Application for Prior Environmental Clearance Pre ...environmentclearance.nic.in/writereaddata/Online/TOR/09_Jan_2019... · Prefeasibility Report Deepak Nitrite Limited, MIDC Roha

Prefeasibility Report Deepak Nitrite Limited, MIDC Roha

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Application for Prior Environmental Clearance

Pre-Feasibility Report

For

Proposed Establishment of Pesticide specific intermediates & Synthetic Organic Chemical

Manufacturing

Category 5 (b) and 5(f)

Prepared By

M/s Deepak Nitrite Limited

Plot No 53A, MIDC Roha, 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 ................................................................................................................................. 7 EXPORT POSSIBILITY ................................................................................................................................................................ 7 DOMESTIC / EXPORT MARKET ................................................................................................................................................ 7 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 ............................................................................................................... 12

Project layout is at Annexure II ......................................................................................................................... 12 Product chemistry, Process description, Process block diagram and material required is

mentioned at Annexure IV. ....................................................................................................................................................... 12 RAW MATERIAL REQUIRED ................................................................................................................................................... 12

Details of Machineries and Utilities required ............................................................................................... 12 Solvent Management plan ................................................................................................................................... 15

WATER, ENERGY / POWER AVAILABILITY AND SOURCE ................................................................................................. 16 Water ........................................................................................................................................................................... 16 Power ........................................................................................................................................................................... 17 Fuel ................................................................................................................................................................................ 17 Manpower .................................................................................................................................................................. 17

WASTE GENERATION, MANAGEMENT AND DISPOSAL ...................................................................................................... 18 Water Pollution ........................................................................................................................................................ 18 Solid Waste Management .................................................................................................................................... 21 Air Pollution .............................................................................................................................................................. 22

SCHEMATIC OF EIA PURPOSE .............................................................................................................................................. 24

4 SITE ANALYSIS ......................................................................................................................................................... 25

CONNECTIVITY ........................................................................................................................................................................ 25 LAND FORM, LAND USE AND LAND OWNERSHIP ................................................................................................................ 25 TOPOGRAPHY (ALONG WITH MAP) ...................................................................................................................................... 25 EXISTING LAND USE PATTERN .............................................................................................................................................. 25 EXISTING INFRASTRUCTURE ................................................................................................................................................. 25 SOIL CLASSIFICATION ............................................................................................................................................................. 25 CLIMATE DATA FROM SECONDARY SOURCES ..................................................................................................................... 26 SOCIAL INFRASTRUCTURE AVAILABLE ................................................................................................................................ 26

5 PLANNING BRIEF ..................................................................................................................................................... 27

PLANNING CONCEPT .............................................................................................................................................................. 27 POPULATION PROJECTION .................................................................................................................................................... 27 LAND USE PLANNING ............................................................................................................................................................. 27 ASSESSMENT OF INFRASTRUCTURE DEMAND (PHYSICAL AND SOCIAL) ....................................................................... 27 AMENITIES / FACILITIES....................................................................................................................................................... 27

6 PROPOSED INFRASTRUCTURE ........................................................................................................................... 28

INDUSTRIAL AREA (PROCESSING AREA) ............................................................................................................................ 28 RESIDENTIAL AREA (NON PROCESSING AREA) .................................................................................................................. 28


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GREEN BELT ........................................................................................................................................................................... 28 SOCIAL INFRASTRUCTURE..................................................................................................................................................... 28 CONNECTIVITY ........................................................................................................................................................................ 28 DRINKING WATER MANAGEMENT ........................................................................................................................................ 28 SEWAGE SYSTEM .................................................................................................................................................................... 28 INDUSTRIAL WASTE MANAGEMENT..................................................................................................................................... 28 SOLID WASTE MANAGEMENT................................................................................................................................................ 28

POWER REQUIREMENT AND SUPPLY / SOURCE ................................................................................................................. 28

7 REHABILITATION & RESETTLEMENT PLAN ................................................................................................. 29

8 PROJECT SCHEDULE AND COST ESTIMATES ................................................................................................. 30

LIKELY DATE OF START OF CONSTRUCTION AND LIKELY DATE OF COMPLETION ......................................................... 30 ESTIMATED PROJECT COST ................................................................................................................................................... 30

9 ANALYSIS OF THE PROPOSAL (FINAL RECOMMENDATION) ................................................................... 31

List of Annexures Annexure No Description I Plant location / Google image of plant site II Layout plant of the proposed establishment 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 project is for manufacture of Pesticide specific intermediates & synthetic organic chemicals at (vacant plot of company) plot no 53 A, 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 Proposed Project location Plot No. 53A, Roha Industrial area, Tal Roha, Dist.

Raigad. 4 Total land area of the plot 20,224 sq m 5 Proposed built up area 30,000 sq m 6 Name of the project Proposed manufacture of Pesticide specific

intermediates & Synthetic Organic chemicals 7 Estimated project cost Rs. 150 Crores 8 Products Refer section 3.4 9 Raw material Refer section 3.6 10 Water Total water requirement will be 1756 cmd.

It will be supplied by MIDC. 11 Power Power requirement for the project will be 5000

KVA, which will be procured from MSEDCL.


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It is proposed to install 3 No of DG sets each of 1000 KVA for emergency power requirement.

12 Manpower Proposed manpower requirement for operational phase will be 500 Nos. ( Permanent 215 + Contract 285 = Total 500)

Pollution Potential and mitigation measures 13 Water Pollution Refer section 3.9 14 Air pollution Refer section 3.9

16 Hazardous waste Refer section 3.9 17 Green belt development The unit will develop 6698 sq m green belt within

plot.


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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 and designation Qualification Experience, Years

1 Mr. Deepak C. Mehta (Chairman & Managing Director)

B.Sc 40

2 Mr. Umesh Asaikar (Chief Executive Officer)

B.E., Mechanical Engineering Masters in Management Science

39

3 Mr. Ajay C. Mehta (Managing Director)

M.S., Chemical Engineering 34

4 Mr. Maulik D. Mehta (Whole Time Director)

B.B.A & Masters in Industrial and Organizational Psychology

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5 Ms. Nimesh Kampani (Independent Director)

Chartered Accountant 40

6 Mr. Sudhin Choksey (Independent Director)

Chartered Accountant 42

7 Mr. Sudhir Mankad (Independent Director)

Masters’ degree in History 40

8 Dr. R. H. Rupp (Independent Director)

Masters’ degree in History 38

9 Dr. Swaminathan Sivaram (Independent Director)

PhD in Chemistry 41

10 Dr. Indira J. Parikh (Independent Director)

PhD in Chemistry 30

11 Mr. S. K. Anand (Independent Director)

B.E. Chemical Engineering 46

Regulatory Framework The proposed establishment 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), 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.


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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 green field 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 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 also 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.

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.

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 this 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.


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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 establishing unit for manufacture of Pesticide specific intermediates &

synthetic organic chemicals. There is no interlinking of any project.

Location

The proposed project 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, 180 25’ 47.62”N and 730 9’ 24.79”E at elevation above Mean sea level of 12 meters.

Geographical plant site coordinates are as below: Direction Latitude Longitude

North east corner 180 25’ 48.67”N 730 9’ 28.71”E

North west corner 180 25’ 50.70”N 730 9’ 23.46”E


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South east corner 180 25’ 44.48”N 730 9’ 26.92”E

South west corner 180 25’ 46.53”N 730 9’ 21.72”E

Details of Alternative sites

No alternate site examined as this is vacant plot owned by Deepak Nitrite within established MIDC area.

Size or magnitude of operation

The unit proposes to establish manufacturing facility of following Pesticide specific

intermediates & synthetic organic chemicals. Proposed products and quantities,

Product No

Product CAS No. Quantity, TPA

1. ADENINE (6- Amino Purine) 73-24-5 2000 2. 3-NAP (3 Nitro acetophenone) 121-89-1

3. 3-AAP (3 Amino acetophenone) 99-03-6

4. 3-HAP (3 Hydroxy acetophenone) 121-71-1

5. 2,3-Xylenol 526-75-0

6. 2,4-Xylenol 105-67-9

7. 2,5-Xylenol 95-87-4

8. Phenyl Hydrazine 100-63-0

9. Triazinone 33509-43-2 4500 10. Thiocarbohydrazide (TCH) 2231-57-4

11. 3-ABTF ( 3 Amino benzotrifluoride) 98-16-8 2000 12. TFMAP (3-Triflouromethyl Acetophenone) 349-76-8

13. SMIA (2-Furanacetic acid, α-(methoxyimino)-, ammonium salt)

97148-39-5 600

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

3159-07-7 2000 15. Guanine 73-40-5

16. Aciclovir 59277-89-3

17. PMPA (TENOFOVIR) ((R)-9-[2-Phosphonomethoxy) propyl]adenine)

107021-12-5

18. Omeprazole Chloro Intermediate (2-Chloromethyl-3,5-Dimethyl-4-methoxy pyridine hydrochloride)

86604-75-3

19. Omeprazole Nitro Intermediate (2,3,5-trimethyl-4-nitropyridine N-oxide)

86604-79-7

20. 7-ETP (7-Ethyl tryptophol)Etodolac intermediate

41340-36-7

21. S-Alcohol (Duloxetine Intermediate) 132335-44-5

22. 2-Methyl-3-Amino Benzotrifluoride (MTA) 54396-44-0

23. Pilot Plant products (Synthetic Organic Chemicals)

Not applicable

240


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Product No

Product CAS No. Quantity, TPA

24. Distillation of crude Chemicals/solvents such as Nitroxylenes, Nitrocumens, crude Toluene, Crude benzotrifluoride, Crude Methanol etc, Spent acid recovery, Formamide recovery

Not applicable

1200

Total 12540

NOTE: Some products from above list are used for Agro intermediates which falls under Activity 5(b) of EIA notification, 2006. There are no by products generated. End use application of products are as below Products Uses/ Applications:

Sr. No.

Name of Products End Use of Products

1 6-Aminopurine (Adenine) Diagnostic aid; Food additive 2 3-Nitro Acetophenone (3NAP) Pharma and Agro Intermediate 3 3-Amino Acetophenone (3AAP) Pharma and Agro Intermediate

4 3-Hydroxy Acetophenone (3HAP) Pharma and Agro Intermediate 5 2,3-Xylenol Pharma and Agro Intermediate 6 2,4-Xylenol Pharma Intermediate 7 2,5-Xylenol Pharma and Agro Intermediate

8 Phenyl Hydrazine Base Pharma and Agro Intermediate 9 1,2,4 Triazinone (Metribuzin

Intermediate) Agro Intermediate

10 Dichloropicolin Agro Intermediate 11 Thiocarbohydrazide (TCH) Agro Intermediate 12 5-amino-3-cyano-1(2,6-dichloro-4-

trifluromethylphenyl) pyrazole [Fipronil Intermediate]

Agro Intermediate

13 Benzotrifluride (BTF) Pharma and Agro Intermediate 14 3-Amino Benzotrifluride (3-ABTF) Pharma and Agro Intermediate 15 3-(Trifluoromethyl)Acetophenone

(TFMAP) Agro Intermediate

16 SMIA Pharma Intermediate

17 Dibenzo[b,f][1,4]thiazepine-11(10H)- one (DBTZ) [Quetiapine Intermediate]

Pharma Intermediate

18 Guanine Pharma Intermediate 19 Aciclovir/acyclovir Useful as anti-retro virus drug. 20 (R)-9-[2-Phosphonomethoxy)

propyl]adenine (Tenofovir) PMPA Intermediate for Tenofovir, an anti-retroviral drug used for treating HIV/AIDS.

21 2-Chloromethyl-3,5-Dimethyl-4- methoxy pyridine hydrochloride (Omeprazole Chloro Int.)

Pharma Intermediate


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22 2,3,5-trimethyl-4-nitropyridine N-oxide (Omeprazole Nitro Int.)

Pharma Intermediate

23 3-Ethyl Tryptophol (Etodolac Intermediate)

Pharma Intermediate

24 S-Alcohol (Duloxetine Intermediate) Pharma Intermediate 25 2-Methyl-3-Amino Benzotrifluoride

(MTA) Pharma Intermediate

26 3-Hydroxy benzotrifluoride Pharma and Agro Intermediate

Project description with Project details

Project layout is at Annexure II

Product chemistry, Process description, 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 suppliers’ 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


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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.

Details of Proposed Equipment and Machineries Sr. No

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

1 Reactors Glass lined 18 5 KL, 6.3 KL, 8 KL

2 Reactors MS 12 3 KL, 8 KL, 10 KL 3 Reactors HDPE 2 3 KL, 5 KL 4 Reactors SS 28 1 KL, 3 KL, 8 KL, 18 KL 5 Distillation set SS/MS 8 8 KL, 12 KL 6 Absorption Column SS/MS 6 800 mm, 1000 mm dia 7 Crystallizer SS/MS 8 12 KL, 18 KL, 20 KL 8 Dryers SS/MS 18 200 Kg, 400 kg 9 Centrifuge SS/MS 12 24", 36"

10 Sparkler filter SS/MS 12 2 KL, 3 KL 11 Nutsche Filter SS/MS 9 6 KL, 8 KL

12 Condensers SS/MS 46 5 m2, 8 m2, 15 m2, 20

m2, 60 m2 13 Chillers -- 5 1000TR

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

1,500 CFM 15. Cooling Tower -- 1 3000TR 16. Air compressor -- 1 17. TFH -- 1 6 Lacs. Kcal/hr

BULK LIQUID STORAGE TANK DETAILS Detailing of Storage tanks along with their required capacities is tabulated below:


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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 for offsite distillation to 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:


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Resource optimization

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

Water, Energy / Power availability and source

Water

Total amount of required process water is tabulated below:


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(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 0 40 40 2 Industrial process 0 1086 1086

3.1 Industrial cooling 0 300 300 3.2 Boiler 0 300 300 4 Gardening 0 30 30 Total 0 1756 1756

Water will be sourced from MIDC.

Power

Total power requirement is 5000 KVA and will be sourced from MSEDCL.

Fuel

3 no of D. G. set having capacities 1000 KVA (3 no) are required to meet energy requirement. Apart from it, one boiler is required whose details are tabulated below:

Sr. No Item Fuel Quantity Required at full load

1 Boiler (16 TPH) Coal 2667 kg/hr (64 TPD Dry basis )

Manpower

Expected manpower requirement for operational phase of the project will be

1 2 3 A B C D=A+B+C E=3XA F=3XB G=3XC H=E+F+G

Qty Max. Qty Max. Qty Max. QtyFresh

water

From

processWith RM

Total water

consumptionFresh water

From

processWith RM

Total water

consumption

Water

requirement

(MT/Yr) (MT/Yr) (MT/M) (MT/Day) MT/MT MT/MT MT/MT MT/MT MT/day MT/day MT/day MT/day MT/Day

ADENINE 2000 166.67 5.95 62.53 1.05 1.45 65.04 372.22 6.24 8.66 387.12

3-NAP 2000 166.67 5.95 10.32 0.15 0.34 10.81 61.41 0.88 2.04 64.33

3-AAP 2000 166.67 5.95 5.56 0.30 1.11 6.97 33.07 1.80 6.61 41.48

3-HAP 2000 166.67 5.95 4.90 0.17 0.03 5.09 29.14 0.98 0.15 30.27

2,3-Xylenol 2000 166.67 5.95 8.19 0.17 0.00 8.36 48.78 0.99 0.00 49.77

2,4-Xylenol 2000 166.67 5.95 7.33 0.18 0.00 7.51 43.62 1.06 0.00 44.68

2,5-Xylenol 2000 166.67 5.95 9.75 0.35 0.00 10.10 58.05 2.08 0.00 60.13

Phenyl Hydrazine 2000 166.67 5.95 10.50 0.41 6.73 17.64 62.50 2.44 40.06 105.00

Triazinone 4500 375.00 13.39 14.63 0.22 6.85 21.71 195.99 2.94 91.79 290.72

Thiocarbohydrazide (TCH) 4500 375.00 13.39 1.11 0.00 0.52 1.63 14.88 0.00 6.99 21.88

3-ABTF 2000 166.67 5.95 0.32 0.41 0.78 1.51 1.91 2.44 4.65 9.00

TFMAP 2000 166.67 5.95 12.81 0.00 0.00 12.81 76.25 0.00 0.00 76.25

SMIA 600 600 50.00 1.79 7.84 0.23 11.00 19.07 14.00 0.41 19.64 34.05 34.05

DBTZ (Quetiapine Int.) 2000 166.67 5.95 27.27 0.77 0.69 28.73 162.32 4.58 4.08 170.98

Guanine 2000 166.67 5.95 9.71 0.02 8.93 18.66 57.80 0.12 53.15 111.07

Aciclovir 2000 166.67 5.95 44.00 0.20 5.14 49.34 261.90 1.19 30.61 293.70

PMPA (TENOFOVIR) 2000 166.67 5.95 12.00 0.20 0.65 12.85 71.43 1.19 3.87 76.49

Omeprazole Chloro Int. 2000 166.67 5.95 33.75 1.50 6.80 42.05 200.89 8.93 40.48 250.30

Omeprazole Nitro Int. 2000 166.67 5.95 6.47 0.87 0.53 7.87 38.51 5.18 3.13 46.82

7-ETP (Etodolac int.) 2000 166.67 5.95 2.43 0.10 1.90 4.43 14.46 0.60 11.31 26.37

S-Alcohol (Duloxetine Intermediate) 2000 166.67 5.95 1.00 0.03 1.54 2.57 5.95 0.17 9.16 15.28

MTA 2000 166.67 5.95 4.75 0.44 1.38 6.57 28.28 2.60 8.24 39.12

Synthetic Organic Chemicals 240 240 20.00 0.71 1.00 0.00 0.00 1.00 0.71 0.00 0.00 0.71 0.71Distillation of crude

Chemicals/solvents such as

Nitroxylenes , Nitrocumens , crude

Toluene , Crude benzotrifluoride ,

Crude Methanol etc ,

Spent acid recovery , Formamide

1200 100.00 3.57 0.00 0.00 1.00 1.00 0.00 0.00 3.57 3.57 3.57

1086

Product

2000

2000.00

293.70

387.12

290.72

76.25

Total water consumption (KL/ day)

4500

2000


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Permanent, No Contracts, No Total , No

215 285 500

Waste generation, Management and disposal

Water Pollution

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

(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 0 30

30

It will be treated in independent STP plant. Treated water will be used for gardening

2 Trade effluent

S.N. Qty Qty QtyEffluent

Quantity

Effluent

Gen.

Max Effluent

product

(MT/Yr) (MT/M) (MT/day) MT/MT MT/Day MT/Day

1 ADENINE 2000 167 6.0 37.4 223

2 3-NAP 2000 167 6.0 2.55 15

3 3-AAP 2000 167 6.0 7.77 46

4 3-HAP 2000 167 6.0 2.30 14

5 2,3-Xylenol 2000 167 6.0 13.57 81

6 2,4-Xylenol 2000 167 6.0 9.34 56

7 2,5-Xylenol 2000 167 6.0 4.21 25

8 Phenyl Hydrazine 2000 167 6.0 5.00 30

9 Triazinone 4500 375 13.4 15.85 212

11 Thiocarbohydrazide (TCH) 4500 375 13.4 2.70 36

15 3-ABTF 2000 167 6.0 1.20 7

16 TFMAP 2000 167 6.0 10.26 61

17 SMIA 600 600 50 1.8 16.70 30 30

18 DBTZ (Quetiapine Int.) 2000 167 6.0 40.36 240

19 Guanine 2000 167 6.0 38.64 230

20 Aciclovir 2000 167 6.0 33.50 199

21 PMPA (TENOFOVIR) 2000 167 6.0 46.80 279

22 Omeprazole Chloro Int. 2000 167 6.0 24.94 148

23 Omeprazole Nitro Int. 2000 167 6.0 10.45 62

24 7-ETP (Etodolac int.) 2000 167 6.0 22.62 135

25 S-Alcohol (Duloxetine Intermediate) 2000 167 6.0 16.80 100

26 MTA 2000 167 6.0 0.84 5

Synthetic Organic Chemicals 240 240 20 0.7 10 7 7.14

812

2000

Product

Comperative Statement of effluent load

Total effluent generation (kL/day)

223

212

61

279

4500

2000

1000


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2.1 From Process 0 812

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

2.2 From utilities 0 125 125 Total 0 967 967

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 0 40 40 0 10 10 0 30 30 Industrial

process 0 1086 1086 0 274 274 0 812 812

Cooling tower/ Boiler

0 600 600 0 475 475 0 125 125

Gardening 0 30 30 0 30 30 0 0 0 Total 0 1756 1756 0 789 789 0 967 967

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. Maximum trade effluent generation from the proposed facility (in worst case scenario) will be 967 cmd and will be treated in proposed MEE and ETP (capacity 1000 cmd). Treatment Scheme for Trade Effluent The total effluent generation from proposed project will be 967 cmd. Effluent generation from manufacturing process 812 cmd, utilities (Boiler and Cooling Tower) 125 cmd and domestic 30 cmd. Low concentrated effluent 125 cmd from utilities (boiler and cooling tower) and manufacturing processes 533 cmd will be directly sent to ETP for further treatment. High concentrated effluent generated from manufacturing process 279 cmd will be collected and treated in proposed MEE. Treated effluent in MEE will be further sent to ETP. The treated water will be sent to CETP. Design Details and Performance projections of Proposed MEE are tabulated below:

Sr. No.

Waste- water Stream

Unit High COD/TDS Process to

Stripper

Design Consideration

(Stripper)

Stripper Outlet (Feed

to MEE)

Design Consideration

(MEE)

1 Hydraulic Flow Rate

KLD 279 300 270 300

2 pH - 6.0-8.0 6.0-8.0 6.0-7.0 6.0-8.0

3 TDS (max.) mg/L 18,000 20,000 12,000 15,000

4 COD (max.) mg/L 59,000 70,000 15,500 20,000


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5 BOD (max.) mg/L 13,500 14,000 5,000 5,500

ETP treatment scheme-

1. Primary Treatment

The system will be designed to treat 1000 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 1000 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 1000 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 Collection in the final Collection tank from where it will be discharge to proposed upgraded CETP. 4. 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 pumped to the decanter for dewatering. The solid cake from the decanter will be sent for disposal to Hazardous waste disposal site. The filtrate from the Filter press will be drained to the collection tank. Design details and Performance Projection of ETP are tabulated below:


21

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 1500-2000 175-215 <250 5 TSS mg/L 350-450 35-75 <100 6 TDS mg/L 3000 1800 <2100 7 Oil and

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

Solid Waste Management

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:

Type of waste Source Cate- gory

Quantity of Waste Generated per

Annum

Method of Disposal

MEE Salt MEE Sch -1 35.3

10,800 MT To CHWTSDF for landfill Hyflow Mfg. of Prod.

No.14 127.8 MT

Iron Sludge Mfg. of Prod. No.14

Sch-1 35.3

766.8 MT To CHWTSDF for landfill

Process waste (Organic)

Mfg. of Prod. No. 3, 21 and 23

Sch - 1 35.3

799.3 MT

To CHWTSDF for incineration OR Co- Processing

Charcoal Sludge Mfg. of Prod. No. 1,15

Sch – 1 36.2

174.4 MT

Residue Mfg. of various Products.

Sch - 1 36.2

654.3 MT

Spent Catalyst Mfg. of various existing and

proposed products

Sch - 1 19.2

63.8 MT Sell / Regeneration & Re-use

Waste /Residue Containing Oil

Plant & Machineries

Sch - 1 33.2

1.04 KL To CHWTSDF for landfill

Used /Spent Oil Sch - 1 5.1

2.8 MT selling to registered recyclers OR Reused as Lubricant within


22

premises Empty barrels/

containers/liners contaminated with

hazardous chemicals /wastes

Raw Material Storage & Handling

Sch –I 33.1

100 MT selling to scrap vendors

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 are process gas generation in the form of NOx, NH3, H2S/SO2, HCl. Unit will

provide adequate scrubbing system (water / acid / alkali scrubbers) to control emission

of process gas into atmosphere. Details of proposed process gas stack are given in

following Table. Schematic diagram of air pollution control measures are given in

subsequent figure.

Details of proposed process gas stack: Sr. No.

Stack Attached to Height & Dia. (m)

Pollutant APCM Management of Output

1 Reactor of Adenine 10 & 0.15

NH3 < 175 mg/NM3

Water Scrubber NH3 Solution - Sell to authorized end-

users 2 Reactor of Thio

carbohydrazide 10 & 0.15

H2S < 45 mg/NM3

Caustic Scrubber NaHS Solution – Sell to authorized

end- users

3 Reactor of SMIA 31 & 0.45

NOx < 3 kg/ton in

HNO3

NOx absorption tower with NaOH as

Scrubbing media. Caustic absorber

NaHS Solution – Sell to authorized

end- users

(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


23

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

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.


24

Release from sampling lines • Closed loop system is used.

Schematic of EIA Purpose

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

-


25

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).

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 is vacant at present and is for industrial use.

Existing infrastructure

There is no infrastructure at plot site. The Plot is located in well-developed notified MIDC area.

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.

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.


26

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 infrastructure such as schools, Hospitals, market place and other amenities are available. Transport facilities by rail and road are available.


27

5 PLANNING BRIEF

Planning Concept

The plot is in well-established MIDC Roha Industrial area.

Purified Water supply from MIDC, Road facility with illumination, Infrastructure facilities

available in the established MIDC.

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.

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.


28

6 P RO PO SED IN F RASTRUCT URE

Industrial Area (Processing area)

Deepak Nitrite proposed to establish Pesticide specific intermediates & synthetic organic chemicals manufacturing unit at its vacant plot within MIDC.

Residential area (non processing area)

No Residential area has been proposed within the plant site.

Green Belt

Green belt has been planned along the boundary of the plot. And will be maintained as per guidelines.

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.

Industrial waste management

Refer 3.9 above

Solid waste management

Refer 3.9 above

Power requirement and supply / source

Power requirement is 5000 KVA which shall be sourced from MSEDCL.


29

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

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


30

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,

No Description Estimated investment, Rs. Crores

1 Land and site development 4 2 Buildings 30 3 Plant and Machineries 96 4 Environmental protection measures 10 5 Others 10 Total 150


31

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.


32

ANNEXURE I Plant location / Google image of plant site Site with 1 km radius area

Site with 10 km radius area


33

ANNEXURE II

Layout plant of the proposed establishment with area statement

AREA STATEMENT

Description Area in sq m

Total Plot area (53A) 20,224

Built up area 9043

Roads 2114

Green belt within Plot (33.12%) 6698

Parking area (10.34%) 2,114


34

ANNEXURE III Proposed Water Balance

Proposed ETP flow diagram

WATER BALANCE

Domestic Gardening

Total water requirement: 1756(F – 1726, R – 30)

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

3010

30

1086 600 0

Effluent Treatment Plant

812

125

915

Low volatiles form stripper(Recycle/Reuse/Disposal)

9 MEE Salts to CHWTSDF

13

Treated waste water

to CETP

274

475

Stripper

MEE

279533

270 257


35

ANNEXURE IV Product details Process Reactions and Process description


36

1) Product - 6-Aminopurine (Adenine) Input Raw Materials:

No.

Name of Raw Material

Consumption (MT/Month)

1 Aniline 77.7

2 H2SO4 123

3 Sodium nitrite 120.6

4 Malononitrile 47.2

5 NaOH 146.8

6 NH3 11.9

7 Formamide 142.9

8 Hydrogen gas 3

9 Catalyst 1

10 Charcoal 15.9 Reaction:

Process block diagram

Stage: 1 Preparation of Phenylazomalononitrile

Stage: 2 Preparation of 6-Aminopurine(Adenine)


37


38


39

Process description: Stage 1 1. Charge water and start stirring. Add slowly sulphuric acid. 2. Cool mass to desired temp. Addition of aniline and NaNO2 by maintaining temperature. Add water and dissolved Malononitrile with heating and cool it followed by addition of Malononitrile solution in diazo mass maintaining temperature. 3. Add sodium hydroxide. 4. Charge water for wet cake washing and add wet cake under stirring Heat mass for hot filtration. 5. Dry wet cake at desired temperature. 6. Use dry Phenyl azomalononitrile for second stage. Stage 2 1 .Charge formamide, start stirring and cool. 2. Start ammonia purging in formamide to prepare solution Addition of sodium hydroxide. Charge ammonical formamide solution and add Phenyl azomalononitrile . 3. Add Catalyst to reaction mass. 4. Flush autoclave with Nitrogen gas then take Hydrogen pressure. 5. Filter the catalyst Transfer filtrate for Formamide recovery under vacuum. 6. Recover first cut of formamide containing moisture and then main formamide Fraction. Apply Hot filtration to remove impurities and add charcoal and stir and filter. 7. Get dry final product.


40

2) Product - 3 Nitro Acetophenone (3 NAP) Input Raw Materials:

No. Name of Raw Material Consumption (MT/Month)

1 Aceto phenone 25.25

2 98% H2SO4 140

3 70% HNO3 20

4 Methanol 3.75

5 Na2CO3 0.5

6 EDC 4.5

7 Dry ice 214

8 Water 265

Reaction:


41

Process block diagram: (All quantities are in kg)


42

Process description:

1. Charge 98% H2SO4 and cool it.

2. Start addition of Acetophenone within 1 to 1.5 hr by maintaining low temperature.

Further cool reaction mass to under stirring

3. Start addition of previously prepared mix acid in Acetophenone + H2SO4 reaction mass 4. Then submit wet solid for HPLC analysis, which shows Acetophenone less than 1.0%, if not

continued stirring. 5. After completion of reaction, quench nitrated mass in ice cold water under stirring.

Filter solid through PP filter cloth.

6. Wash crude wet solid of 3-NAP in equivalent wt of water at desired temperature.

7. Filter solid through PP filter cloth and suck well under vacuum

Wash wet solid by bicarbonate.

8. Filter solid through filter cloth and suck dry under vacuum.

9. Unload wet solid and add Methanol, then start stirring and raise temperature to reflux.

10. Keep reflux to clear solution of mass observed, then cool mass slowly under stirring.

11. Filter solid under vacuum , suck well and unload wet solid

12. Dry unloaded wet solid in air dryer.

13. Submit dry 3-NAP sample for HPLC analysis as per specification


43

3) Product - 3-Amino Aceto Phenone (3AAP) Input Raw Materials:


1 3-Nitro Acetophenone 24.16

3 Acetic Acid 1.17

4 Water 108.67

5 Iron powder 25.33

7 10% NaHCO3 (100% basis) 2.33

9 Toluene 10

10 Hyflo 6

Reaction:


44



1. Charge water and add Acetic acid to adjust pH. Heat the mixture up to high temp. 2. Charge iron powder under stirring. Raise temperature.

3. Slowly add 3-NAP in lots simultaneously

4. Adjust pH with 10 % sodium bicarbonate soln.

5. Heat upto high temperature. Filter through hyflo and wash the bed with toluene & water mixture. Then cool it up to room temperature then to below room temperature.

6. Maintain 1 hour and centrifuge; wash cake with chilled water.


45

4) Product - 3 Hydroxy Aceto Phenone (3-HAP) Input Raw Materials:


1 Conc. H2SO4, kg 10.83

2 DM water, lit 23.33

3 3-AAP, kg 10.83

4 NaNO2 5

5 Water 0.91

6 MIBK 104.16

7 Sat. NaCl soln 10.83

Reaction:


46



47


1. Charge conc. sulphuric acid under stirring to D.M. water then Cool this mixture.

2. Charge 3-AAP. Cool again and add a soln of sodium nitrite in water, slowly. Maintain temperature for 30 hours.

3. Add this reaction mass slowly to a mixture of MIBK and water and stir it for 2 hrs.

Separate the layers. Stir the MIBK layer with saturated sodium chloride solution and keep it for settling.

4. Separate MIBK layer, concentrate it, chill it ,

5. Centrifuge the crystallized 3-HAP, and dry it.


48

5) Product - 2,3 Xylenol Input Raw Materials:

No. Name of Raw Material Consumption (MT/ Month)

1 2,3-Xylidine 150

2 Sulphuric Acid 19.8

3 NO gas 42.8

4 NO2 gas 65.6

5 Toluene 32.2

6 Urea 6.2

7 Water 1119.8

Reactions:


49



50


1. Charge water H2SO4. ( Sulphuric acid 35%) / (Aq.spend acid recycle)

2. Add slowly 2,3-Xylidine. Exothermic reaction occurs, so cool this reaction mixture.

3. Slowly add the mixture of nitric oxide (NO) and (NO2) nitrogen dioxide in desired proportion.

4. Stir the reaction mass the and store this Diazo mass at low temperature.

5. Test starch iodide paper test Excess Nox should kill with Urea/sulfamic acid (Solution A)

6. Charge 34% Sulphuric acid solution/ Aq.effluent recycle ,Water & toluene and stir

7. Add slowly solution A (diazo mass) under maintained temperature and stir it further. 8. Separate out bottom aqueous layer, wash it with toluene and aqueous spend layer to be

recycled for next batch .

9. Mix both organic layer and wash with water and use directly for next step.

10. Take Organic layer for toluene recovery

11. Recover toluene at atmospheric pressure 12. Take crude conc. 2,3-Xylenol mass for distillation under vacuum and collect fraction of 2,3

Xylenol.


51

6) Product - 2,4 Xylenol Input raw Materials:


1 2,4-Xylidine 53.4

2 Sulfuric acid 65.7

3 NaNO2 32.8

4 Toluene 9.8

5 Tri ethanolamine 0.4

6 Soda Ash 1.1

Reaction


52

Process block diagram: (All quantities are in Kg)


53


1. Charge water and 2,4-Xylidine then slowly add sulphuric acid and toluene followed by heating this mixture

2. Prepare solution of sodium nitrite in water

3. Add slowly sodium nitrite solution into above reaction mass within maintained temperature

4. Further maintain the reaction mass. Check for unreacted 2,4-Xylidine.

5. Cool the reaction mass to RT and allow settling

6. Separate out bottom aqueous layer and wash it with toluene

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

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

9. Distill out the toluene

10. Cool the bottom mass and distilled out remaining toluene under vacuum

11. Distill out product under vacuum (Used 2 feet SS packed column for distillation),

1st fraction containing toluene to be recycled in next batch

12. Collect main fraction as finished good

13. Re-distill the main cut of fractional distillation to remove moisture content within limit

14. Recycle the bottom cut in next batch.


54

7) Products - 2,5 Xylenol Input Raw Materials:

No. Raw Material Consumption (MT/ Month)

1 2, 5 Xylidine 32.1

4 H2SO4 28.7


6 MIBK 4.8

7 Hexane 7.8

Reaction:



55

Process description

Operations

1. Charge water in reactor and start stirring & add 98% H2SO4, MIBK, 2,5-Xylidine. 2. Add NaNO2 solution to above mass, due to exothermicity of reaction, temperature rises,.

3.Maintain this temperature throughout the reaction

3. After complete addition of NaNO2 solution, stir the mass, and cool this mixture.

4. Separate the two layers (organic on the top) & aq. layer extract with MIBK .

5. Wash the total organic layer with water, to remove the acidity

6. Recover MIBK at atmospheric pressure, using packed column

7. Apply vacuum for removing traces of MIBK.

8. Purify the final product by high vacuum distillation

9. Charge n – Hexane & 2,5-Xylenol and start stirring

10. Filter and wash then note the weight of cake and dry solid


56

8) Product - Phenyl Hydrazine Input Raw Materials:

Sr. No Name of Raw Material Consumption (MT/Month)

1 Aniline 107.1

2 Hydrochloric acid 709.8

3 Sodium nitrite,40% 214.3

4 Sodium bisulfite,40% 530.4

5 NaOH 444.6

6 Soda ash 204.9

7 Toluene 357.6

8 Water 1399.6

Recovery of Solvent

No. Name of Raw Material Qty(MT/Month)

1 Toluene 37.48


57

Reaction

Stage-1 : Di-Azotization of Aniline

Stage: 2 Reduction of Di-azonium salt & Hydrolysis.


58



59


60

Process description

Stage:1 Preparation of Di-Azonium Salt.

Process:

1. Charge water and start stirring. Then add HCl solution followed by aniline addition.

2. Stir and cool reaction mass. 3. Start addition of sodium nitrite solution at low temperature and maintain this reaction

mass.

4. Kill excess Nox using Sulfamic acid.

Stage:2 Reduction and hydrolysis.

Process: 1. Adjust the pH of sodium hydrogen sulfite solution using caustic lye the cool the reaction

mass.

2. Start addition of diazo mass in NaHSO3 solution at low temperature

3. After compete addition of diazo slowly increase reaction mass temp & maintain it.

4. Heat the reaction mass 5. Add slowly HCl solution and maintain temperature, SO2 gas will get scrubbed in caustic

scrubber after reaction

6. Cool this reaction mass and filter wet cake

7. Take wet cake in water and start stirring

8. Neutralize Hydrochloride salt using Caustic lye and adjust pH

9. Extract the reaction mass using Toluene

10. Separate Organic layer with emulsion and Aqueous layer

11. Give another two extraction to aqueous layer

12. Separate Organic layer and Aqueous layer


61

13. Mix all organic layers perform filtration through hyflow to remove emulsion in organic layer

14. Add Ethylene glycol in bottom before distillation

15. Distilled out Toluene under vacuum

16. Remove the traces of Toluene by applying high vacuum

17. Cool this distilled Bottom mass (phenyl hydrazine)

18. Take weight of conc. bottom Phenyl hydrazine brown liquid & analyze it

19. Add quantitative water in crude to make solution as per specification

20. After water addition check sample as per specification

21. Recycle distilled Toluene in next batch for extraction

9) Product - Triazinone INPUT

Sr. No. Name of Raw Material Consumption (MT/Month)

1 Dichloropinacoline 426.3

2 48% Cslye 735

3 Catalyst 0.00

4 12% NaOCl 1763.9

6 Thiocarbohydrazide 259.7

7 30% HCl 1376.9

Reaction

Process block diagram:


62


63

Process description: 1. Charge water and CSLye solution with normal water supply. 2. Raise temperature under stirring and add lots of Dichloro Pinacolone. 3. Add catalyst and start addition of NaOCl post stirring, then filter catalyst and kept filtrate ml for next step. 4. Charge TCH & HCl solution and start heating under stirring. 5. Start addition of filtrate ml in TCH + HCl solution. 6. Stop stirring and cool mass and filter solid. 7. Wash wet solid by DM water and filter solid. Air dry solid to reduce LOD.


64

10) Product - Thiocarbohydrazide (TCH) Input Raw Materials:

No. Cost Head Consumption (MT/MT product)

1 Hydrazine hydrate (80%) 512.4

2 Carbon disulphide 298.1

3 47% Cslye 31.1

4 Mercaptoethanol 29.5

5 20% Cslye 99.4

Reaction:

Process block diagrams: (All quantities are in kg)


65

Process description: 1. Charge hydrazine hydrate & Catalyst in reactor and start stirring. 2. Cool this mass under stirring and start addition of carbon disulphide (lot-1). 3. Then after completion start addition of carbon disulphide (Lot-2). 4. After addition stir mass for few hours then raise temperature. 5. Maintain for 10 hrs after stirring. 6. Remove sample and filter through cloth then wash solid sample with equal amount of water and send for analysis. 7. Cool the mass and filter it. 8. Unload wet solid and add DM water under stirring and raise temperature. 9. After some time, cool mass and filter the solid 10. Suck dry under vacuum and unload wet solid and dry solid


66

11) Product - 3 Amino Benzotriflouride (3-ABTF) Input Raw Materials:


1 BTF 186.3

2 H2SO4 389

3 HNO3 117

4 Soda ash 4.3

5 Water 242.9

6 Catalyst 0.2

7 H2 gas 7.8

Reaction

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

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


67



68


69


Stage: 1

1. Charge Sulphuric acid and start stirring then add benzoflouride.

2. Cool the reaction mass at desired temperature

3. Add slowly nitric acid maintaining temp

4. Maintain temperature of reaction mass for 3 hrs.

5. Take out sample for GC analysis and check %BTF by GC; it should be less than 1%.

6. Add water under stirring. Temperature raised to RT

7. Keep it for settling and separate out layers.

8. Bottom layer is spent acid.

9. Top organic layer is crude 3-nitrobenzotrifluoride.

10. Wash organic layer with sodium carbonate solution.

11. Layer separate out.

12. Send aqueous layer to ETP.

13. Distill out organic layer of nitro-benzotrifluoride under vacuum

14. Send residue for disposal.

Stage: 2

.

1. Add distilled 3-nitrobenzotrifluoride and catalyst.

2. Take flush autoclave with Nitrogen then take hydrogen pressure in autoclave. 3. Start stirring & maintain temperaturand hydrogen pressure until hydrogen absorption

stops 4. After completion of reaction remove sample and analyze for unreacted nitrobenzo-

trifluoride 5. Take out the reaction mass. 6. Filter reaction mass and washings to recover catalyst for recycle. 7. Take filtrate for distillation of Amino BTF under vacuum 8. Remaining distillation residue to be disposed


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12) Product - Triflouro Methyl Acetophenone (TFMAP) Input Raw Materials:

No.



1 3-ABTF 193.8

2 H2SO4 240.8

3 Toluene 46.6

4 NaNO2 89.1

5 Sulfamic acid 6.6

6 AAO 85.8

7 Acetic acid 24.1

8 CuSO4 18.1

9 NaOH 157.3

10 HCl 273.9

Reactions:


71



72

Process description: STAGE-1- 1. Charge water and start stirring . 2 .Add slowly sulfuric acid. Add 3-ABTF slowly under stirring and heat solution. 3. Cool the reaction mass. Prepare sodium nitrite solution in water. 4. Add of sodium nitrite solution within 1 hrs. Maintaining temperature. 5. Stir the reaction mass then check SI positive for diazo mass. 6. Add sulphamic acid solution to decompose excess sodium nitrite. 7. Store this diazomass solution by controling temperature . 8. Charge water, acetaldoxime and glacial acetic acid and start stirring. 9. Then add copper (II) sulfate and toluene.Cool it to desired temperature. 10. Add slowly solution with maintaining temperature and pH. 11. Stir it further, maintaining pH. Increase temperature to RT and allow to settle 12. Separate out bottom aqueous layer, wash it with toluene and sent to ETP. 13. Mix both organic layer take for second stage STAGE-2 : 1. Charge organic layer into it and start stirring. 2. Add hydrochloric acid. Heat it to up to desired temperature and maintain it for 6 hrs. 3. Take out sample and analyze by GC for 3'-(Trifluoromethyl) acetophenone-oxime. 4. Cool the reaction mass to room temp and allow settling. 5. Bottom aqueous layer to be sent for analysis.Top organic layer is crude TFMAP in toluene. 6. Wash organic layer with sodium hydroxide solution. 7. Separate bottom aqueous layer. 8. Take Organic layer of toluene for atmospheric recovery 9. Cool bottom mass and distilled out remaining toluene and TFMAP under vacuum . 10. Discard residue.


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13) Product - SMIA Input Raw Materials:

No. Name of Raw Material Qty (MT/Month)

1 2 Acetyl Furan 62.7 2 HCl (30%) 402.7 3 Sod nitrite 176.5 4 Caustic Soda Lye (100%) 29.8 5 Sodium Chloride 183.8

6 Butyl Acetate 22.4

7 Methanol 35.7

8 Catalyst A 28

9 MA HCl 42.6

10 Ammonia 7

11 Activated Charcoal 2.1

12 MDC 21

Reactions:


74



75


76


Stage 1 : Oxidation.

1. Set up assembly and charge water then start stirring and heating. 2. Add HCl (30%) heat then add 2-Acetyl furan . 3. Then Add SNI solution followed by catalyst addition 4. Cool the reaction then extract it with Methylene dichloride 5. Recover 2-acetyl furan by and MDC distillation 6. Adjust pH 4.5 by CS lye solution.

Stage 2 : Oximation. 1. Add MA HCl solution in Reaction mass. 2. Maintain the reaction mass at desired temp. and pH.

3. Cool the reaction mass and 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

Stage 3 : SMIA Ammonium salt.

1. Add the n-Butyl acetate solution, cool it.

2. Purge the ammonia gas till pH reaches 6-7, then maintain

3. Filter the reaction mass trough centrifuge and Spin well

4. Collect the wet cake, filtrate Butyl acetate, Oily solution

Stage 4 : Purification

1. Take SMIA wet cake with Methanol at RT.

2. Start stirring and raise temperature to get clear solution.

3. Filter reaction mass through hyflo bed

4. Distill 50% methanol by weight of filtrate ml

5. Cool bottom mass and centrifuge solid

6. Dry the wet cake

7. Recovered the SMIA from filtrate.


77

14) Product - Quetiapine INT (DBTZ) Input Raw Materials:


1 Thiophenol 14.1

2 caustic lye 12.6

3 1-chloro-2-nitro benzene 20.5

4 TBAB 0.1

5 Conc. HCl 0.1

6 Acetic acid 1.2

7 Iron powder 24.7

8 Toluene 13.1

9 phenyl chloroformate 20.1

10 Na2CO3 15.8

11 polyphosphoric acid 107.1

12 phosphorus pentoxide 28.9

13 Methanol 28.6

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

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


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

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


79



80


81

Process description

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

1. Charge caustic solution. Add thiophenoland stir the reaction mass at same temperature 2. Then add TBAB.Add 1-chloro2-nitrobenzene at ambient temperature and stir reaction. 3. Heat the reaction mass to reflux temperature till reaction completion. 4. After completion of reaction add water in reaction mass and cool the reaction. 5. Adjust the pH by adding HCl and stir the reaction mass. 6. Filter the reaction mass at ambient temperature and wash the cake with hot water. 7. Wet product can be used for next stage on LOD basis. Stage: 2 Preparation of 2-(phenyl sulfanyl)-aniline 1. Charge water, acetic acid and Fe-powder then heat the reaction mass up to warm. 2. 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. 3. 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. 4. 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. 5. Filter organic layer through celulite 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

1. Charge stage 2 organic layers and heat the reaction mass and start stirring. 2. Add one part of Phenyl chloro formate solution in Toluene into reaction mass and stir. 3. After the addition raise the temperature and stir till reaction completion. 4. After completion of reaction add water under cooling condition. 5. Separate the two layers and wash the organic layer with water. 6. Take the organic layer for solvent recovery and organic mass to be used for the next stage.

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

1. Charge poly phosphoric acid and P2O5 powder under stirring and heat the reaction mass and stir. 2. Add stage 3 at this temperature and heat the reaction mass up to reflux and stir till reaction completion. 3. After completion of reaction cool the reaction mass and add water. 4. After addition of water cool the reaction to ambient temperature. 5. Filter the reaction mass at warm temperature and wash it with water. 6. Take the wet cake in RBF and add methanol for purification.Cool the mass slowly and filter. 7. Recover the methanol by distillation and recycle in next batch. 8. Dry the final product under vacuum at ambient temperature.


82

15) Product - Guanine Input Raw Materials:


1 Methyl cyanoacetate 23.3

2 Guanidine nitrate 30.3

3 Sodium methoxide 25.7

4 Methanol 23.3

5 H2SO4 0.00

6 Formamide 9.4


8 Formic acid 46.6

9 Sodium dithionite 7.5

10 HCl 287.4

11 CSLye 46.6

12 Charcoal 0.8

13 Water 562.5

Reaction

Stage: 1 Preparation of 2,4-diamino-6-hydroxy-5-nitrosopyridine

Stage: 2 Preparation of Guanine


83



84

Process description

Stage:1 Preparation of 2,4-diamino-6-hydroxy-5-nitrosopyridine

1. Charge methanol and sodium methoxide and stirr.

2. Add Guanidine,HNO3 and stir mass. 3. Filter mass at RT remove NaNO3 and wash wet solid with fresh methanol, keep wet NaNO3 for drying at warm condition. 4. Collect filtrate ml and wash ml, transfer to reactor. 5. Start heating under stirring and maintained reflux 6. prepare solution of sodium methoxide & methanol and store in addition funnel 7. Take Methyl cyno acetate in another addition funnel and start simultaneous addition of sodium methoxide and Methyl cyno acetate at reflux then stirr the mass and send sample for HPLC analysis. 8. After completion of reaction start distillation to recover solvent at atmospheri pressure.

9. Cool mass and Filter to get dry solid

10. Prepare solution of sodium nitrite in water. 11. Cool above mass and start addition of NaNO2 solution then stir mass at same temperature. Give sample for HPLC analysis.

12. After completion of reaction,filter mass at RT and give water wash, then dry solid.

Stage:2 Preparation of Guanine

1. Charge above solid and add Formamide and stir mass then add Formic acid then raise temperature to reflux and add sodium dithionite.

2. After dithionite addition stirr reaction masss. Send sample for HPLC analysis. 3. After completion of reaction, distill formamide under vacuum then cool the reaction add water and cool reaction mass.

4. Filter the solid and suck dry well.

5. Charge above crude guanine and add 10% HCl and raise temperature

6. Add charcoal and stir, then filter charcoal through hyflo and remove charcoal sludge. 7. Cool filtrate ml under stirring and filter solid (Guanine.HCl),suck dry wet solid under vacuum.

8. Wash solid with l water and suck dry under vacuum

9. Remove wet solid of guanine.HCl then add water. Add CSlye to set neutral pH , stir mass

10. Filter the solid and wash with water.

11. Dry wet solid


85

16) Product - Acyclovir Input Raw Materials:


1 Guanine 26.8

2 Acetic anhydride 304.6

3 acetic acid 401.8

4 Water 1178.6

5 Methanol 89.7

6 Dioxolane 29.8

7 PTSA.H2O 1.3

8 Phosphoric acid 1.9

9 Toluene 76.5

10 Ethyl acetate 76.5

11 Methyl amine solution 229.6


86

Reactions:

Stage: 1 Preparation of Diacetyl guanine

Stage: 2 Preparation of Dioxolane-diacetate.

Stage: 3 Preparation of Acyclovir


87



88


Stage: 01 Preparation Diacetyl guanine 1. Charge guanine, acetic anhydride and acetic acid. 2. Reflux reaction mass for two days, during which time the mixture became an almost clear solution. 3 .Removed acetic acid by distillation under vacuum. 4. Collect solid by filtration, wash with water followed by methanol and dry to give pure Diacetyl guanine .

Stage: 02 Preparation of Dioxolane-diacetate.

1. Charge acetic acid then add addition of acetic anhydride with stirring at room temperature. 2. Cool the reaction mass then add PTSA and slowly added dioxolane with stirring. 3. Remove acetic acid by distillation under vacuum in first fraction. 4. By fractional distillation collect pure liquid product(Stage 02) in second fraction and used as in next step.

Stage: 3 Preparation of Acyclovir

1. Charged toluene and phosphoric acid with stirring at room temperature.

2. Add Diacetyl guanine (stage 01) followed by slow addition of (stage 02) with stirring.

3. Maintain the reaction mass at reflux temperature for several hours. 4. Cool the reaction mass to room temperature then solid dissolve in ethyl acetate and added methyl amine with stirring. 5. Maintain reaction mass for few hours at same temperature. 6. Cool the reaction mass and Collect the solid by filtration and carried out recrystallization in water to give pure final product (acyclovir).


89

17) Product - Tenofovir Input Raw Materials:


1 Adenine 74.4

2 NaOH (48% Lye) 70.7

3 DMF 595.2

4 (R)-1,2-Propylene carbonate 74.4

5 MeOH 238.1

6 Isopropanol 238.1

7 NaNH2 27.1

8 Diethyl p-toluenesulfonyloxymethyl phosphonate 167.4

9 MgCl2 32.9

10 Toluene 190.8

11 HCl (Dry) 350.9

12 MDC 234.4

13 Acetone 52.5

14 Water 589.3

Reaction

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

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


90

Process block diagrams


91

Process description Stage:1 Preparation of (R)-9-(2-Hydroxypropyl) adenine 1. Charge Adenine and DMF under stirring. 2. Add NaOH flakes followed by addition of (R)- Propylene carbonate. 3. Heat the reaction mass to reflux temperature and maintain till the reaction completed. 4. Cool the reaction and add methanol-isopropyl alcohol mixture then stir. 5. Filter the solid then wash the solid with chilled isopropyl alcohol. 6. Dry the product under vacuum.

Stage:2 Preparation of (R)-9-[2-(Phosphonomethoxy) propyl] adenine 1. Charge Dimethyl formamide followed by addtion of (R)-9-(2-Hydroxypropyl) adenine then stir the reaction mass. 2. Cool the reaction mass and add slowly NaNH2 to the solution then add MgCl2 powder. 3. Add diethyl p-toluenesulfonyloxymethyl phosphonate solution (dissolved in toluene) slowly then maintain the reaction at warm temperature.Again cool the reaction mass and purged dry HCl for few hours. 4. then again raise temperature to reflux and maintain. 5. After completion of the reaction quenched the mass in water and wet cake washed with MDC at room temperature. 6. Separate the MDC & aquoues layer precipitated out with NaOH solution then stir. 7. Filter the solid then wash the solid with chilled water followed by acetone. 8. Dry the product under vacuum.


92

18) Product - 2-Chloromethyl-3,5-Dimethyl-4-methoxy pyridine hydrochloride ( Omeprazole Chloro Int.) Input Raw Materials:


1 2,3,5-Collidine 15.4

2 Hydrogen peroxide(50%) 13.8

3 Glacial Acetic acid 7.7

4 Phosphotangstic acid 0.2

5 Sulphuric acid 98.2

6 Nitric acid 48.7

7 Toluene 50.5

8 Coustic lye 196.7

9 Methanol 433.9

10 Coustic flakes 10.3

11 MDC 625.4

12 Acetic acid 11.4

13 Acetic anhydride 33.8

14 Thionyl chloride 10.4

Recovery of Solvent

No. Name of Raw Material Qty (MT/Month)

1 Methanol 216.56

2 Toluene 30.93

3 MDC 382.92

Reaction

Stage: 1 Preparation of 2,3,5-Collidine N-Oxide

Stage: 2 Preparation of 4-Nitro-2,3,5-collidine N-oxide


93

Stage:3 Preparation of 4-Methoxy-2,3,5-collidine N-oxide

Stage:4 Preparation of 3,5-Dimethyl-4-methoxy-2-hydroxy-methylpyridine

Stage:5 Preparation of 2-Chloromethyl-3,5-Dimethyl-4-methoxy pyridine hydrochloride


94

Process block diagrams:


95

Process description

Stage:1 Preparation of 2,3,5- Trimethyl pyridine N-oxide

Process:

1. Charge 2,3,5 - Collidine and catalyst solution. 2. Heating raised and slowly start addition of H2O2 solution.

3. Keep reaction mass maintained or and confirm reaction completion by GC analysis.

4. After reaction completion, slowly start distillation of water under reduced pressure

5. Cool the reaction mass and slowly add acetic acid under stirring.

6. Further distill solvent under reduced pressure until not solvent come out.

7. Cool the product and store in close container.

Stage:2 Preparation of 2,3,5-trimethyl-4-nitropyridine N-oxide

Process:

1. Charge 2,3,5 - Collidine N-oxide and add drop wise sulfuric acid under stirring.


96

2. Heating raised and start drop wise addition of HNO3 while maintaining.

3. Keep reaction mass maintained or and confirm reaction completion by GC analysis.

4. After reaction completed, cool reaction mass & slowly quenched in ice water under stirring.

5. Adjust the pH by 30% NaOH solution.

6. Add toluene and stir, then wait for settling of organic layer. 7. Separate the organic layer and again add toluene to aqueous layer for further product e extraction.

8. Combine the organic layers and distill the toluene under reduced pressure.

9. Cool bottom mass and maintain, then crush and filter under vacuum.

10. Dry final product under vacuum and store in close dark container.

Stage:3 Preparation of 4-Methoxy-2,3,5-collidine N-oxide

Process:

1. Charge 2,3,5-trimethyl-4-nitropyridine N-oxide and methanol under stirring. 2. Heat upto reflux and slowly start addition of NaOH solution in methanol.

3. Keep reaction mass maintained and confirm reaction completion by GC analysis.. 4. After reaction completed cool the mass to room temperature and adjust the pH by sulphuric acid and stir. 5. Remove methanol by distillation and extract the product with MDC.

6. Further distill solvent under reduced pressure until solvent does not come out.

7. Cool the product, Filter and store in close container.

Stage:4 Preparation of 3,5-Dimethyl-4-methoxy-2-hydroxy-methylpyridine

Process:

1. Charge 4-Methoxy-2,3,5-collidine N-oxide and add dropwise acetic acid under stirring.

2. Heating raised and start dropwise addition of acetic anhydride while maintaining. 3. Keep reaction mass maintained and confirm reaction completion by GC analysis..

4. After reaction completed cool the reaction mass and add methanol under stirring. 5. Distil out solvent under reduced pressure until not solvent come out.

6. Add caustic lye solution and water at room temperature under stirring.

7. Heating raised to reflux and maintaining temperature.

8. Cool the reaction mass and product extract with MDC at room temperature.

9. Further distill solvent under reduced pressure until not solvent come out.

Stage:5 Preparation of 2-Chloromethyl-3,5-Dimethyl-4-methoxy pyridine hydrochloride

Process:

1. Charge 3,5-Dimethyl-4-methoxy-2-hydroxy-methylpyridine and add MDC under stirring.

2. Cool the reaction mass and start addition of Thionyl chloride. 3. Keep reaction mass maintained and confirm reaction completion by GC analysis.

4. After reaction complised remove the MDC under reduce pressure upto 70%.

5 .Filter the solid and wash wet cake with methanol and suck dry completely.

6. Dry final product under vacuum and keep in closed container.


97

19) Product - 2,3,5-trimethyl-4-nitropyridine N-oxide( Omeprazole Nitro Int.) Input Raw Materials:

No.



1 2,3,5-Collidine 34.3

2 Hydrogen peroxide(50%) 30.9

3 Glacial Acetic acid 17.1

4 Phosphotangstic acid 0.4

5 Sulphuric acid 68.6

6 Nitric acid 54.9

7 Toluene 92.6

8 Coustic lye 171.4

Reactions:

Stage: 1 Preparation of 2,3,5-Collidine N-Oxide

Stage: 2 Preparation of 4-Nitro-2,3,5-collidine N-oxide


98



99


Stage:1 Preparation of 2,3,5- Trimethyl pyridine N-oxide

Process:

1. Charge 2,3,5 - Collidine and catalyst solution. 2. Raise Heating and slowly start addition of H2O2 solution while maintaining temperature. 3. Once reaction completed distill out water. 4. Cool the reaction mass and slowly add acetic acid under stirring. 5. Further distilled solvent under reduced pressure until not solvent come out. 6. Cool the product and store in close container.

Stage:2 Preparation of 2,3,5-trimethyl-4-nitropyridine N-oxide

Process: 1. Charge 2,3,5 - Collidine N-oxide and add dropwise sulfuric acid under stirring.

2. Raise Heating and start dropwise addition of HNO3 while maintaining. 3. After reaction complition cool the reaction mass and quenched in ice water under stirring. 4. Adjust the pH using NaOH solution. 5. Add toluene and stir. 6. Separate the organic layer and again add toluene to aqueous layer for further product extraction. 7. Combine the organic layers and distill the toluene under reduced pressure. 8. Bottom mass cool and maintain, then crushed and filtered under vacuum. 9. Final product dried and stored in close container.


100

20) Product- 7-Ethyl tryptophol (Etodolac int.) Input Raw Materials:

Reaction

Stage-1 7-Ethyl tryptophol (Etodolac int.)

Stage-2 2 Preparation of 7-Ethyl tryptophol (ETP)


1 2-ethyl aniline 13.8

2 Conc. HCl 103.4

3 Sodium Nitrite 8.9

4 sodium sulphite 57.6

5 H2SO4 61.9

6 DMAc 68.7

7 2,3 dihydrofuran 7.5

8 Na2CO3 12.4

9 Dichloro methane 59.4

10 NaHCO3 3.7

11 Cyclohexane 14.6


101

Process block diagrams:


102

Process description

Stage:1


103

1. Charge solution of Conc HCl and cool. 2. Add 2ethyl aniline at cooling temperature and stir. 3. Again cool reaction. Add NaNO2 Solution slowly at cooling condition with stirring. 4. Take sodium sulphite solution in another RBF and cool. 5. Add chilled above diazonium chloride solution to the sodium sulphite solution at cooling condition. 6. Stir the reaction. Heat the reaction and add conc H2SO4 slowly and maintain. 7. Cool the reaction mass and stir. 8. Filter the solid then wash the solid with Conc HCl. 9. Filter the solid product again wash with chilled Conc HCl. Stage:2 1. Charge Dimethyl acetamide followed by addition of 2-ethylphenyl hydrazine HCl. 2. Stirr the reaction. Add 2,3 di hydro furan to the above solution at ambient temperature. 3. Heat the reaction mass. Add conc. H2SO4,then maintain the reaction. 4. Monitor the reaction. After completion of reaction cool the reaction mass. Adjust the pH. 5. Extract the reaction mass with MDC. 6. Wash the MDC layer with HCl followed by washing with saturated bicarbonate and water. 7. Distill the MDC. Add cyclohexane to the bottom residue and stir the reaction mass. 8. Filter the product. Dry the product.

21) Product - S-Alcohol (Duloxetine Intermediate) Input Raw Materials:


104

No. Name of Raw Material Consumption

(MT/Month)

1 2- Acetyl Thiophene 22.4

2 Paraformaldehyde 8.5

3 Dimethyl amine-HCl 20.4

4 Conc. HCl 1

5 NaOH 47.5

6 Isopropyl alcohol 314.6

7 Triethanol Amine 15.2

8 Catalyst 0.2

9 Toluene 54.6

10. H2SO4 0.7

Reaction

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



105


106

Process description

Stage-1 1. Charge Isopropyl alcohol (IPA), HCl at RT . 2. Add paraformaldehyde, dimethyl amine hydrochloride & first half of 2-acetylthiophene & stir. 3. Heat reaction mass and maintain for 1hr. 4. Add few crystals of product for seeding to induce partial crystallization. 5. Stir this mixture, again heat reaction to reflux temperature. 6. Add remaining 2-acetylthiophene. 7. Maintain reaction till completion. 8. After completion of reaction, cool the mixture and stir reaction mass. 9. Filter solid under suction, wash with chilled IPA and dry at ambient temperature.

Stage-2

PART - A : 1. Charge 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride. 2. Add IPA, stir for desired time. Adjust PH NaOH solution, again stir for some time. 3. Separate organic layer and add D.M water and adjust PH using H2SO4. 4. Transfer whole reaction mass and add IPA. PART-B : 1. Add tri ethanol amine and water and stir it. 2. Add catalyst and stir at RT to make homogeneous mixture. 3. Add this part -B solution to Part -A and stir. 4. Heat reaction mass under vacuum for IPA and start acetone recovery at RT. 5. Add IPA continuously to make volume during distillation. 6. Distill solvents till reaction completion. 7. After completion of reaction, recover whole IPA and water. 8. Add NaOH solution to increase PH and stir it. 9. Cool mass & stir. Centrifuge it. Add water to wet cake & stir under cooling then again centrifuge it. 10 .Add toluene to wet cake and stir ambient temperature. 11. Filter through hyflow Cool filtrate and again centrifuge it.


107

12. Give sample for HPLC. Dry product in Oven.

22) Product - 2-Methyl-3-Amino Benzotrifluoride (MTA)

Input Raw Materials:

No. Name of Raw Material Consumption

(MT/Month)

1 3,4-Dichloro-6-trifluoromethyl toluene 46.4

2 H2SO4 79.1

3 HNO3 13.8

4 Methanol 0.2

5 Hydrogen 15.8

6 Sodium acetate 16

7 Hydrogen 6.6

Reactions:

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

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


108



109

Operations: Stage-1


110

1. Charge sulphuric acid and 2-NO2-3,4-Dichloro-6-Trifluoromethyl-Toluene 2. Start stirring and start the nitric Acid addition at desired temperature. 3. After reaction completion perform layer separation at hot condition. 4. Cool the spent acid layer at RT and perform filtration to remove traces of 2-NO2-3,4- dichloro-6-Trifluoromethyl-Toluene. 5. Give water wash to top organic layer and perform hot layer separation. 6. Separate out Bottom organic layer and top aqueous layer . 7. Give water washing to aq. Layer for ETP. 8. Take organic layer in soda solution to remove acidity. 9. Perform hot layer separation bottom layer organic and top aqueous layer. 10. Send aqueous layer to ETP to organic layer give water wash to remove excess alkalinity. 11.Take organic layer for Hydrogenation.

Operations: Stage-2 1. Charge 2- No2-3,4-Dichloro-6-Trifluoromethyl toluene in methanol. 2. Add sodium acetate and catalyst and flush the autoclave with nitrogen. 3. Take hydrogen pressure and start stirring. 4. After complete reaction cool the reaction mass and vent hydrogen gas. 5. Remove the reaction mass from autoclave and perform filtration to remove catalyst. 6. Separate out water from organic layer.

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