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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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,
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Independent Director
Chartered Accountant 42
7 Mr. Sudhir Mankad
Independent Director
Masters’ degree in History 40
8 Dr. R. H. Rupp Independent Director
Ph.D in Chemistry 38
9 Dr. Swaminathan Sivaram
Independent Director
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
19
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).
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
5
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,
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Agrochemicals intermediate and Pharmaceuticals
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
Agrochemicals intermediate and Pharmaceuticals
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
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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:
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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)
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Sr No. Name of CompoundProduct
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
17
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
Sr No. Name of CompoundProduct
Number
1 Methanol
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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:
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
5 2 Nitro Benzotri Flouride (3NBTF) 0.00 0 0.0
6 4 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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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 --
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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:
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Flouride (3NBTF) 0.00 0 0.0
64 Nitro Benzotri
Flouride (3NBTF) 0.00 0 0.0
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Sale to actual users /TSDF
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
Sale to actual users /TSDF
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
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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.
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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.
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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.
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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.
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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.
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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
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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.
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ANNEXURE I Google image of study area Site with 10 km radius area
Site with 1 km radius area
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ANNEXURE II Plot transfer order
Plot No. 8 attached, Plot No. 32-34 Lease document under approval at MIDC.
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Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
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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.
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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
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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
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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
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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
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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
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DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
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2) 3 ABTF
DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
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DEEPAK NITRITE LIMITED
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
Distillation residue
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
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DEEPAK NITRITE LIMITED
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)
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3) Ortho Anicidine
DEEPAK NITRITE LIMITED
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
2 Liquid Effluent 3.76 7
3 0.001 0.002
4 0.001 0.002
5 0.020 0.036
Description
Water Consumption
Distillation residue
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
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DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
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4) TMHQ
DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
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DEEPAK NITRITE LIMITED
APL DIVISION
Production of TMHQ 50 MT/Month
Reaction:
Stage-I Preparation of TMHQ
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5) 2,4 Nitro Xylene
Process Description:
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
Distillation residue
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
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DEEPAK NITRITE LIMITED
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
Distillation residue
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
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DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
61
6) 3,4 Nitro Xylene
DEEPAK NITRITE LIMITED
APL DIVISION
STAGEWISE MASS BALANCE
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
2 Liquid Effluent 2.19 104
3 0.047 2.23
4 0.714 33.92
Distillation residue
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
63
7) 2,3 Xylenol
DEEPAK NITRITE LIMITED 700 1350
APL DIVISION 850 1639.286
1.928571
STAGEWISE MASS BALANCE
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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Process Description:
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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Reaction:
Stage-I Preparation of 2,5 Xylenol
NH2
CH3
CH3
OH
CH3
CH3
1) NaNO2 + H2SO4
2 ) MIBK
3) 55- 60 o c
Process Description:
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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)
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Process Description:
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Process Description:
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
Reaction Mass 1655.3
Sodium Diothionite 0.9
Reaction Mass 1656.2
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
2-Methyl-p-Phenelene diamine
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
2-Methyl-p-Phenelene diamine
M Wt - 122
Sulphuric Acid
M Wt - 98
2-Methyl-p-Phenelene diamine
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Process Description:
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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Production of SMIA 25 MT/Month
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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%
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
92
Project 2-Cyano phenol
Reaction scheme
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
4-Chloro-6-methylanthranilimide
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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)
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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6-Aminopurine (Adenine) reaction scheme
Stage: 1 Preparation of Phenylazomalononitrile
Stage: 2 Preparation of 6-Aminopurine(Adenine)
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
W/C Drying under vacuum
1.0
Quenching and layer
separation
Condensation
Condensation
Hydrolysis
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Stage:1 Preparation of 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Isopropyl alcohol 12.00
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
Filtration of pure solid
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
105
Process description
Stage:1 Preparation of 3-Dimethyl amino 1-(2-Theinyl) 1-Propanone hydrochloride
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.
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.
27 Give sample for HPLC. Dry product in Oven.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
106
28) DBTZ (Quetiapine Int.)
2- Acetyl Thiophene 0.75
Paraformaldehyde 0.28
Dimethyl amine-HCl 0.68
Conc. HCl 0.04
Isopropyl alcohol 1.77
Reaction Mass 3.5
2.26
Recoverd IPA check
purity & recycle1.81
Isopropyl alcohol 2.85
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
W/C 0.712Recoverd Toluene check
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
Condensation reaction
Reduction and resolution
Distillation and work up
0.667
Crystalisation
Stage 2 Product
W/C Drying
Filtration of pure solid
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Condensation reaction
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
Filtration of pure solid
Aqueous ML send to
ETP
Main filtrate ML
(org. mass)
Rec. MeOH check.
W/C Drying under vacuum
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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.
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
W/C 1.10Recoverd Toluene check
purity & recycle
2.56
0.640
Drying vapour loss
0.1
Sr.No. MT/MT KLD
1 5.00 5.36
2 Liquid Effluent 3.90 4.18
3 0.640 0.69
5 lit RBF With N2 ATM
Layer separation
Condensation
reaction
Crystalisation
High Vacuum Distillation
Precipitation and Filtration
Filtration of pure solid
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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 ,
Clean and dry 3 l it RBF with reflux condenser on oil bath
Started addition of Cocn. H2SO4 ,
Clean and dry 1 l it RBF with reflux condenser on oil bath
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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
2 Liquid Effluent 39.40 42.21
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
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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.
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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
2 Liquid Effluent 8.55 9.16
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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
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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
Stage: 2 Preparation of 2-Methyl-3-Aminobenzotrifluoride
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
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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
Stage: 2 Preparation of 2-Methyl-3-Aminobenzotrifluoride
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
Prefeasibility Report Deepak Nitrite Limited, MIDC Roha
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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%
4-Chloro-6-methylanthranilimide
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
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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
2 Liquid Effluent 25.66 27.50
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