butyl acetate.

4 Add HCl 30% till pH 0.2 at 0-5°C

5 Add NaCl separate the n-Butyl acetate layer and Aq. Layer.

6 further extract with n-butyl acetate 2 times

C Stage : SMIA Ammonium salt.

1 Set up 2 lit RB add the n-Butyl acetate solution in 2 lit RB, cool to 10°C

2 Purge the ammonia gas till pH 6.5-7.0 at 10 15°C,maintain for 30 min

3 Filter the reaction mass trough centrifuge, Spin well for 30- 60 min.

4 collect the wet cake,filtrate Butyl acetate, Oily solution

D Stage : Purification

1 In 2 lit resin kettle take SMIA wet cake Methanol at 25-30°C. .

2 Start stirring and raise temperature to 50-55°C to get clear solution.

3 Filter reaction mass at 50-55°C through hyflo bed

4 Distilled 50% methanol by weight of filtrate ml

5 Cool bottom mass to 0-5°C and centrifuge solid at 0-5°C

6 Dry the wet cake

7 Recovered the SMIA from filtrate.


88

20) Triazenone

FLOW DIGRAM

Input Output

No Raw Material Qty(g) den g/ml Qty (ml) No Raw Material Qty(g) den g/ml Qty (ml)

1 water 1200 1 1200 1 Reaction mass 3074 1.02 3013.7

2 HCl 600 1.14 526.316 2 Rec MDC 200 1.33 150.4

3 2Acetyl furan 222 1.12 198.2 3 Rec 2Acetyl furan 60

4 Sodium Nitrite (40% ) 1258 1.29 975.194 4 Loss 111

6 Acid catalyst 80 0.95 84.2 5 Nox to scrubber 215

7 MDC 300

8 Reaction mass 3074 1.02 3014 5 Aqeous layer 3968 1.2 3306.7

9 MA HCl (42%) 258 6 n-BuAc extract 914 0.9 1015.6

10 NaOH 48% 148 7 loss 180

11 HCl (30%) 372 1.14 326

12 NaCl 550

13 n-Butyl acetate 01 660 0.89 742

14 n-butyl extract 914 0.9 1015.6 8 SMIA salt wet cake 190

15 Ammonia (gas) 20 9 Rec. n- BuAc 630 0.88 715.9

10 Org. oily (impurity) 44 0.9 48.9

11 loss 70

16 SMIA salt wet cake 190 12 SMIA salt wet cake 153 0.5

17 Methanol 1200 0.791 1517.1 13 Distilled Methanol 916 0.791 1158.0

14 Methanol Filtrate 245

15 Loss 76

Oxidation - At

temperature 60°C addition

of SNI solution , addition of

acid catalyst and SNI

solution in pH 3.0 to 3.5

Oximation- temp 20°C,pH

4.0 , maintain for 2

hr.extract with n-BuAc.at

pH 0.2

NH3 gas purging at 10°C

till pH 7.0,maitain for 30

min. centrifuge , spin dry

Purification- By using

Methanol dissolve SMIA in

methanol clarify,

concentrate, cool

Process


89

1,2,4 Triazinone

Block Diagram - 1,2,4 Triazinone

INPUT

Description Quantity UOM

Water 591 Kg

48% Caustic 266 Kg

Dichloro Pinacolone (DCP) 150 Kg

Total 1006 Kg

Catalyst 0.35 Kg

12% NaOCl 591 Kg

Total 1597 Kg

Catalyst Kg 0.34

Loss Kg 17.5

Filtrate ml

(Part-A)Kg 1579

Water 425 Kg

98% H2SO4 106 Kg

Thiocarbohydrazide (TCH) 89 Kg

Filtrate ml (Part-A) 1579 Kg

Total 2199 Kg

50000

ML Kg 1928

Loss Kg 90

Wet Cake Kg 181

Water Wash 1 354 Kg

Cake 181 Kg

Total 536 Kg

ML Kg 358

Wet Cake Kg 177

Water Wash 2 354 Kg

Cake 177 Kg

Total 532 Kg

ML Kg 358

Loss Kg 8

Wet Cake Kg 165

Moisture Kg 17

Loss Kg 1

Dry

PowderKg 148

Centrifuge

GLR

Centrifuge

Dryer ( VTD )

Reactor

Reactor

Catalyst Filter

GLR

Centrifuge

GLR


90

21) TCH

B SOP1 Arrange 3 lit 4-neck RBF having half moon stirrer, thermo pocket, condenser having normal water supply, kept on water batch.

2 Charge water (1000 g) and 48% CSLye (450 g) at 25-30°, raise temperature to 60-65°C under stirring.

3 Make 10 equal part of Dichloro Pinacolone (25.4 g X 10) and add one by one lot at 60°C with in 30 min time interval.

4 Ensure pH of mass become 12-13. post stirring mass for 1 hr at 60°C.

Note:- Remove sample and check % NaCl, which is between 9.5-10.5%

5 Cool mass to 40°C under stirring and add 0.6 g catalyst.

6 Start addition of NaOCl (1000 g) in 1.0-1.5 hr at temperature 40°C, post stirring mass for 2 hr at 70°C

Note:- Freshly prepared NaOCl use

Note:- Remove sample & filter catalyst then submitted sample for wt% Oxy acid on HPLC, which is 6-7%

7 Filter catalyst at 30-40°C and wash with plan water (20 g) .

Note:- Catalyst recycle in next batch. Transfer filtrate ml in addition funnel for addition.

8 Mean while arrange 5 lit 4-neck flask having half moon stirrer, thermo pocket, condenser having normal water supply, kept on water batch

9 Charge water (720 g), 98% H2SO4 (180 g) , TCH (150 g) and start heating to 70°C under stirring.

10 Start addition of filtrate ml in TCH + H2SO4 at 70-75°C in 0.5-1.0 hr.

11 Post stirring mass for 1-2 hr at 70-80°C then cool mass and filter solid through centrifuge

12 Wash wet solid under stirring by DM water (2 time as per wet solid) at 50-55°C and hot filter solid through centrifuge. Dry solid at 80°C till LOD become less than 0.5%.

TCH reaction scheme

Stage Preparation of Thiocarbohydrazide (TCH)

Brief process

1 Arrange 1 lit 4-neck resin kettle having half moon stirrer, thermo pocket, condenser having normal water supply, kept on water batch.

2 Arrange 20% Cslye trap to scrub H2S which is comes out through condenser during reaction.

3 Charge hydrazine hydrate & Catalyst in 1 lit reactor at 30°C and start stirring.

4 Cool mass to 10-15°C under stirring and start addition of carbon disulphide (lot-1) in 1-1.25hr.

5 Start addition of carbon disulphide (Lot-2) in 1-1.25 hr, keep pH of mass 9-10

6 After addition stir mass for 3 hr at 20-25°C then raise temperature to 85-90°C

7 Post stirring mass for 10 hr at 85-90°C.

8 Remove sample and filter through cloth then wash solid samplr with equle ammount of water and send for analysis by titriometric.

9 Then cool mass to 10-15°C and filter through bucchner funnel by filtration cloth.

10 Unload wet solid and add DM water (100 g ) under stirring and raise temperature to 90-95°C .

Note:- During heating vent of condenser should be dip in cslye scrubber

11 After 1 hr post stirring cool mass to 10-20°C and filter solid

12 Suck dry under vacuum and unload wet solid and dry solid at 80-85°C till moisture become less than 0.5%


91

22) 2-CN Phenol

Item UOM Quantity Item UOM Quantity

Hydrazine hydrate kg 157

Carbon disulphide (Lot-1) kg 38

48% Cslye kg 10

Carbon disulphide (Lot-2) kg 39

48% Cslye kg 13

H2S gas kg 119

Wet solid kg 100

Filtrate ml kg 138

Water kg 100 Wet solid kg 95

Wet solid kg 100 Filtrate ml kg 105

Wet solid kg 95 Drying Loss kg 5

Dry solid kg 90

Post stirring for 3 hr at 20-30 & pH-9-10°C

Raise temperature to 85-90°C

STEP- ChlorinationINPUT

Reactor

Cool to 10-15°C

pH- 9-10

Post stirring for 5-10 min & pH-9-10°C

pH- 9-10

Post stirring for 6 hr at 80-85°C

Cool to 20-25°C and filter

Water wash at 90-95°C

Drying

OUTPUT

Project:- Thiocarbohydrazide 100 MT/M


92

Project 2-Cyano phenol

Reaction scheme


93

Project: 2-Cyano phenol

Process

Stage 01

Set Up: 0.5 Lit RBF with condenser, stirrer, water bath, thermowell

1 In clean & dry RBF add methanol start stirring

2 Add salicylic acid stirr well to get clear solution

3 add slowly concentrated sulfuric acid.

4 Maintain reflux for 5 h.

5 Distilled excess methanol at atmospheric pressure

6 Cool the reaction mass to RT.

7 Pour the reaction mass in water

8 Separate the Organic layer & aq. Layer

9 Wash the org. layer with water.

10 Distilled the methyl salicylate under reduce pressure

Stage 02

Set Up: 1.0 Lit RBF with condenser, stirrer, water bath, thermowell

1 Mix the Raw material ammonia soln, methyl salicylate ,ter Butyl amine & sodium meta bisulphite

2 Heat the reaction mass 40°C & maintain for7 hr.

4 recovere excess ammonia by distillation.

5 Cool the reaction mass to RT.

6 Set the pH 5.5 by using dilute H2SO4.

7 Filter the reaction mass

8 Dry the Cake

Stage 03

1 Ensure clean and dry 5 Lit RBF assembly with stirring, addition pot & Dean stark apparatus

2 Charge MCB and salicylamide start stirring & heat to 110

3 Add solid salicylamide and start heating at temperature 110oC

4 Add Thionyl chloride , scrub the HCl & SO2 gasses in water & alkali solution

5 After completion , recovered the MCB

6 Distilled the product 2-Cyano Phenol.

7 Residue to ETP/ inciniration


94

23) 4-Chloro-6-methylanthranilimide

150 MT/M

Details Qty (g) MW Moles Details Qty (g)

Salicylic acid 200 138 1.4348 Reaction mas01 695

Methanol 450 32 13.922

Sulfuric acid 45 98 0.45

Reaction mas 01 695 Reaction mas 02 315

Recovered methanol 380

Reaction mas 02 315 organic layer 245

water 500 Aq. Layer 555

water for wash 250 water wash 265

organic layer 245 Methyl Salicylate 195

Residue 35

loss 15

Details Qty (g) MW Moles Details Qty (g)

Methyl Salicylate 264 152 1.72 Reaction mass 615.5

Ammonia Solution 348 17 5.12

TB Amine 1.4 59 0.02

Sod meta bisulphite 2 190 0.01

Reaction mass 615.5 Reaction mass 540

Recoverd ammonia 50

Loss 25.5

Reaction mass 540 Wet cake 255

Sulfuric acid 2 98 filtrate 285

Wet cake 255 Dry Salicilamide 200

Drying loss 55

MCB 1000 112.5 8.8 NaOH scrubber 436

Salicylamide 138 137 1.00 Loss 58.5

Thionyl chloride 138.5 119 1.15 Reaction mass 1082

47% NaOH scrubber 300 40 3.53

Reaction mass 1082 Recovered MCB 960

Crude mass 122

Crude mass 960 Residue 20

2-Cyano phenol 102

MCB recovery under vacuum

Reflux the reaction mass for 5 h

Stage 03

Distillation

High vacuum distillation

Stage 02

Distilled methanol at atmospheric

pressure

Dry @ 95°C

drowning in water , wash the organic

layer by water

maintain for 110-115°C

Project: 2-Cyano phenol

Stage 01

Maintain the reaction mass for 7 h at

40°C

Recovered ammonia below 65°C

Adjust pH to 5.5 by H2SO4, filter &

suck dry wel


95

4-Chloro-6-methylanthranilimide

CH3 COOHCH

3COOH

NO2CH3

COOH

O2N

CH3

COOH

NO2

m-Toluic acid 3-Methyl-2-nitrobenzoic acid

+

4-Nitro-3-methylbenzoic acid;

+

3-Methyl-6-nitrobenzoic acid

Conc.HNO3

Nitration at 10-15°C


1 Charge conc. HNO3 carefully to 4-neck flask, start stirring and cool to 10-15°C

2 Start addition of solid m-Toluic acid (MTA) pinch by pinch by maintainig temperature of reaction to 10-15°C

3 Complete addition of solid within 1-1.5 hr then keep post stiring for 30 min

4 Check inprocess sample for unreacted MTA.

5 Add chilled water within 2 hr slowly at 10-15°C

6 Filter solid through filter cloth and preserve filtrate mL

7 Wash wet solid with 2 x100 ml water and suck well using vacuum pump

8 Dry the solid at 80°C till moisture is < 1%

9 Hydrogenation of 2-NMTA in methanol using catalyst & H2, then distilled methanol and filter solid.

10 Chlorination of 2-Amino-m-toluic acid using N-Cl-scuccinamide in DMF at 100°C then extracted product using ethyl acetate.

11 Methylation of 2-AMTA using DMS, DBU in acetonitrile at 0-5°C, isolate product after water wash

12 Amination using methyl amine at 60°C and isolate product after workup and water wash

13 Dry at 80-100°C till LOD become less than 0.5% and submitted sample for analysis


96

24) Adenine

Item UOM Quantity Mole wt Mole Item UOM Quantity Mole wt Mole

Conc. HNO3 ml 1171 63 18.2

m-Toluic Acid g 309 135 2.3 Reaction mass (A / addition) g 1460

HNO3 (70%) g 155.5 63 1.7 Wet 2-NMTA- Crop-1 (wet) g 188.5

Washing water g 310 18 17.2 Total acidic filtrate ml g 1350

Washing ml g 325

Wet crop-1 (188.5 g)

Dry crop-1 g 181 181 1.00

Washing ml g 325

Fresh water g 652.5

Total acidic filtrate ml g 1350 1.4 964.3

Wet crop-2 g 275

Aq. Filtrate ml g 1901

Wet crop-2 (275 g)

Dry crop-2 g 135 181 0.7

Item UOM Quantity mole wt Mole Item UOM Quantity mole wt Mole

2-Nitro-m-Toluic acid ml 181 181 1.0

5% Pd/C g 1.5 Recover catalyst g 1.45

Methanol g 550 32 17.2 Recover methanol g 500

Hydrogen nm3 85 2 42.5 2-Amino-m-toluic acid g 136 151 0.9

2-Amino-m-toluic acid g 136 151 0.9 4-Cl-2-Amino-m-Toluic acid g 126 185.5 0.7

DMF g 425 73.1 5.8 Recover DMF g 340 73.1 4.7

N-Cl-Succinimide g 120.5 133.53 0.9 Recover ethyl acetate g 385

Water g 375 18 20.8 Water wash g 625

Ethyl acetate g 450 Succinimide g 75.8 99.09 0.8

4-Cl-2-Amino-m-Toluic

acidg 126 185.5 0.7

Methyl 2- amino-5-Cl-3-methyl

benzoateg 115 199.64 0.6

Acetonitrile g 500 41 12.2 Recover Acetonitrile g 400 41 9.8

Dimethyl sulphate g 102 126.13 0.8 Recover methanol g 102 126.13 0.8

30% HCl g 110 36.5 0.9 Water wash g 400

Water g 500 18 27.8

Methanol g 275 32 8.6

DBU g 112.3

Methyl 2- amino-5-Cl-3-

methyl benzoateg 115 199.64 0.6

4-Cl-6-Methyl anthranilimideg 65 130 0.5

Acetonitrile g 345 41 8.4 Recover Acetonitrile g 275 41 6.7

Mono methyl amine g 85 31.05 2.7 Recover ethylene glycol g 260 62.07 4.2

Ethylene glycol g 345 62.07 1.7 Water wash g 613

Water g 437.5 18 24.3

OUTPUT

1-Lit 4-Neck Flask

Filtration

Drying

Dry Crop-1

80°C/ 10 Kg H2 pressure then filter

catalyst and distilled methanol

Recycle to Next batch

Quenching, At 15-20°C

INPUT Nitration

Distilled DMF and wash with 250 g X 3 by

water and purified by ethyl acetate

STEP-4 (Methylation)

Methylation at 0-5°C then isolate product

by purification and treatment using HCl &

methanol then wash product with water

(500g X 2)

Amination by purging monomethylamine

gas at 60°C then isolate product after

water washing

Quenching,

OUTPUT

Filtration

Drying

2-Lit reactor

STEP-5 (Amination)

INPUT STEP-2 (Hydrogenation)

Chlorination at 100°C/30 min

Dry Crop-2

STEP-3 (Chlorination)


97

6-Aminopurine (Adenine) reaction scheme

Stage: 1 Preparation of Phenylazomalononitrile

Stage: 2 Preparation of 6-Aminopurine(Adenine)


98

Process description

Stage: 1 Preparation of Phenylazomalononitrile

1 Ensure clean and dry 3 l it assembly

2 Charge water and start stirring add slowly sulphuric acid cool

3 Addition of Aniline by maintaining temp

4 Cool mass to desired temp

5 Addition of NaNO2 solution by maintain temp

6 Maintain temp

7 Check SI Paper and kil l extra SNI by adding ammonium sulfamate

8 Add water and dissolved Malononitrile with heating and cooled it

9 Addition of Malononitrile solution in diazo mass maintaining temperature

10 Addition of Sodium hydroxide slowly by maintaining temp

11 Maintain temp & pH

12 After maintaining increase temp up to RT

13 Take weight of fi ltrate give sample for analysis. Send to ETP

14 Charge water for wet cake washing and add wet cake under stirring Heat mass for hot fi ltration

15 Dry wet cake at desired temperature

16 Use dry Phenylazomalononitrile for second stage

Stage: 2 Preparation of Adenine from Phenylazomalononitrile

1 Charge formamide in 3 l it RBF start stirring and cool

2 Start ammonia purging in formamide to prepare solution

3 Charge ammonical formamide solution in 2 l it autoclave and add Phenylazomalononitrile

4 Box up autoclave and start stirring and heating

5 Maintain reaction temperature

6 After completion of reaction the agitation speed decreased, ammonia released by gradually opening valve

7 Scrubb ammonia in water

9 Add Catalyst to reaction mass

10 Box up autoclave and start stirring and heating

11 Flush autoclave with Nitrogen gas then take Hydrogen pressure

12 After Hydrogen gas consumption maintain Pressure and temperature

13 Increase temp and pressure

14 Filter the catalyst

15 Filtrate transfer for Formamide recovery under vacuum

16 Recovered first cut of formamide containing moisture and then Foramide mian fraction

17 Recycle formamide in next batch

18 In bottom mass add water

19 Hot fi ltration to remove impurities

20 Add charcoal and stir for 30 min and fi lter

21 Discard charcoal sludge

22 Cool fi ltrate and Isolate Adenine by fi ltration and suck dry.

23 Recycle purification fi ltrate

24 Final product dry


99

25) PMPA

DM Water 1000

Sulphuric acid 155

Aniline 98

Sodium Nitrite 76.1

Water for NaNO2 152

Diazo mass 1481.1

Recycle

Diazo mass 1481.1

Malononitrile 59.5 Aq.Filtrate 1464.6

NaOH 185

Water for NaOH 69

Wet cake 330

Washing filtrate 1060

Wet cake 330

Water wash 1000 Drying water loss 115

Dry powder 155

NH3 gas 25

Dry phenyl azo

malonitrile155 Water recovery 20

Formamide 1320

Ammonia 40

Reaction mass 1470

Reaction mass 1470

Raney-Ni Catalyst 5

Hydrogen gas 3.8

Hydrogenated mass 1478.8

Reco Raney Ni

catalyst5

Hydrogenated mass 1478.8

Filtrate 1473.8

Rec.Formamide 1140

Bottom mass 268

Vapour loss during

distillation65.8

Bottom mass 268

DM water 2000 Aq filtrate 2267

Activated charcoal 20 Charcol sludge 21

Aq filtrate 2190

Aq filtrate 2267

Drying loss 9

Dry Adenine 67.5

Diazotization reaction

Condensation reaction

Hydrogenation

Washing and drying

Cyclization

Hot filtration

Formamide recovery

Charcolisation

Under reduced pressure

Cyclization

2 lit RBF

Cooling and filtration

Wet cake drying


100

Project Name : PMPA (TENOFOVIR)

Stage:1 Preparation of (R)-9-(2-Hydroxypropyl) adenine

Stage:2 Preparation of (R)-9-[2-(Phosphonomethoxy) propyl] adenine

Project Name : PMPA (TENOFOVIR)

Stage:1 Preparation of (R)-9-(2-Hydroxypropyl) adenine

Process:

1 Arrange 10 lit resin kettle on heating Bath having stirrer, Thermo pocket, condenser with water circulation.

2 Charge Adenine and DMF at room temperature under stirring.

3 Add NaOH flakes followed by addition of (R)- Propylene carbonate drop-wise at room temperature.

4 Heat the reaction mass to reflux temperature and maintain till the reaction complesed.

5 Cool the reaction and add methanol-isopropyl alcohol mixture then stir.

6 Filter the solid then wash the solid with chilled isopropyl alcohol.

7 Dry the product under vacuum at 60°C.

Stage:2 Preparation of (R)-9-[2-(Phosphonomethoxy) propyl] adenine

Process:

1 Arrange 10 lit resin kettle on heating bath having stirrer, Thermo pocket, condenser with water circulation.

2 Charge Dimethyl formamide followed by addtion of (R)-9-(2-Hydroxypropyl) adenine then stir the reaction at room temperature.

3 Cool the reaction mass and add slowly NaNH2 to the above solution then add MgCl2 powder lot wise at ambient temperature.

4 Heating raise to room temperature and add diethyl p-toluenesulfonyloxymethyl phosphonate solution (dissolved in toluene) slowly then maintain the reaction at warm temperature

5 Again cool the reaction mass and purged dry HCl for few hours then again raise temperature to reflux and maintain.

6 After completion of the reaction quenched the mass in water and wet cake washed with MDC at room temperature.

7 Separate the MDC layer and aquoues layer precipitated out with NaOH solution then stir for few minutes.

8 Filter the solid then wash the solid with chilled water followed by acetone.

9 Dry the product under vacuum at 70°C.


101

26) S-Alcohol (Duloxetine Int.)

Adenine 1.39

NaOH 0.07

DMF 6.39

(R)-1,2-Propylene carbonate 1.39MeOH 4.44

Isopropanol3.44

Main fitrate ML sent

to recovery

Reaction mass 17.12 16.12

Isopropanol 1.00

Wet Cake 1.54 1.00

Vapour loss

0.3

Dry wt 1.25

NaNH2 0.51

Diethyl p-toluene sulfonyl

oxymethyl phosphonate3.13

MgCl2 0.62

Toluene 3.56

HCl (Dry) 6.55

Reaction Mass 14.36

14.19

MDC 4.38 Vapour loss

Water 11.00 Org. mass 29.74 0.9

NaOH (48% Lye) 1.25

Reaction mass 16.63

water (Chilled) 1.00

Acetone 0.98

Wet Cake(Pure) 1.12 17.49

Vapour loss

0.1

3.56

W/C Drying under vacuum

Filtration Main aquoues ML

send to ETP.

Precipitation

Main Org. layer sent

to recovery

Washing ML send

to recovery

Final Product

Filtration of pure solid


1.0

Quenching and layer

separation

Condensation

Condensation

Hydrolysis


102

Project Name : S-Alcohol (Duloxetine Intermediate)

Stage:1 Preparation of 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride

Stage 2 Preparation of (S)-3-( Dimethyl amino 1-(2-theinyl) 1-Propanol

Process description


1 Ensure clean and dry 1 Lit 4N RBF

2 Charge Isopropyl alcohol (IPA), HCl at RT .

3 Add paraformaldehyde, dimethylamine hydrochloride and first half of 2-acetylthiophene in the above RBF and stir at RT.

4 Heat reaction to ambient temperature and maintain at this temperature for 1hr.

5 Add few crystals of product for seeding to induce partial crystallization. Stirr this mixture for 1hr at at this temperature.

6 Again heat reaction to reflux temperature. Add remaining 2-acetylthiophene. Maintain reaction for 5-6hr or till completion at this temperature.

7 After completion of reaction, cool the mixture. Stirr reaction for 30min at at this temperature. Precipitate of product will observe.

8 Filter solid under suction. Wash two times with chilled IPA. Dry at ambient temperature.

Stage: 2 Preparation of (S)-3-( Dimethyl amino 1-(2-theinyl) 1-Propanol

Part -A

1 Charge 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride in RBF. Add IPA, stirr for 15 min.

2 Adjust PH- 11 to 12 by 25% NaOH ,stirr for 45 min.

3 Separate organic layer and add D.M water and make PH- 9 using H2SO4. at R.T.

4 Transfer whole reaction mass to another RBF. Add IPA.

Part -B

5 Add tri ethanol amine and water in another RBF and stirr it.

6 Add catalyst and stir for 30 min at RT to make homogeneous mixture

7 Add this part -B solution to Part -A and stirr for 30 min.

8 Heat reaction mass under vaccume(600 to 700 mm-Hg vacumm) for IPA and Acetone recovery at RT.

9 Add IPA contineusly to make volume during distillation.

10 Distill solvents till reaction completion

11 After completion of reaction, recover whole IPA and water at warm temperature.

12 Add 50% NaOH till PH -12 to13 and stirr it at at warm temperature.

13 Cool mass to , stirr for 2.0 hrs .Centrifuge it.

14 Add water to wet cake and stirr for 30 min under cooling then again cenrtifuge it.

15 Add toluene to wet cake and stirr for 30 min at ambient temperature. Filter through hyflow

16 Cool filtrate for 1.0 hrs and again centrifuge it.

17 Give sample for HPLC. Dry product in Oven.


103

2- Acetyl Thiophene 1.40

Paraformaldehyde 0.56

Dimethyl amine-HCl 1.27

Conc. HCl 0.06

Isopropyl alcohol 7.19

Reaction Mass 10.5

5.0

Recoverd IPA check

purity & recycle


Triethanol amine 0.94 0.50

Catalyst 0.014Recovered Acetone

with IPA

Isopropyl alcohol 1.05 1.2

Recovered IPA

NaOH Solution 2.96 4.8

Rxn Mass 16.0

Main aquous ML to ETP

Water (w/c washing) 1.00 16.6

W/C 0.4

Solid sludge for disposal

Toluene3.39 0.112

Celite bed 0.10 Toluene Layer 3.7

2.2

W/C 1.5Recoverd Toluene check

purity & recycle

0.4

Bottom residue A/F

Toluene recovery

1.0

Final Product

Toluene filtrate ML send

to recovery

Wet Cake 5.46

Crystalisation

W/C Drying


Bottom residue A/F IPA

recovery

Reduction and resolution

Filtration of stage 1 solidMain Filtrate ML send

for Recovery

Mannich reaction

Filtration of stage 2 solid

Distillation and work up


104

27) N-Methyl Duloxetine oxalate

Project Name : N-Methyl Duloxetine oxalate

Stage:1 Preparation of 3-Dimethyl amino 1-(2-Thienyl) 1-Propanone hydrochloride

Stage 2 Preparation of (S)-3-( Dimethyl amino) 1-(2-thienyl) 1-Propanol

Stage:3 Preparation of (S)-(+)-N,N-dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl) propanamine oxalate


105

Process description


1 Ensure clean and dry 1 Lit 4N RBF

2 Charge Isopropyl alcohol (IPA), HCl at RT .

3 Add paraformaldehyde, dimethylamine hydrochloride and first half of 2-acetylthiophene in the above RBF and stir at RT.

4 Heat reaction to ambient temperature and maintain at this temperature for 1hr.

5 Add few crystals of product for seeding to induce partial crystallization. Stirr this mixture for 1hr at at this temperature.

6 Again heat reaction to reflux temperature. Add remaining 2-acetylthiophene. Maintain reaction for 5-6hr or till completion at this temperature.

7 After completion of reaction, cool the mixture. Stirr reaction for 30min at at this temperature. Precipitate of product will observe.

8 Filter solid under suction. Wash two times with chilled IPA. Dry at ambient temperature.

Stage: 2 Preparation of (S)-3-( Dimethyl amino 1-(2-theinyl) 1-Propanol

Part -A

1 Charge 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride in RBF. Add IPA, stirr for 15 min.

2 Adjust PH- 11 to 12 by 25% NaOH ,stirr for 45 min.

3 Separate organic layer and add D.M water and make PH- 9 using H2SO4. at R.T.

4 Transfer whole reaction mass to another RBF. Add IPA.

Part -B

5 Add tri ethanol amine and water in another RBF and stirr it.

6 Add catalyst and stir for 30 min at RT to make homogeneous mixture

7 Add this part -B solution to Part -A and stirr for 30 min.

8 Heat reaction mass under vaccume(600 to 700 mm-Hg vacumm) for IPA and Acetone recovery at RT.

9 Add IPA contineusly to make volume during distillation.

10 Distill solvents till reaction completion

11 After completion of reaction, recover whole IPA and water at warm temperature.

12 Add 50% NaOH till PH -12 to13 and stirr it at at warm temperature.

13 Cool mass to , stirr for 2.0 hrs .Centrifuge it.

14 Add water to wet cake and stirr for 30 min under cooling then again cenrtifuge it.

15 Add toluene to wet cake and stirr for 30 min at ambient temperature. Filter through hyflow

16 Cool filtrate for 1.0 hrs and again centrifuge it.


Stage: 3 Preparation of (S)-(+)-N,N-dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl) propanamine oxalate

18 Ensure clean and dry 500ml 4N RBF

19 Add 1-Fluoronaphthalene and (S)-(-)-N,Ndimethyl-3-(2-thienyl)-3-hydroxypropanamine in a 500 mL round bottom flask and stirred for 10 minutes.

20 Add Powdered potassium tertiary butoxide and heat to reflux temperature. Maintain reaction for 20-22hr

21 After completion of reaction cool reaction to RT and extract with Toluene

22 Wash aq layer with Toluene. Wash Combined Toluene layer with HCl solution.

23 Wash the acidic aqueous layer with Dichloromethane and wash the combined organic layer with NaOH solution

24 Distill organic layer then add Ethyl acetate and again distill under Vacuum.

25 Add a solution of ethyl acetate and oxalic acid to the reaction mass at RT. and Stirr for 60-90 minutes at RT.

26 Filter the Solid ,wash with cold ethyl acetate twice and dry to yield the product.



106

28) DBTZ (Quetiapine Int.)

2- Acetyl Thiophene 0.75

Paraformaldehyde 0.28

Dimethyl amine-HCl 0.68

Conc. HCl 0.04


Reaction Mass 3.5

2.26

Recoverd IPA check

purity & recycle1.81


Triethanol amine 0.53 0.45

Catalyst 0.010Recovered IPA &

AcetoneH2SO4 0.0400 0.1425

Recovered IPA

48% NaOH Solution 0.56 2.7

Rxn Mass 2.4

Main aquous ML to

ETP

Water (w/c washing) 1.00 2.7

W/C 0.7

Solid sludge for

disposalToluene 1.65 0.112

Celite bed 0.10 Toluene Layer 2.3

1.6


purity & recycle

1.57

Bottom residue A/F

Toluene recovery

0.07

Loss in drying

0.04

1-Fluoronapthalene 0.77

potassium tertiary

butoxide0.58

Toluene 2.810

MDC0.77 Aq layer

HCl 0.12 1.760

48% NaOH 0.040

Water used 2.000

Ethyl acetate 0.52 Recovered Toluene

Oxalic acid 0.46 2.810

0.727 Recovered MDC

0.770

0.52

Recoverd Ethyl acetate

check purity & recycle

0.49

1.2

0.026

Drying vapour loss

0.2

Precipitation

Final Product 1.0

Ethyl acetate filtrate

ML send to recovery

Bottom residue A/F

Ethyl acetate recovery

W/C Drying

Filtration

Org layer sepearation

2.487

5 lit RBF


Reduction and resolution

Distillation and work up

0.667

Crystalisation

Stage 2 Product

W/C Drying


5 lit RBF With N2 ATM

Filtration of stage 1 solidMain Filtrate ML send

for Recovery

Mannich reaction

Bottom residue A/F

IPA recovery

5 lit RBF

Toluene filtrate ML

send to recovery

Wet Cake 1.26

Filtration of stage 2 solid


107

Project Name : Dibenzo [b, f][1,4] thiazepine-11(10H)-one [DBTZ] (Quetiapine Int.)

Stage: 1 Preparation of (2-nitrophenyl) phenyl sulfide

Stage: 2 Preparation of 2-(phenyl sulfanyl)-aniline

Stage: 3 Preparation of phenyl-2-(phenyl sulfanyl)-phenylcarbamate

Stage: 4 Preparation of dibenzo [b, f][1,4] thiazepine-11(10H)-one


108

Process description

Stage:1 Preparation of (2-nitrophenyl) phenyl sulfide

Process:

1

2

3

4

5

6

7

8

9

Stage:2 Preparation of 2-(phenyl sulfanyl)-aniline

Process:

1

2

3

4

5

6

7

8

9

10

11

Process:

1

2

3

4

5

6

7

Stage: 4 Preparation of dibenzo [b, f][1,4] thiazepine-11(10H)-one

Process:

1

2

3

4

5

6

7

8

9

10

Arrange 10 lit resin kettle assembly.

Charge caustic solution.

Add thiophenol at ambient temperature and stir the reaction for 60min at same temperature then add TBAB.

Add 1-chloro2-nitrobenzene at ambient temperature and stir reaction.

Heat the reaction mass to reflux temperature till reaction completion.

After completion of reaction add water in reaction mass atthis temperature and cool the reaction.

Adjust the pH by adding 30% HCl and stir the reaction mass.

Filter the reaction mass at ambient temperature and wash the cake with hot water.

Wet product can be used for next stage on LOD basis.

Arrange 20 lit resin kettle on heating bath having stirrer, thermo pocket, condenser with water circulation.

Charge water, acetic acid and Fe-powder then heat the reaction mass up to warm.

Addition of (2-nitrophenyl) phenyl sulfide solid is done in one lot.

Heat the reaction mass to reflux till reaction completion.

After completion of reaction add water and cool the reaction mass and filter. Filtrate ML keeps separately.

Unload Iron sludge and stir with toluene. Filter and wash the cake with toluene.

Combine both the toluene and to this add main aqueous filtrate then stir the reaction mass for 30min.

Separate the organic layer and wash it with Na2CO3 solution. Separate aqueous layer.

Separate organic layer and wash with Na2CO3 solution and filter and wash with water.

Filter organic layer through celite bed and further wash the organic layer with water.

Separate the organic layer and used in next batch.

Stage: 3 Preparation of phenyl-2-(phenyl sulfanyl)-phenylcarbamate

Arrange 20 lit resin kettle assembly.

Charge stage 2 organic layers and heat the reaction massand start stirring.

Add one part of Phenyl chloroformate solution in Toluene slowly into reaction mass at at warm temperature

and stir.

Take the wet cake in RBF and add methanol for purification.

After the addition raise the temperature and stir till reaction completion.

After completion of reaction add water under cooling condition

Separate the two layers and wash the organic layer with water till neutral pH.

Take the organic layer for solvent recovery and organic mass to be used for the next stage.

Arrange 30 lit resin kettle on heating bath having stirrer, thermo pocket, condenser with water circulation.

Cool the mass slowly and filter.

Recover the methanol by distillation and recycle in next batch.

Dry the final product under vacuum at ambient temperature.

Charge polyphosphoric acid and P2O5 powder under stirring and heat the reaction mass and stir.

Add stage 3 at this temperature and heat the reaction mass up to reflux and stir till reaction completion.

After completion of reaction cool the reaction mass and add water.

After addition of water cool the reaction to ambient temperature

Filter the reaction mass at warm temperature and wash it with water.


109

29) TMP

Item Qty Item Qty

UOM KG UOM KG

Thiophenol 0.66

48% caustic lye 0.55

1-chloro-2-nitro

benzene0.95

TBAB 0.00

Water Lot-1 0.99

Water Lot-2 1.98

Conc. HCl (30%) 0.15

Reaction Mass 5.3

Water Lot-3 0.66

Wet Cake 1.39 4.55

St-1 (Wet Cake) 1.39

Acetic acid 0.07

Water Lot-4 6.93

Iron powder 1.18

Water Lot-4 1.39

Reaction Mass 10.9

Toluene Lot-1 2.08 7.0 Aq. ML 6.39

Main filtrate Org.

mass2.56

3.6 Solid waste 3.58

Toluene Lot-2 1.39

2.5641 1.11

Water Lot-5 1.39

Na2CO3 0.03 2.3 Aq. ML 2.31

Hyflo bed 0.20 Org. Layer (dry) 3.31

0.63 Solid waste 0.63

2-(Phenyl

sulfanyl)-aniline in

toluene

3.34

phenyl

chloroformate0.88

Na2CO3 0.70

Toluene lot - 3 1.00

Water Lot-6 1.40

Water Lot-7 1.00Aqueous ML send to

ETP

Reaction Mass 8.3 4.5 Aq. ML 4.5

Water Lot-8 1.00

Conc. HCl (30%) 0.01

Organic layer 3.793

1.01 Aq. ML 1.01

1.9

Bottom mass 1.692

polyphosphoric

acid (PPA)5.08

St-3 (Oily Mass) 1.69

P2O5 (anhydrous) 1.37

Water Lot-9 5.08

Reaction Mass 11.84 Main ML send to ETP

11.5 Aq. ML 11.5

Water Lot-10 5.08

Wet Cake(Crude) 0.34Aqueous ML send to

ETP

7.6

Methanol 4.00

4.0

wet cake 1.10

4.0 Residue 0.12

Aqueous ML send to

ETP


Organic Layer separation and

work up

Toluene-2 frm. w/c

washing

Reduction reaction and

filtration

Filtration and W/C washing

with toluene

Distillation

MATERIALS BALANCE - DBTZ

INPUT OUTPUT

Fe-Sludge to solid

waste

Condensation and Nitration

reaction


Aqueous ML send to

ETP

Main filtrate ML

(org. mass)

Rec. MeOH check.


Final Product

Purification and filtration

Filtration and washing

Aqueous ML send to

ETP

Aqueous ML send to

ETP

Hyflo solid waste

Organic layer work up and

filtration

Cyclisation reaction and work

up

1.00

Methanol ML to

Recovery.

Rec. Toluene check

analysis

30 Lit RBF


110

Trimethyl phenol (TMP) reaction scheme

Stage Preparation of Trimethyl phenol (TMP)

Trimethyl phenol (TMP) reaction scheme

Brief process

1 Charge catalyst in Vapour phase reactor

2 Prepaired solution of 2,3-Xylenol+Water+Methanol

3 Start heating of reactor to 350°C

4 Start dossing of above prepaired mixture at same rate through dossing pump

5 Collect output and submitted sample

6 Separate water from output and distilled methanol

7 Separate TMP through distillation

Item UOM Quantity Mole wt Mole Item UOM Quantity Mole wt Mole

2,3-Xylenol G 357 122.50 2.91

Methanol G 282 99.80 Reaction mass G 491

Water G 125 2,3-Xylenol W% 40.000

2,5-Xylenol W% 1.8

2,3,6-TMP W% 36

Methanol A% 5.2

Water G 70

Reaction mass G 491 Methanol G 100

Methanol A% 98

H2O % 70

Bottom mass G 375

2,3-Xylenol G 195

2,3,6-TMP G 165

2,5-Xylenol G 5

Residue G 10

OUTPUT

V.P. Reactor with 140 ml (100 g) Catalyst

Heat to 350°C

Addition at 140 ml/Hr (1 Bed volume),

Collect output and separate water layer

Distilled methanol + water

Vacuum distillation using SS pack column

INPUT STEP- Chlorination


111

30) Chlorophenesin

Project Name : Chlorophenesin

Process description

1 Ensure clean and dry 1 Lit 4N assambly.

2 Charge Epichlorohydrin(0.68 kg) and D.M water(3.0 kg) followed by catalytic amount of H2SO4 (6.0 g) addition slowly at room temperature.

3 Raise temperature to reflux using oil bath and maintain for 45-60 Min at same temperature.

4 Meanwhile In other clean 0.5 Lit 4N RBF charge 0.8 kg of p-Chlorophenol and 0.76 kg 48% NaOH solution then stir for 30 min at room temperature.

5 After maintaining at reflux temperature then cool the reaction mass to warm temperature.

6 To the reaction mass (Point 5.) add slowly pre-prepared p-Chlorophenol sodium salt solution within 30-45min at reflux temperature.

7 Maintain the reaction mass at reflux temperature for 3-4hr or ti l l completion on HPLC (p-Chlorophenol NMT 1.0 % Area).

8 Meanwhile maintain the pH 10-11.5 using 48% NaOH solution, if required.

9 After completion of reaction cool to room temperature and separate organic layer then discared the aqueous layer.

10 Organic layer charged in same RBF and add DM Water(2.0 kg) then adjust pH 6.5-7.0 using conc. HCl(30.0 g) at cold condition.

11 Stir for 45-60min at same temperature and fi ltered the solid crude wet cake.

12 Water and p-Chlorophenol removed by high vacuum distil lation (High vacuum) at high temperature.

13 The remaining bottom mass cool to room temperature and add toluene(2.5 L) under stirring.

14 Cool the mass upto chill ing condition and fi ltered followed by bed wash of chilled toluene (0.7 L).

15 Final solid product (1.0 kg) dry under vacuum(550-600 mmHg) at room temperature.


112

31) Methoxy MePPDA

p-chlorophenol 0.80

Sulphuric acid 0.01

Epichlorohydrin 0.68

48% NaOH 0.76

Water 3.00

Reaction Mass 5.2

Aqueous layer to the

ETP3.15

Aqueous ML to the ETP

Conc. HCl 0.03 2.3

Water 2.00

Org. Layer 1.85

Water and First cut send

to disposal

0.75

Pure org. cut 1.1

Toluene 3.20

3.2


purity & recycle

2.56

0.640

Drying vapour loss

0.1

Sr.No. MT/MT KLD

1 5.00 5.36


3 0.640 0.69

5 lit RBF With N2 ATM

Layer separation

Condensation

reaction

Crystalisation

High Vacuum Distillation

Precipitation and Filtration


5 lit RBF

Toluene filtrate ML send

to recovery

Org. layer 2.10

Description

Water Consumption

Residue

Bottom residue A/F

Toluene recovery

1.0

Final Product

W/C Drying


113

Project Name : 2-Mehoxy methyl para phenylene diamine

Stage I: Preparation of 6-Nitro-1,3-bezodioxane

Stage II : Preparation of 2-Methoxymethyl-4-nitrophenol

Stage III : Preparation of 2-Methoxymethyl-4-Nitroaniline

Stage IV : Preparation of 2-Methoxy methyl para phenylene diamine


114

Process description

Stage I: Preparation of 6-Nitro-1,3-bezodioxane

1

2 Charge water then add 4- Nitro phenol. Add 1,3,5-Trioxane

3

4 Heat reaction mass .

5 After completion of the reaction, cool the mixture.

6 Stirr the mixture and fi lter the reaction mass, wash with water.

7 For purification, Again arranged assembly with 4N,1L rbf with reflux condensor on oil bath.

8 Charge IPA and wet cake.

9 Heat the reaction mass.

10 Stop heating and cood the reaction mass.

11 Filter the solid and wash with IPA.

Stage II : Preparation of 2-Methoxymethyl-4-nitrophenol

1

2 Charge methanol and stage-01

3

4 Heat reaction mass. Mainatane for 2 hrs.

5 After completion of the reaction, reaction mass is quenched in D.M water.

6 Stirr the mixture.

7 Filter the reaction mass and wash with D.M water.

Stage III : Preparation of 2-Methoxymethyl-4-Nitroaniline

1

2 Charge stage-02, n-Propanol, K2CO3 and KI and 2-Chloroacetamide.

3 Heat to get reflux temp. Maintain for 3 hr.

4 After completion of reaction on TLC, Start addition of KOH solution

5 Maintain for 3-4 hrs.

6 Recover the n-propanol.

7 Add water and maintain for 30 min.

8 Cool and maintain for 1 hr.

9 Filter and wash with water. Wet wt of solid = 73.0 g

10 Arrange assembly with 4N 500 ml rbf,TP and condenser on oil bath.

11 Charge toluene and above wet cake.

12 Add charcoal 10% and maintain the temperature.

13 Filter the charcoal through hyflo and wash with toluene.

14 Cool it and fi lter to get material

Stage IV : Preparation of 2-Methoxy methyl para phenylene diamine

1 Charge stage 04, methanol and pd/C in autoclave.

2 Flush N2 and then H2

3 Apply gas pressure and heating.

4 Maintain the reaction mass ti l l completion of reaction.

5 After completion of reaction, Cool it to room temp.

6 Add charcoal and maintain for 1hr.

7 Filter the charcoal and distil lation of methanol.Followed by toluene stripping.

8 Add Toluene and heat, cool it to get product.

Clean and dry 3 l it RBF with reflux condenser on oil bath

Started addition of Cocn. H2SO4 ,


Started addition of Cocn. H2SO4 ,



115

32) 2- ACF

Project Name :2-Methoxy methyl para phenylene diamine 30 MT/M

Item Qty Item Quant

UOM Kg UOM Kg

water 20.12

4-Nitrophenol 2.01

1,3,5 Trioxane 1.03

H2SO4 8.85

Reaction Mass 32.01

27.48

4.53

2.2

2.33

Methanol 5.67

Sulphuric acid 1.49

Reaction Mass 9.36

5.67

Water 15.42 19.1

wt cake of solid 3.6

15.5

Vapour loss

2.15 1.5

Chloroacetamide 1.21

potassium Iodide 0.20

1- Propanol 13.83

Potassium carbonate 0.85

Potassium hydroxide 0.96 Reaction Mass 19.20

13.83

Water 20.15

Rxn mass 25.52

Wt cake of solid 1.6

23.92

Toluene 6.11

Activated carbon 0.16 Reaction mass 7.87

Toluene 2.03

Celite 0.01

0.17

Toluene 1.63

Wet cake 1.63

9.77 8.30

Vapour loss

Dry wt 1.45

0.2 1.47

methanol 14.50

H2 Gas 0.10

Pd/C Catalyst 0.07 Reaction mass 16.12

mehanol 2.90

Celide 0.01

0.08

Bottom mass 1.36 17.40

Toluene 1.09

wt of solid 1.2

1.09 0.93

Vapour loss

Dry wt 1

0.2 0.16

Sr.No. MT/MT KLD

1 55.69 59.67


3 1.629 1.75

4 0.25 0.26

Water Consumption

Residue

Solid waste

Filtrate ml Recovery of Toluene

Bottom mass residueDry material under vacuum

Cool and filter the solidFiltrate ml+wml

Description

Filtration of solid

Hot filtration

Dry material under vacuum

Celite filtration

Solid waste

Distillation of Methanol

Purification with toluene

Reduction

Filterate Ml+Wml

Recovery of Toluene

Bottom mass residue

Recovered solvent

Condensation and smiles

rearrangment

Stage-4 insitu stage-3

Purification

Solid waste

MATERIALS BALANCE

cool the reaction mass and

filter the product.

INPUT

Filtrate ml+wml

Distillation

Dry material in oven

Water quenching

Hydrolysis

Filtration of solid

Distillation of Methanol

Filter the solid

Recovery of

Methanol

Water quenching rxn mass

Dry material in oven

Recovered solvent

OUTPUT

Stage-1

Maintain the reaction mass.

Filterate Ml+Wml

for recycle

Stage -2

Vapour loss


116

Project : 2Acetyl Furan

Reaction scheme

Brief Lab Process

1 In dry reactor charge acetic anhydride & cool to 15-20°C

2 Add Acetic acid & Zinc chloride

3 Add Furan in 3 hr.

3 Heat to 70°C & 80 for 5 hr & 4 hr respectively

4 Cool the mass to 20-25°C

5 Add water & stir well.

6 Add Ethylene dichloride (EDC)

7 Separate Aq & EDC layer.

8 wash the EDC layer with Soda ash solution till pH 7

9 Recovered EDC & 2-Acetyl furan by distillation.


117

33) MTA

Project : 2Acetyl Furan 30 MT/MFLOW DIGRAM

Input Output

No Raw Material g Qty(g) No Raw Material Qty(g)

1 Furan g 276 1 Reaction mass 855

2 Acetic anhydride g 496 2 Loss 27

3 Acetic acid g 96

4 Zinc Chloride g 14

5 Reaction mass g 855 3 Organic layer 1384

6 Water g 1710 4 Aq. Layer 2176

7 EDC g 1050 5 Loss 55

10 Organic layer g 1384 9 Organic layer -3 1338

11 20% soda ash soln g 368 10 Aq. Layer 388

11 Loss 26

12 EDC layer -3 g 1338 12 2-Acetyl furan 300

13 13 EDC recovered 916

14 residue 93

15 Loss 29

Sr.No. MT/MT KLD

1 5.70 6.11


4 0.31 0.33

Water Consumption

Residue

Add soda solution till pH

7.0-7.5, separate the Org

& Aq. layer

Recoverd EDC & 2-Acetyl

furan by distillation

Process

addition of Furan in

reaction mixture &

maintain temperature

Work up addition of water

& EDC in reaction mass &

separate

Description


118

2-Methyl-3-Amino Benzotrifluoride (MTA) reaction scheme

Stage: 1 Nitration of 3,4-Dichloro-6-(trifluoromethyl)toluene

Stage: 2 Preparation of 2-Methyl-3-Aminobenzotrifluoride


119

2-Methyl-3-Amino Benzotrifluoride (MTA) Brief process

Process description

Stage: 1 Nitration of 3,4-Dichloro-6-(trifluoromethyl)toluene

1 Ensure clean and dry 1 Lit Kettle assembly

2 Charge sulphuric acid and 2-NO2-3,4-Dichloro-6-Trifluoromethyl-Tolueneand start stirring

3 Maintain the reaction mass at temperature

4 Start the nitric Acid addition at desired temperature

5 Maintain the reaction mass temperature

6 Give sample for GC analysis 3,4-Dichloro-6-Trifluoromethyl-Toluene should be less than 0.2%

7 After reaction completion perform layer separation at hot condition

8 Cool the spent acid layer at RT and perform filtration to remove traces of 2-NO2-3,4-Dichloro-6-Trifluoromethyl-Toluene

9 To top organic layer give water wash at temperature and perform hot layer separation.

10 Bottom organic layer and top aqueous layer .Separate out both layers

11 Water washing aq. Layer for ETP

12 Take organic layer for soda solution at hot temperature to remove acidity

13 Perform hot layer separation bottom layer organic and top aqueous layer. Send aqueous layer to ETP

14 To organic layer give water wash at hot temperature to remove excess alkalinity.

15 Bottom organic layer and top aqueous layer separate.

16 Take organic layer for Hydrogenation


1 Ensure clean and dry 2Lit Autoclave assembly.

2 Charge 2- No2-3,4-Dichloro-6-Trifluoromethyl toluene in methanol

3 Add sodium acetate and catalyst and flush the autoclave with nitrogen

4 Take hydrogen pressure and start stirring

5 Start heating up to desired temperature. Maintain temperature and pressure

6 After complete hydrogen absorption maintain it for 1 to 2 hrs

7 Cool the reaction mass at RT and vent hydrogen gas

8 Flush the autoclave with nitrogen gas

9 Remove the reaction mass from autoclave and perform filtration to remove catalyst

10 Separate out water from organic layer

11 Give organic layer sample for GC analysis


120

34) 2-NMTA

2-Methyl-3-Amino Benzotrifluoride (MTA) mass balance

Stage: 1 Nitration of 3,4-Dichloro-6-(trifluoromethyl)toluene 30 MT/M

H2SO4 852 Org. Layer 577

HNO3 148 Spent acid 1095 Hazardous Waste

Water 172

Org. Layer 577 Org. Layer 576

Water 100 Aq. Layer 101 Effluent

Org. Layer 576 Org. Layer 575

Soda soln. 100 Aq. Layer 101 Effluent

Org. Layer 575

Water 100

Aq. Layer 101 Effluent

Equivalent MTA 361.1


Methanol 550

Catalyst 5.8 Rxn. Mass 1073.8

Sodium acetate 172

Hydrogen 71

Rxn. Mass 1073.8 Main filtrate 878

Water 300 Water filtrate 490 Effluent

Recovered catalyst 5.8 Hazardous Waste

Main filtrate 878 Recovered Methanol 548

Bottom mass 330

Bottom mass 330 Org. Layer 174

NaOH 170 Aq. Layer 326 Effluent

Org. Layer 174 MTA 173

Water 150 Aq. Layer 150 Effluent

2-NO2-3,4-Dichloro-6-

Trifluoromethyl-Toluene275

2-NO2-3,4-Dichloro-6-

Trifluoromethyl-Toluene

MATERIALS BALANCE MTA

574

3,4-Dichloro-6-

trifluoromethyl toluene500

Hydrogenation

Methanol recovery

Caustic solution Washing

Filtration and water wash to wet cake

Nitration

Soda washing

Water Washing

Water Washing

Water Washing


121


CH3 COOHCH

3COOH

NO2CH3

COOH

O2N

CH3

COOH

NO2

m-Toluic acid 3-Methyl-2-nitrobenzoic acid

+

4-Nitro-3-methylbenzoic acid;

+

3-Methyl-6-nitrobenzoic acid

Conc.HNO3

Nitration at 10-15°C

1 Charge conc. HNO3 carefully to 4-neck flask, start stirring and cool to 10-15°C

2 Start addition of solid m-Toluic acid (MTA) pinch by pinch by maintainig temperature of reaction to 10-15°C

3 Complete addition of solid within 1-1.5 hr then keep post stiring for 30 min

4 Check inprocess sample for unreacted MTA.

5 Add chilled water within 2 hr slowly at 10-15°C

6 Filter solid through filter cloth and preserve filtrate mL

7 Wash wet solid with 2 x100 ml water and suck well using vacuum pump

8 Dry the solid at 80°C till moisture is < 1%


Consumption kg/kg

Raw material Unit Qty

1 m-Toluic acid kg 1.85

2 HNO3 98% kg 6.76

3 HNO3 70% kg 0.93

4 process water kg 11.20

5 lime 80% kg 7.87


122

30 MT/Month

Item UOM Quantity Density Volume Item UOM Quantity Density Volume

Conc. HNO3 ml 507 1.52 333.6

m-Toluic Acid g 139 1.2 115.8 Reaction mass (A / addition) g 626 1.37 456.9

HNO3 (70%) g 70 1.42 49.3 Wet 2-NMTA- Crop-1 (wet) g 85 0.72 118.1

Washing water g 278 1 278.0 Total acidic filtrate ml g 588 1.4 420.0

Washing ml g 278.5 1 278.5

Wet crop-1 (85 g)

Dry crop-1 g 78 0.73 106.8

Washing ml g 588 1 588.0

Fresh water g 562 1 562.0

Total acidic filtrate ml g 588 1.4 420.0

Wet crop-2 g 115 0.73 157.5

Aq. Filtrate ml g 1225 1.15 1065.2

Wet crop-2 (115 g)

Dry crop-2 g 81.5 0.72 113.2

Sr.No. MT/MT KLD

1 10.31 11.04


Dry Crop-1

Description

Water Consumption

Quenching, At 15-20°C

OUTPUT

Drying

Quenching, Total water- 840 g

Filtration

Filtration

Drying

Dry Crop-2

Project:- 4-Chloro-6-methylanthranilimide

DRDC, 20-2-18

1-Lit 4-Neck Flask

LABORATORY PROCESS: 2-NMTA

INPUT STEP

Documents

Application for Prior Environmental Clearance Pre-Feasibility Report · 2019-05-09 · Application for Prior Environmental Clearance Pre-Feasibility Report For Proposed Expansion