LIST OF ANNEXURESenvironmentclearance.nic.in/writereaddata/Online/TOR/26_Oct_2019_185545677DUCW4LCS...11 list of annexures sr. no. name of annexure i list of products with their production

11

LIST OF ANNEXURES

SR. NO. NAME OF ANNEXURE

I LIST OF PRODUCTS WITH THEIR PRODUCTION CAPACITY

II LAYOUT MAP OF THE PLANT

III BRIEF MANUFACTURING PROCESS DESCRIPTION

IV DETAILS OF WATER CONSUMPTION WASTEWATER GENERATION AND TREATMENT

V DETAILS OF PROPOSED EFFLUENT TREATMENT PLANT

VI DETAILS OF HAZARDOUS SOLID WASTE MANAGEMENT AND DISPOSAL

VII DETAILS OF STACKS AND VENTS

VIII DETAILS OF HAZARDOUS CHEMICALS STORAGE FACILITY

IX GIDC PLOT ALLOTMENT LETTER

X MEMBERSHIP OF COMMON MEE,TSDF AND CHWIF

XI TOPO SHEET

XII GIDC WATER SUPPLY LETTER

XIII PRODUCT WISE SOLVENT, SPENT SOLVENT & ITS RECOVERY

XIV DETAILS OF PROJECT COST AND EMS BUDGET

XV HON’BLE NGT ORDER FOR CRITICALLY POLLUTED AREA & ITS COMPLIANCE BY

CPCB

12

ANNEXURE – I

LIST OF PRODUCTS WITH THEIR PRODUCTION CAPACITY& RAW MATERIALS

SR.

NO. NAME OF PRODUCTS

CAS no. /CI no

QUANTITY

(MT/MONTH)

1 Ketoconazole and its intermediates 65277-42-1

35

1A Cis-Tosylate 154003-23-3

1B Cis-Bromobenzoate 16887-76-6

1C N, N, Bis (2-chloroethyl) amine Hydrochloride 821-48-7

1D 1-Acetyl-4-(4-Hydroxy Phenyl) Piperazine 67915-02-0

2 2-Chloro Ethylamine Hydrochloride 870-24-6

3 Meloxicam and its intermediates 71125-38-7

3A 2-Amino-5-methyl Thiozol 7305-71-7

3B Methyl Benzothiazine Isopropyl Ester 35511-15-0

4 Chloroxazone 95-25-0

5 1-(2, 3 DichloroPhenyl) Piperazine HCL 119532-26-2

6 1-(4-Methoxy-Phenyl)-4-(4-Nitro-Phenyl)-

Piperazine 74852-61-2

7 N-Methyl-1-Naptheline Methyl Amine

Hydrochloride 65473-13-4

8 Ambroxol HCl 23828-92-4

9 1-[2-(2-Hydroxyethoxy) ethyl] piperazine (HEEP) 13349-82-1

10 2,4-Dichloroacetophenone 2234-16-4

11 2,4-Dichlorovelrophenone 2234-16-4

12 1-(3-Chlorophenyl)Piperazine 65369-76-8

13 1-[2-(2-Hydroxyethyl)Ethoxy]Piperazine 13349-82-1

14 1-(3-Chloropropyl)-4-(3-Chlorophenyl)Piperazine

Hydrochloride 52605-52-4

15 1-(2-Methoxyphenyl) Piperazine Hydrochloride 5464-78-8

R & D 10 Kg/Month

TOTAL 35

13

ANNEXURE-I (CONT…)

PRODUCT WISE RAW MATERIALS CONSUMPTION:

Sr.

no

Product Raw Material CAS No MT/Month

1A Cis-Tosylate

CBB -- 45.5

IMD 288-32-4 40.418

DMF 15175-63-0 2.17

Toluene 108-88-3 97.762

Sodium Bicarbonate 774595-73-2 8.638

Sodium hydroxide 8012-01-9 7

HCl 7647-01-0 9.1

Ethyl acetate 141-78-6 99.54

Carbon 121565-74-0 0.35

Vacuum salt -- 0.35

Methylene dichloride 75-09-2 166.796

P-Toluene Sulfonyl Chloride 98-59-9 27.118

Sodium carbonate 497-19-8 17.934

Hydrochloric acid 7647-01-0 0.7

Methanol 67-56-1 83.12

Sr.

no


1B Cis-Bromobenzoate

2,4-DCAP 500015-20-3 23.32

Benzoyl Chloride 98-88-4 21.64

Bromine 7726-95-6 21.84

CS Flakes 1310-73-2 8.44

Glycerin 56-81-5 12.64

Liq. Ammonia 1336-21-6 17.47

Methanol 67-56-1 101.37

N- Butanol 71-36-3 7.00

PTSA 6192-52-5 0.63

Sr.

no.

Product Raw Materials CAS No.

MT/Month

1. Ketoconazole

CBB Coomassie Brilliant Blue - 53.55

IMD 288-32-4 47.6

DMF 15175-63-0 2.548

Toluene 108-88-3 115.024


Sodium hydroxide 8012-01-9 11.662

HCl 7647-01-0 10.71

Ethyl acetate 141-78-6 269.178

Carbon 121565-74-0 1.778

Vacuum salt - 0.406

Methylene Dichloride 75-09-2 196.238

P-Toluene Sulfonyl Chloride 98-59-9 31.906

Sodium carbonate 497-19-8 21.098


Methanol 67-56-1 130.116

Para hydroxyl phenyl n- acetyl piperazine - 19.558

Dimethyl sulfoxide 67-68-5 58.128

Sodium methoxide powder 124-41-4 4.802

Acetone 67-64-1 23.338

14


TEBAC 56-37-1 0.44

Toluene 108-88-3 80.26

Sr.

no


2 2-Chloro Ethyl Amine

Hydrochloride

Monoethanolamine 141-43-5 21.88

Thionyl chloride 7719-09-7 48.13

NaOH 1310-73-2 5.47

EDC 107-06-2 65.63

Sr.

no


3 Meloxicam

4-Hydroxy-2-methyl-2-H (ester) 24683-26-9 27.72

2- Amino 5 Methyl Thiazole 7305-71-7 10.64

Toluene 108-88-3 216.16

Methanol 67-56-1 154.42

Carbon 121565-74-0 2.52

Sr.

no


3A 2-Amino-5-Methyl

Thiozol

Propionic aldehyde 123-38-6 21.84

Sulfuryl chloride 7791-25-5 43.82

Thiouria 62-56-6 13.16

HCl 7647-01-0 5.46

Toluene 108-88-3 32.76

NaOH 1310-73-2 2.24

Sr.

no


1c

N, N, Bis (2-

chloroethyl) amine

Hydrochloride

Diethanol amine 111-42-2 21.00



Ammonium hydroxide 1336-21-6 8.75

EDC 107-06-2 140.00

Sr.

no


1D

1-Acetyl-4-(4-

Hydroxy Phenyl)

Piperazine

Di ethanol amine 111-42-2 18.03



Ammonium hydroxide 1336-21-6 8.75

Toluene 108-88-3 140.00

Sodium sulphate 7757-82-6 0.88

4-Amino phenol 123-30-8 18.55

Acetic anhydride 108-24-7 17.33

Potassium Carbonate 584-08-7 7.00


Methanol 67-56-1 175.00

Activated Carbon 64365-11-3 2.66


15

Sr.

no


3B

Methyl

Benzothiazine

Isopropyl Ester

DMF 15175-63-0 13.16

IPA 67-63-0 69.02

Sodium Saccharine 82385-42-0 29.12

Sodium Metal 7440-23-5 3.64

Sodium Sulphate solution 7757-82-6 3.36

DMS 75-18-3 2.66

HCl 7647-01-0 2.24

Xylene 1330-20-7 9.66

Methanol 67-56-1 9.66

Sr.

no


5

1-(2, 3 Dichlorophenyl)

Piperazine

Hydrochloride

2,3-Dichlorophenylamine 608-27-5 17.85

Bis-2(2-chloro-ethyl)-amine 821-48-7 18.73

Xylene 1330-20-7 175.00

Acetone 67-64-1 175.00

Activated carbon 121565-74-0 0.88

Sr.

no


6

1-(4-Methoxy-

Phenyl)-4-(4-Nitro-

Phenyl)-Piperazine

1-(4-Methoxy phenyl) Piperazine 38212-30-5 21.88

p-Nitro Chloro Benzene 100-00-5 17.85

Potassium Carbonate 584-08-7 7.88

DMF 15175-63-0 87.50

Sr.

no


7

N-Methyl-1-

Napthalenemethylamine

Hydrochloride

Naphthalene 91-20-3 22.40

Formaline 50-00-0 5.25


Phosphoric Acid 7664-38-2 8.75

MDC 75-09-2 140.00

Acetic acid 64-19-7 87.50

Sodium Carbonate 497-19-8 1.75

Sodium sulpahte 7757-82-6 1.75

Methyl amine 74-89-5 5.43

Methanol 67-56-1 140.00

Acetone 67-64-1 87.50

Sr.

no


4 Chloroxazone

4-Chloro-2- Amino Phenol 95-85-2 33.25

Urea 57-13-6 33.25

Hydrochloric Acid 7647-01-0 7.43

Methanol 67-56-1 105.00

Activated Carbon 121565-74-0 3.93

Sulphuric Acid 7664-93-9 3.50

Acetic Acid 64-19-7 17.50

Sodium Hydrosulphite 7775-14-6 1.75

16

Sr.

no


8 Ambroxol HCl

Methanol 67-56-1 119.39

Methyl Anthranilate 134-20-3 18.84

Bromine 10097-32-2 21.99

Liq. Ammonia 7664-41-7 5.35

Hydrogen Peroxide 7722-84-1 7.10

THF 109-99-9 244.80

Sodium Boro Hydride 137141-62-9 5.53

Acetic Acid 64-19-7 68.31

Toluene/EDC 108-88-3 87.98

Sodium Borohydride 137141-62-9 3.51

Trans 4-Amino Cyclohexanol 27489-62-9 37.14

IPA 67-63-0 113.11

Act Carbon 121565-74-0 0.31

HCl 7647-01-0 8.48

Sr.

no


9

1-[2-(2-

Hydroxyethoxy)ethyl]

piperazine

Piperazine 110-85-0 27.06

2- (2-chloroethoxy) ethanol 628-89-7 13.47


Methanol 67-56-1 14.50

Sr.

no


10 2,4-

Dichloroacetophenone

1,3-dichloro benzene 541-73-1 163.34

Aluminum chloride 7446-70-0 148.89

acetyl chloride 8012-01-9 87.78

Sr.

no


11

2,4-

Dichlorovelrophenone

1,3-dichloro benzene 541-73-1 163.34

Aluminum Chloride 7446-70-0 148.89

N- Veratroil Chloride 7646-85-7 87.78

Sr.

no


12 1-(3-

Chlorophenyl)Piperazine

3-Chloroaniline 108-42-9 26.60

Bis-(2-Chloroethyl)aminehydrochloride 821-48-7 37.45


Toluene 108-88-3 80.15

Sr.

no


13 1-[2-(2-Hydroxyethyl)

Ethoxy]Piperazine

2-Chloroethoxyethanol 628-89-7 27.65

Piperazine 110-85-0 57.75


Methanol 67-56-1 83.30

17

Sr.

no


14

1-(3-Chloropropyl)

-4-(3-Chlorophenyl)

Piperazine

Hydrochloride

1-(3-Chlorophenyl)piperazine 65369-76-8 24.15

1-Bromo-3-chloropropane 109-70-6 19.25


Conc. HCl (30%) 7647-01-0 15.05

Isopropyl alcohol 67-63-0 72.45

Toluene 108-88-3 96.60

Sr.

no


15

1-(2-Methoxyphenyl)

Piperazine

Hydrochloride

o-Anisidine 90-04-0 22.40

Bis(2-Chloroethyl)amine Hydrochloride 821-48-7 32.20


Toluene 108-88-3 66.50

IPA.HCl 7647-01-0 30.10

Isopropyl alcohol 67-63-0 66.50

18

ANNEXURE – II

LAYOUT MAP OF THE PLAN

19

MAJOR PLANT MACHINERY

Sr.No. Equipment’s Capacity Proposed

Nos.

1 SS316 rector with condenser and receiver 3000 Lit 5




5 GLR Reactor with condenser, receiver 3000 Lit 4

6 GLR Reactor with condenser, receiver 4000 Lit 4

7 ANFD (Agitated Nutch Filter Dryer) 48" 4

8 Nutch Filter 48" 3

9 SS sparkler filter 24"X16 2

10 Rotary Vacuumed Dryer 1000 Kg 1

11 Rotary Vacuumed Dryer SSR 1000 kg 1

12 MS Storage tank 15000 Lit 3

13 SS Storage tank 15000 Lit 3

14 HDPE Storage tank 20000 Lit 3

15 SS Storage Tank 5000 Lit 1

16 Aluminum Storage Tank 12000 Lit 1

17 Glass Assembly (for pilot plant R&D) 50 Lit 2

18 Glass Addition Pot 50 5

19 Trey Dryer 96 2

20 Steam Boiler 2 TPH 1

21 Cooling Tower 20 TR 1

22 vacuum pump 755 mm/Hg 4

23 PP & SS pumps -- 4

20

LAND BREAK-UP AREA

Sr.

No

Name

Area Into Sq.Mt.

1 Office & Qc Lab 102.96

2 Rm & Fg Stores 103.42

3 Production Block 285.93

4 ETP 102.25

5 Hazardous Waste 53.37

6 Evg. Store 37.83

7 Utility Block 74.30

8 Tank Farm 84.98

9 Solvent Store 84.98

10 Security Cabin 9.85

11 RCC Road 292.77

12 Open Storage 92.48

13 Green Belt 652.66

14 Total Area 1977.78

21

ANNEXURE – III

BRIEF PROCESS DESCRIPTION

1. KETOCONAZOLE AND ITS INTERMEDIATES:

KT-I: CBB is reacted with IMD in the presence of DMF as solvent. The reaction mass is quenched in sodium

bicarbonate solution and the product is extracted with toluene.

The aqueous layer is kept for IMD recovery. The organic layer containing the product is reacted with

Sodium hydroxide solution.

After completion of the reaction, the pH of the mass is adjusted with hydrochloric acid. The mass is

diluted with water and centrifuged.

The wet cake is dissolved in ethyl acetate and treated with carbon. The mass is filtered and the ethyl

acetate is distilled off. The residue is cooled and centrifuged.

The mass is dried to produce KT-I.

O O

O O

N NaOH

O O

+

O OH NaO

+ +HBr

Br

N

N

Cl Cl H

Cl Cl N

Cis-Bromobenzoate Imodazole Sodium benzoate

Hydrogen Bromide

C18H15O4BrCl2 (446.12) C3H4N2 (68.07) [(2S,4R)-2-(2,4-dichlorophenyl)- C7H5O2Na (144.10) HBr (80.91)

2-(1H-imidazol-1-ylmethyl)-1,3-dioxolan-4-yl]methanol C14H14N 2O3Cl2 (329.18)

KT-II (1 a . Cis-Tosylate) KT-I is reacted with PTSC in the presence of sodium carbonate and methylene chloride as solvent.

The reaction mass is diluted and the organic layer separated. Methylene chloride is distilled off

completely from the organic layer and the residue is diluted with methanol and water.

The mass is centrifuges and washed with methanol and water mixture. The mass is dried to produce

Cis-Tosylate (KT-II)

22

KT-III

Cis-Tosylate (KT-II) is reacted with Para hydroxyl phenyl N-acetyl piperazine and sodium methoxide

in the presence of dimethyl sulfoxide as solvent.

After completion of the reaction, sodium hydroxide solution is charged into the reactor and

maintained. The mass is centrifuged.

The wet cake is treated with water and further by acetone. The wet cake is taken for next stage.

KT-IV

The wet cake is dissolved in ethyl acetate and methanol, and treated with carbon. The mass is filtered

and the solution distilled off. The residue is cooled and centrifuged. The material is dried to produce

Ketoconazole.

23

Material Balance:

Stage-I

INPUT QTY. MT OUTPUT QTY. MT

CBB 1.53 KT-I 0.88

IMD 1.36 DMF 0.07

DMF 0.07 IMD (Rec) 0.71

Toluene 3.29 Toluene (Rec) 2.94

Sodium Bicarbonate 0.29 Ethyle acetate (Rec) 3.18

Sodium hydroxide 0.24 Aq. Effluent 1.58

Water 0.40 Spent carbon 0.01

HCl 0.31 Distillation Residue 0.01

Ethyl acetate 3.35 Process loss 1.47

Carbon 0.01

Vacuum salt 0.01

0.00

Total 10.85 Total 10.85

Stage-II


KT-I 0.88 KT-II 1.18

Methylenechloride 5.61 0.00

P-toluene sulfonyl chloride 0.91 Methylenechloride (Rec) 6.27

Sodium carbonate 0.60 Methanol (Rec) 2.70

Hydrochloric acid 0.02 Distillation Residue 0.01

Methanol 2.79 Process loss 0.67


Stage-III


Cis-tosylate (kt-ii) 1.18 KT-III 1.27

Para hydroxyl phenyl n- 0.56 0.00

acetyl piperazine 0.00 Methanol 0.01

Dimethyl sulfoxide 1.66 Dimethyl sulphoxide (Rec) 1.53

Sodium methoxide powder 0.14 Acetone (Rec) 0.54

Sodium hydroxide 0.10 Aq. Effluent 0.65

Acetone 0.67 Distillation Residue 0.01

Methanol 0.01 Process loss 0.62

Water 0.32 0.00


Stage-IV


KT-III 1.27 Ketoconazole 1.00

Ethyl acetate 4.35 Ethyl acetate 4.19

Methanol 0.91 Methanol 0.85

Carbon 0.04 Spent carbon 0.04

Distillation Residue 0.02

Process loss 0.48


24

1. B CIS-BROMO BENZOATE:

Stage-I: Charge toluene, 2,4-dichloroacetophenone and glycerin onto a stainless steel reactor.

Charge PTSA and water into the reactor, and heat the mass to reflux.

Maintain the mass at reflux for 24 hours.

After completion of the reaction, cool the mass below 35°C and transfer the mass to a glass lined

reactor.

Charge n-butanol in the reactor containing the mass and cool below 15°C.

Slowly add bromine into the reactor and maintain the mass below 15°C.

After completion of the reaction, adjust the pH of the mass to 8 with liquor ammonia.

Charge water into the reactor, stir and settle.

Separate the organic layer and wash with water. Meanwhile, charge water and sodium hydroxide into

a stainless steel reactor.

Transfer the organic layer from GL reactor into the SS reactor.

Cool the mass and charge TEBAC. Add benzoyl chloride slowly into the reactor below 20°C and

maintain.

After completion of the reaction, settle the mass.

Separate the organic layer and wash with sodium bicarbonate solution followed by water.

Distill off toluene completely and dilute the residue with methanol.

Cool the mass and centrifuge. Dry the material at 60 – 65°C to produce Cis-bromo benzoate.

Chemical Reaction:

25

O

O

CH3

OH Toluene

PTSA O OH

HO

OH

+

CH3 + H2O

Cl Cl Water Cl Cl

2,4-Dichloroacetophenone Glycerin Intermediate

compound Water

C3H8 O3 (92.09)

C8H6 OCl2 (189.04)

(Not isolated) H2O (18.01)

C11 H12O3Cl2 (263.12)

O O

O OH

n-Butanol

O OH

CH3 + Br2 Liquor ammonia Br + HBr

Cl

Cl

Water

Bromine Cl

Cl

Intermediate compound Br2 (159.80) Intermediate compound Hydrobromic acid

(Not isolated)

(Not isolated)

HBr (80.91)

C11H12O3Cl2 (263.12)

C11H11O3BrCl2 (342.01)

O Cl O

O

Sodium hydroxide

O

O OH

O O

Br + TEBAC

Br

+NaCl + H2O

Cl

Water Cl

Cl Cl Sodium chloride Water

Intermediate

compound Benzoyl chlride

ClNa (58.44)

H2O (18.01)

Cis-Bromobenzoate

(Not isolated) C7H5OCl (140.56)

C18H15O4 BrCl2 (446.12)

C11H11O3 BrCl2 (342.01)

Material Balance:

Cis-Bromo benzoate

INPUT QTY.

MT OUTPUT

QTY.

MT

2,4-DCAP 0.67 Cis-Bromo benzoate 1.00

Benzoyl Chloride 0.62 Methanol (Rec) 2.07

Bromine 0.62 Toluene (Rec) 2.26

CS Flakes 0.24 Emission HBr 1.33

Glycerin 0.36 Spent solvent 0.66

Liq. Ammonia 0.50 Aqueous effluent 1.93

Methanol 2.90 Distillation Residue 0.09

N- Butanol 0.20 Process loss 0.61

PTSA 0.02

Sodium Bicarbonate 0.04

TEBAC 0.01

Toluene 2.29

Water 0.14


26

1. C N,N Bis (2-Chloroethyl) Amine Hydrochloride Stage-1

Di ethanol amine undergoes chlorination with Thionyl chloride in presence of EDC and Methanol to

give N, N, Bis (2-chloroethyl) amine Hydrochloride.

Stage-1 H

H Cl N Cl

HO N

OH+ SOCl2 + HCl

HCl

Diethanol amine Thonyl chloride 36.5 Bis(2-Chloroethyl)amine

118.97

Hydrochloride

C4H10Cl3N

C H 11

NO 2

4

105.14 178.49

+ SO2

+ H2O

64.06 18.02

Material Balance:

INPUT QTY.

MT OUTPUT

QTY.

MT

Di ethanol amine 0.60 N,N,Bis (2-Chloroethyl)

Amine Hydrochloride 1.00

Thionyl chloride 0.68 EDC Recovery 3.6

Hydrochloric acid 0.22 EDC Loss 0.08

Ammonium hydroxide 0.25 Effluent water 0.50

EDC 4.00 Process emissions(Sulphur

dioxide) 0.36



27

1. D 1-Acetyl-4(4-Hydroxy Phenyl) Piperazine

Route of Synthesis:

Stage-1

Di ethanol amine undergoes chlorination with Thionyl chloride in presence of Toluene and

Methanol to give stage-1 compound.

Stage-2

Stage-1 compound reacts with 4-Amino-phenol and Acetic anhydride to give Stage-2 compound.

Stage-3

Stage-2 compound (Tech) undergoes purification in presence of water and Methanol to give 1-Acetyl-

4-(Hydroxy Phenyl) Piperazine product.

Chemical Reaction:

28

Material Balance:

INPUT QTY.

MT OUTPUT

QTY.

MT

Di ethanol amine 0.52 Stgae-1 0.86

Thionyl chloride 0.59 Toluene Recovery 3.60

Hydrochloric acid 0.18 Toluene Loss 0.08

Ammonium hydroxide 0.25 Process emissions

(Sulphur dioxide) 0.52

Toluene 4.00 Inorganic solid waste 0.03

Sodium sulphate 0.03 Distillation Residue 0.03


INPUT QTY.

MT OUTPUT

QTY.

MT

Stage-1 0.86 Stage-2 1.05

4-Amino phenol 0.53 Acetic acid Recovery 0.29

Acetic anhydride 0.50 Inorganic solid waste 0.03

Potassium Carbonate 0.20 Process Emission 0.53

Sodium sulphate 0.03 Distillation residue 0.03


INPUT QTY.

MT OUTPUT

QTY.

MT

Stage-2 1.05 1-Acetyl-4-(Hydroxy Phenyl)

Piperazine 1.00

Methanol 5.00 Methanol Recovery 4.75

Activated Carbon 0.08 Methanol loss 0.10

Sodium sulphate 0.03 Effluent water 0.29

Water 0.24 Spent Carbon 0.08

Inorganic solid waste 0.04



29

2 . 2-Chloro Ethyl Amine Hydrochloride

Manufacturing Process:

In a dry GL fitted with a sealed mechanicals stirrer, an efficient reflux condenser, and addition flask is

placed of Thionyl Chloride and Ethylene Dichloride.

Throughout, the entire period of operation, as the reaction is very exothermic. Monoethanol amine is

added through the flask and slow addition.The cooled mass over a period of an hour, during which time

there is a copious evolution of sulfur dioxide.

After all the Diethanol amine has been added, the cooling is stop and the reaction mixture.

Chemical Reaction:

OH-CH2- CH2-NH2 + SOCl2 Cl-CH2- CH2-NH2.HCl + SO2

Monoethanolamine Thionyl Chloride 2-Chloro ethyl amine HCl Sulphur oxide

Or

Mass balance:

INPUT QTY.

MT OUTPUT

QTY.

MT

Monoethanolamine 0.63 Finish Product 1.00

Thionyl chloride 1.38 EDC Recovery 1.84

NaOH 0.16 Process Loss 0.13

EDC 1.88 EDC Loss 0.04

Inorganic Salt 0.13 0.00 HCl 25 % 0.91

TOTAL 4.03 TOTAL 4.03

NH2

OH

NaOH

EDCMONO ETHANOL AMINE

Cl

NH2

ClH

2-CHLOROETHYLAMINEHCL

+ T C

+NaSO 4

2-chloroethanam ine

EDC (Media)

30

3. Meloxicam and its intermediates:

Meloxicam Manufacturing Process:

Take toluene in SS-vessel & add required quantity of ester at room temperature then raise the

temperature to 650C & slowly.

Add 2 Amino 5 Methyl Thiazole & reflux the material at 1120C for 8 hour then cool the mass &

centrifuge to get the Meloxicam crude.

Now purify the Meloxicam crude by methanol and carbon treatment.

Chemical Reaction:

Mass Balance:

INPUT QTY.

MT OUTPUT QTY.

MT

4-Hydroxy-2-methyl-2-H (ester) 0.79 Meloxicam 1.00

2- Amino 5 Methyl Thiazole 0.31 Toluene Rec. 5.54

Toluene 6.18 Spent Carbon 0.07

Methanol 4.41 Methanol Rec 4.32

Carbon 0.07 Drying Loss 0.70

0.00 MeOH (wood Alcohol) 0.12


31

3. A 2-Amino-5-Methyl Thiozol

Process Description.

Method for synthesis of 2-amino-5-methylthiazole used as an intermediate compound in

synthesis of drugs. Method for synthesis of 2-amino-5-methylthiazole involves the following

steps: chlorination reaction of propionic aldehyde with sulfuryl chloride, successive addition of

lower alcohol and alkali aqueous solution to alkaline pH value of medium, separation of organic

phase containing 2-chloropropionic aldehyde acetal, condensation of water with thiourea.

Organic phase is added directly to thiourea in acid aqueous solution. Method provides increasing

yield of the product and to simplify the process.

CHEMICAL REACTION.

Mass balance:

INPUT QTY.

MT OUTPUT QTY.

MT

Propionic aldehyde 0.63 Finish Product 1.00

Sulfuryl chloride 1.25 Tol. Recovery 0.84

Thiouria 0.38 Tol. Loss 0.02

Water 0.41 In Organic Salt 0.15

HCL 0.16 HCl 25 % 0.13

Tolune 0.94 Aqu. Water 0.48

NaOH 0.06 Process Loss 1.19


32

3. B Methyl Benzothiazine Isopropyl Ester


1.) METHYL BENZOTHIAZINE ISOPROPYL ESTER (PROCESS)

• Check & clean reactor (S.S.R. 3000 LTR.)

• Charge DMF – 270 KG.

• Add Sodium Saccharine – 600 KG.

• Charge IPCA – 390 KG.

• Charge H2O (2000 LTR.) + NA2 CO3 (50 KG.)

• Stir for 2 hrs. At certain temp.

• Filter it water – 1100 ltr. Goes to etp.

• DMF + IPA mix goes for distillation (510 KG.)

• Wet cake dry in tray dryer (750 KG.)

• Dry Material – 660 KG.

• In Another S.S.R. Take IPA (1500 LTR.)

• Add Na Metal (75 KG.)

• Take above na metal + IPA Solution In S.S.R.

• Add dry material – 330 KG. UNDER STRING.

• Charge DMS – 255 KG. HEAT UPTO 750C

• Distilled Off – IPA – 800 LTR.

• Add Hcl – 180 LTR.

• Filter It IPA – 650 LTR. FOR DISTILLATION

• H2O + NA2SO3 510 KG GOES TO ETP.

• Crude Material (330 KG) TAKEN IN S.S.R. FOR PURIFICATION.

• Charge XYLENE (200 LTR.) CHARGE MEOH – (200 LTR.)

• Stirr for 2 hrs. FILTER IT.

• Pure material – (260 KG.) - IIND CROP ML. RECIRCULAT

33

Mass balance:

Input Qty. MT Output Qty. MT

DMF 0.38 Stage-1 0.92

IPA 0.54 Loss 0.01

Sodium Saccharine 0.83 IPA + DMF 0.90

H2O 0.17 Effluent 0.09



Stage-I 0.92 Product 1.00

IPA 1.43 0.00

Sodium Metal 0.10 IPA 1.40

Sodium Sulphate solution 0.10 Xylene 0.27

DMS 0.08 Methanol 0.27

0.00 Loss 0.13

HCl 0.06 effluent 0.09

Ice 0.07 Inorganic Salt 0.07

Xylene 0.28 Distillation residue 0.07

Methanol 0.28


34

4. Chlorzoxazone

Process Description:

Charge Urea, Acetic aci d and Hydrochloric acid with 4-Chloro-2- Amino Phenol. In the reactor and heat

upto 95 0C and maintain for 1 hr. Check TLC then centrifuge crude material at 30 0C ,then wash with

water till neutral pH .

Add Charcoal and heat to reflux for 2 hr at 55 0C Filter hot through Sparker, collect clear filtrate in

crystalliser.

Collect clear filtrate in crystalliser and keep temp 45 0C in crystalliser. W ash sparklers carbon bed with

Acetone and transfer it to crystalliser.

Add Hydrose with water then fast add DM Water 15 minutes at 70 0C. Slowly cool to 40 0C

Apply chilling and chill the material up to 10oC and maintain for 1 hrs.

Centrifuge the material a t 10 0C and collect for Acetone Recovery.

Wash the cake with D M water till chloride free, unload material and dry at 90 0C, check LOD and unload

from dryer.

Chemical Reaction:

35

Material Balance:


4-Chloro-2- Amino Phenol 0.95 Chloroxazone 1.00

Urea 0.95 Loss 1.73

Hydrochloric Acid 0.21 Effluent 0.81

Methanol 3.00 Methanol 2.94

Activated Carbon 0.11 Inorganic Salt 0.13

Sulphuric Acid 0.10 Distillation residue 0.09

Acetic Acid 0.50

Water 0.81

Sodium Hydrosulphite 0.05


36

5. 1-(2, 3 Dichlorophenyl) Piperazine Hydrochloride

Stage-1

2, 3-Dichloro-phenylamine undergoes condensation with Bis-(2-chloro-ethyl)-amine in presence of Xylene

and Acetone to give 1-(2,3-Dichloro-phenyl)piperazine Hydrochloride.

Stage-1

Cl

Cl Cl

Cl

H

Xylene,

. HCl

NH2 +

N

Acetone

N

Cl Cl

NH

2,3-Dichloro- Bis-(2-chloro-

phenylamine

ethyl)-amine

1-(2,3-Dichloro-phenyl)-piperazine

C6H5Cl2N

C4H9Cl2N

Hydrochloride

162.02 142.03 C

10H

13Cl

3N

2

267.58

+ HCl

36.46

Material Balance:


2,3-Dichlorophenylamine 0.51 Product 1.00

Bis-2(2-chloro-ethyl)-amine 0.54 Xylene Recovery 4.75

Xylene 5.00 Xylene Loss 0.10

Acetone 5.00 Acetone Recovery 4.75

Activated carbon 0.03 Acetone Loss 0.10

Water 0.28 Effluent water 0.28

Process emission 0.25

Spent carbon 0.03

Distillation residue 0.09


37

6. 1-(4-Methoxy-Phenyl)-4-(4-Nitro-Phenyl)-Piperazine Process Description:

Stage-1:

1-(4-Methoxyphenyl) Piperazine condensed with p-Nitro-1-Chloro Benzene in presence of Potassium

Carbonate to give 1-(4-Methoxy-Phenyl)-4-(4-Nitro-Phenyl)-Piperazine.

Stage-1

OCH3

NO2

N

H3CO

N

N

NO2

N

H +

+ 1/2 K2CO3 DMF

Cl

1-(4-Methoxyphenyl) p-Nitro-1- 69.0 1-(4-Methoxy-phenyl)-4-

piperazine chlorobenzene (4-nitro-phenyl)-piperazine

C11

H16

N2O

C6H4ClNO2 C17

H19

N3O

3

192.3 157.6

313.35

+ KCl + 1/2CO

2

+ 1/2

H O

2

74.55 22.0 9.0

Material Balance:


1-(4-Methoxy phenyl ) 0.63

1-(4-Methoxy-Phenyl)-4-

(4-Nitro- Phenyl)-

Piperazine

1.00

Piperazine 0.00 DMF Recovery 2.38

p-Nitro Chloro Benzene 0.51 DMF Loss 0.05

Potassium Carbonate 0.23 Effluent Water 0.25

DMF 2.50 Process Emissions(Carbon

Dioxide) 0.07

Water 0.25 Distillation Residue

0.05


38

7. N-Methyl-1-NapthaleneMethylamine Hydrochloride

Process Description:

Stage-1

Naphthalene reacts with Formalin and Hydrochloric acid in presence of phosphoric acid and

MDC to give Stage-1 compound.

Stage-2

Stage-1 compound reacts with methyl amine in presence of Toluene to give Methyl-

napthalen-1-ylmethyl-amine Hydrochloride.

N-METHYL-1-NAPTHALENEMETHYLAMINE HYDROCHLORIDE

39

Mass Balance

Input Qty.

MT Output

Qty.

MT

Naphthalene 0.64 Stgae-1 0.86

Formaline 0.15 MDC Recovery 3.92

Hydrochloric acid 0.19 MDC Loss 0.40

Phosphoric Acid 0.25 Acetic acid Recovery 2.45

MDC 4.00 Acetic acid loss 0.05

Acetic acid 2.50 Effluent water 0.34

Sodium Carbonate 0.05 Inorganic solid waste 0.20

Sodium sulpahte 0.05 (Sodium sulphate) 0.00

Water 0.34 Distillation Residue 0.05


Input Qty.

MT Output

Qty.

MT

Stage-1 0.88 N-Methyl-1-

NapthalenemethylamineHydrochloride

1.00

Methyl amine 0.16

Methanol 4.00 Methanol Recovery 3.93

Acetone 2.50 Methanol Loss 0.06

Water 0.31 Acetone Recovery 2.45

Acetone loss 0.05 Effluent water 0.28 Distillation Residue 0.04

Total 7.84 7.84

40

8. Ambroxol HCl

Process Description: Ambroxol HCl

In a clean dry GLR charge Methanol,Methyl Anthranilate, cool to 15 to 20 OC. Add Bromine

maintaining temp at 15-20 OC , maintain for 2 hrs at 15-20 OC . Add H2O2 - 50% maintaining temp

15 -20 OCand then for 3.0 Hrs at 15 -20 OC , charge water , make PH by Liq. Ammonia 25% to 7.0

to 7.50.

In a clean dry SSR Charge THF, Step I and acetic acid , add slowly sodium Borohydride at 15 -20 OC within 4-5 hrs, raise temperature to RT ,

Maintain 4 hrs at RT, distill out THF under vacuum max at 70 OC , After distillation completed

charge water , cool to Rt , Start Centrifuge And give methanol wash for each lot, Spin dry unload

& dry in tray dryer.

Charge reaction mass from step 3 & Manganese dioxide at RT .Charge EDC, Activated Carbon,

Hyflow , Stirr for 1.0 Hrs and raise temperature to 95 OC to 110 OC Start filtration & collect all ML

to another SSR, big filtration require, after filtrationcomplete give cake wash tolune , in another

SSR , Collect all ML distillate , Toluene under vacuum at 80 OC. Cooltro RT , Chill to 15 OC , Maintain

5.0 Hr at 15 OC , Centrifuge , Give methanol wash to material , spin dry , Unload cake and dry in

FBD.

In clean dry SSR charge Toluene,step 5 under stirring. Charge Trans 4-Amino Cyclohexanol,

reflux at 110 OC. Remove water through distillation, After removing water distill out Toluene

atmospherically .Cool to RT . Chill to 10 OC . Centrifuge the mass & wash with Toluene& Spin Dry

unload cake.

In Cool dry SS Reactor charge methanol. Charge Step 6 on dry basis .Chill to 10 OC and add Sodium

Borohydride at 10 -15 OC within 4 Hrs. Raise Temperature to RT for 1.0Hr.

Check TLC. If Complies Raise Temperature Refux 70- 80 OC , Maintain for 2.0 Hr. Cool to RT, Chill

to 10 OC. Start centrifuge , Spin dry unload cake..

In clean dry SS reactor charge Iso propyl Alcohol. Charge Ambroxol Base (Step 5) on dry basis.Heat

and reflux.

Check clear solution , If ok charge Act. Carbon .Filter.

Through Sparkler having Hyflow Bed & collect all Ml in GLR. In GLR collect all Ml cool.

41

Chemical Reaction:

STEP-1

Br2

+

NH3 ⇒

+

H2O2

METHANOL METHYL STEP-1 YEILD

ANTHRANILATE

STEP-2

STEP

-1

TETRA SODIUM BORO ACETIC METHAN 2-AMINO-3,5-

DIBROMOBENZALDEHY

DE

HYDROFURA HYDRIDE ACID OL

N

STEP-3

STE

HCL

P-2

+

C6H14O3 MNO2

⇒

NH3

ACETO TRANS-4-AMINO AMBROXOL

NE CYCLOHEXOL

42

Material Balance:

Input Qty.

MT Output

Qty.

MT

Methanol 3.41 Recovered Methnaol 3.24

Methyl Anthranilate 0.54 Ml To Etp 1.40

Bromine 0.63 Loss Methanol 0.17

Liq. Ammonia 0.15 Step I Output 1.02

Hydrogen Peroxide 0.20

Water 0.90


Step 2

Input Qty.

MT Output

Qty.

MT

Step I 1.02 Recovered THF 1.66

Thf 1.78 Loss THF 0.12

Sodium Boro Hydride 0.12 Effluent 0.66

Acetic Acid 0.02 Step II Output 0.87

Water 0.36


STEP 3

Input Qty.

MT Output

Qty.

MT

STEP II 0.87 Recovered Toluene 4.58

Toluene 5.21 Loss Toluene 0.64

Charcoal 0.04 Effluent 0.36

Manganese Dioxide 1.93 Spent Carbon 0.05

Water 0.36 Step III Output 0.73

Solid Waste of MnO2 2.05


43

Step 4

Input Qty.

MT Output

Qty.

MT

Step 3 0.73 Recovered Toluene 2.39

Toluene 2.51 Los Toluene 0.13

Sodium Borohydride 0.10 Solid Waste 0.06

Trans 4-Amino

Cyclohexanol 0.29 Step IV Output 1.06


Step 5

STEP IV 1.06 Recovered IPA 3.07

IPA 3.23 Loss IPA 0.16

Act Carbon 0.01 Process Loss 0.21

HCL 0.24 Spent Carbon 0.01

Output Step V 1.00



44

9. 1-[2-(2-Hydroxyethoxy)ethyl]piperazine


Piperazine monohydrochloride prepared with 2- (2-chloroethoxy) ethanol in was added the

reaction solvent, wherein the piperazine monohydrochloride and 2- (2- The molar ratio of

added-chloroethoxy) ethanol was (piperazine 2- (2-chloroethoxy) ethanolthe use of a polar

solvent such as ethanol solvent.

An amount of ethanol is added, in a weight ratio of g / g operator, is 2- (2-chloroethoxy)

ethanol added in an amount of 2.4 times; stirring warmed to 40 ° C; in at this temperature for

2 hours.

After completion of the reaction, distillation under reduced pressure below 600C to remove

about half of the ethanol 30 g, cooled to 150C, filtered , and the filter cake was washed with

a small amount of ethanol is piperazine dihydrochloride, 500C 7 hours drying after recyclabe.

The filtrate was filtered slowly heated to 90 ° C, the0020methanol was removed in vacuo and

the residue was distilled under reduced pressure after the high purity piperazine 1- [2- (2_-

hydroxyethoxy) ethyl] piperazine (HEEP) crude.

To give 1- [2- (2_-hydroxyethoxy) ethyl] piperazine (HEEP) crude vacuum distillation in

vacuum.

Chemical Reaction:

NH

NH

+Cl

OOH

N

NH

OOH

Na OH

water

piperazine

M.F.= C4H10N2

M.W = 86.13

2-(2-chloroethoxy)ethanol

M.F = C4H9ClO2

M.W.= 124.56

2-[2-(piperazin-1-yl)ethoxy]ethanol

M.F.= C8H18N2O2

M.W.= 174.24

M.W.= 39.99

+ Na Cl + OH2

M.W= 58.44

Mass Balance:

Input Output

Piperazine 0.77

1- [2- (2_-

hydroxyethoxy) ethyl]

piperazine

1.00

2- (2-chloroethoxy) ethanol 0.38 Methanol 0.40

water 0.13 Waste water 0.13

Sodium hydroxide 0.28 Drying loss 0.44

Methanol 0.41 Distillation Residue 0.01

Solvent loss 0.005


45

10. 2,4‐Dichloroacetophenone


In glass lined reactor1,3-dichloro benzene and aluminium chloride was mixed and then

acetyl chloride was added to it at 15-200C. Whole mixture was refluxed overnight.

Generated hydrochloric acid gas was scrubbed by water.

After completion of reaction whole mixture was dumped in to water then organic layer

was separated and excess benzene was removed by simple distillation and 2,4-

dichloroacetophenone was distilled by vacume distillation.

Chemical Reaction:

Mass Balance:

INPUT QTY (kg) OUTPUT QTY (kg)

1,3-dichloro benzene 0.78 Finish Product 1.00

Aluminium chloride 0.71 30% HCL solution 0.63

acetyl chloride 0.42 25% Aluminium sol. 1.28



46

11. 2,4‐Dichlorovelrophenone


In glass lined reactor1,3-dichloro benzene and aluminium chloride was mixed and then

n-veratyl chloride was added to it at 15-200C. Whole mixture was refluxed overnight.

Generated hydrochloric acid gas was scrubbed by water.

After completion of reaction whole mixture was dumped in to water then organic layer

was separated and excess benzene was removed by simple distillation and 2,4-

dichloroacetophenone was distilled by vacume distillation.

Chemical Reaction:

Mass Balance:

INPUT QTY (kg) OUTPUT QTY (kg)

1,3-dichloro benzene 0.78 Finish Product 1.00

Aluminium chloride 0.71 30% HCL solution 0.63

n- veratroil chloride 0.42 25% Aluminium sol. 1.28



47

12. 1‐(3‐Chlorophenyl)Piperazine

Process Description

Into reactor, charge 745 Kg water, 305 Kg 3-chloroaniline, 427 Kg Bis (2-Chloroethyl)

amine hydrochloride and 287 Kg sodium hydroxide at room temperature. Take

temperature 90 °C within 15 hours. Monitor the reaction performance by analytical

method. After completion of reaction cool to 35 °C and add 916 lit Toluene at 35 °C in 2

hrs. Stirr for 1 hrs and filter the sodium chloride (inorganic salts) slurry and collect the

filtrate separately. Separate organic layer and take for the solvent recovery. After solvent

recovery finally apply full vacuum to distill final product 1-(3-Chlorophenyl) piperazine.

Mass Balance:

Input Quantity Output Quantity

3-Chloroaniline 0.76 1-(3-Chlorophenyl)Piperazine 1.00

Bis-(2-Chloroethyl)Aminehydrochloride 1.07 Process Loss 0.09

Sodium Hydroxide 0.72 Effluent 3.23

Toluene 2.29 Recovered Toluene 2.08

Water 1.86 Toluene Loss 0.22

0.00 Distillation Residue 0.09


48

13. 1‐[2‐(2‐Hydroxyethyl)Ethoxy]Piperazine

Process Description

Into reactor, charge 818 Kg Water and 495 Kg piperazine at room temperature. Add 238

kg 2� chloroethoxyethanol at 60 °C in 180 minutes. Stir for 12 hrs at 70 °C and monitor the

reaction performance by analytical method. After completion of reaction, add 77 kg

sodium hydroxide and 715 lit methanol and stirr for 3 hours. Filter the inorganic solid.

Distilled out methanol, water, excess piperazine and finally product under high

vaccum.

Mass Balance:


2-Chloroethoxyethanol 0.79 1-[2-(2-Hydroxyethyl)Ethoxy]-Piperazine 1.00

Piperazine 1.65 Recovered Piperazine 1.10

Water 2.73 Effluent 3.22

Sodium Hydroxide 0.26 Recovered Methanol 2.30

Methanol 2.38 Methanol Loss 0.08


Process Loss 0.03


49

14. 1‐(3‐Chloropropyl)‐4‐(3‐Chlorophenyl)Piperazine Hydrochloride

Process Description

Charge 414 Kg 1�(3�Chlorophenyl) piperazine, 829 kg water and 84 kg sodium hydroxide at

room temperature into clean reactor. Add 1�Bromo�3�chloropropane 332 kg in 2 hrs at 30�40°C.

Raise the temperature up to 70 deg C. Monitor the reaction performance by analytical methods.

After completion of reaction, cool the mass to 25 to 30 °C and add toluene 1657 lit, filter the inorganic

product (sodium bromide). From the filtrate separate organic layer and distilled toluene under

vacuum. After distillation of toluene, add 1243 lit Isopropanol and conc. HCl (30%) 256 kg under

cooling. Cool to 15 °C. Centrifuge the product and dry the product under vacuum. Filtrate taken for

the solvent recovery. Unload and dry the material at 45 to 50°C in vacuum tray drier (VTD) till to reach

the required LOD (Loss on Drying) of the product. Expected weight is 245 Kg.

Chemical Reaction:

Mass Balance:


1-(3-Chlorophenyl)piperazine 0.69

1-(3-Chloropropyl)-4-(3-

chloroph-enyl)piperazine

HCl 98 %

1.00

1-Bromo-3-chloropropane 0.55 Sodium bromide 0.36


Sodium hydroxide 0.14 Recovered toluene 2.49

Conc. HCl (30%) 0.43 Toluene Loss 0.28

Isopropyl alcohol 2.07 Recovered IPA 1.86

Toluene 2.76 IPA Loss 0.21 0.00 Distillation Residue 0.09 0.00 0.00


50

15. 1�(2�Methoxyphenyl) Piperazine Hydrochloride

Process Description

Into reactor, charge 313 Kg water, 127 Kg o�anisidine, 184 Kg Bis(2�Chloroethyl)amine

hydrochloride and 123 Kg sodium hydroxide at room temperature. Take temperature 90 °C within

15 hours. Monitor the reaction performance by analytical method. After completion of reaction cool

to 35 °C and add 916 lit Toluene at 35 °C in 2 hrs. Stirr for 1 hrs and filter the sodium chloride

(inorganic salts) slurry and collect the filtrate separately. Separate organic layer and take for the solvent

recovery. After solvent recovery add isopropyl alcohol 380 lit, and IPA.HCl 171 kg under cooling.

Stirr for 3 hours. Centrifuge the product and dry the product under vacuum. Filtrate taken for the

solvent recovery. Unload and dry the material at 45 to 50°C in vacuum tray drier (VTD) till to reach the

required LOD (Loss on Drying) of the product. Expected weight is 200 Kg.

Chemical Reaction:

Mass Balance:


o-Anisidine 0.64

1-(2-

Methoxyphenyl)piperazine

HCl

1.00

Bis(2-Chloroethyl)amine Hydrochloride 0.92 Process loss 0.72


Sodium hydroxide 0.62 Recovered toluene 1.70

Toluene 1.90 Toluene loss 0.20

IPA.HCl 0.86 Recovered IPA 2.40

Isopropyl alcohol 1.90 Isopropyl alcohol Loss 0.17



51

ANNEXURE-IV

DETAILS OF WATER CONSUMPTION, WASTEWATER GENERATION AND TREATMENT

WATER CONSUMPATION

Sr. No. Category Water Consumption Remarks

(KL/Day) Source

1 Domestic 2.0 GIDC Water Supply Authority

2 Gardening 2.0

3 Industrial

Process 4.0

(1-[2-(2-Hydroxyethyl)

Ethoxy]Piperazine)

Boiler 15.0

Cooling 1.0

Washing 1.0

Scrubbing 2.8

3 Total Industrial 23.8

Total (1+2+3) 27.8

WASTEWATER GENERATION

Sr. No. Category

Waste Water

generation Remarks

(KL/Day) Mode of discharge

1 Domestic 1.6 Septic Tank & Soak pit

2 Gardening Nil

3 Industrial

Process 4.0

1-(3-Chlorophenyl)

Piperazine

Boiler 0.4

Cooling 0.2

Washing 1.0

Scrubbing 2.8

0.9 KLD HCl in ETP

0.7 KLD NaHSO3 Sell to End User

0.7 KLD Liq. Ammonia Reuse with premise

0.5 NaBr Sell to End User

3 Total Industrial 8.4

Total (1+2+3) 10

NOTE:

� Domestic wastewater will be discharged through Septic Tank/ Soak Pit System.

� Total industrial waste [email protected] KLD will be sent to Common Evaporation Facility

(M/s BEIL, Ankleshwar)

� Solvent Stripper 0.06 KLD (1.5%) Recovery from process wastewater.

52

PROPOSED WATER BALANCE DIAGRAM:

Source: GIDC Water Authority

Water: 27.8 KL/Day

Dom: 2.0 KL/Day

Process

4.0 KL/Day

Boiler

15 KL/Day

Cooling

1.0 KL/Day

Septic Tank & Soak

Pit: 1.6 KL/Day

Ind.: 23.8 KLD Green Belt: 2.0 KL/Day

Washing

1.0 KL/Day

6.44 KLD ETP

(Primary Treatment)

Scrubbing

2.8 KL/Day

3.94 1.0

1.9

NaHSO3

0.7 KLD

Liq.

Ammonia

0.7 KLD

NaBr

0.5 KLD

0.2 0.4

Common MEE

0.9 HCl

8-10%

Solvent

Stripper (1.5%)

0.06 KLD

53

ANNEXURE-V

DEAILS OF PROPOESD EFFLUENT TREATMENT PLANT

DETAILS OF EFFLUENT TREATMENT PLANT

Process Description of Effluent Treatment Plant

The details of ETP are as follows.

Wastewater shall be collected in Equalization cum Neutralization Tank (ENT-01) where the

continuous addition and stirring of Caustic solution is done to maintain neutral pH of

wastewater from Caustic Dosing Tank (CDT-01) as per requirement by gravity into ENT-01 to

neutral effluent by using a Flash Mixer.

Then after, neutralized wastewater shall be pumped to Primary Settling tank (PST-01. Alum

and Polyelectrolyte shall be dosed from Alum Dosing Tank (ADT-01) and Polyelectrolyte

Dosing Tank (PDT-01) respectively by gravity into PST-01 to carry out coagulation by using a

Mixer.

Then Clear supernatant from PTS-01 shall be collected in treated effluent Sump (TES-01)

before sent to common MEE of M/s. BEIL Ankleshwar for further treatment and Disposal.

Sludge settled in PST-01 shall be sent to Filter Press (FP-01), dewatering shall be carried out

before storage in HWSA and ultimate disposal to TSDF. Leachate from FP-01 shall be sent back

to ENT-01 for further treatment

SIZE OF TANKS

S.N. Name of unit Size (m x m x m) No

.

MOC/

Remark

Retention

Time

FLOW: 0.259 KL/Hr

1 Equalization cum Neutralization Tank

(ENT-01) 2.0 x 2.0 x (1.0+0.5 F.B.) 1 RCC M25

24 hr

2 Primary Settling Tank (PST-01) 1.1 x 1.1 x 1.1 1 MSFRP 5 hr

3 Filter Press (FP-01) 5 KLD 1 PP+MS

4 Collection Tank (CT-01) 2.0 x 2.0 x 1.5 1 RCC M25 24 hr

RCC M25 = REINFORCED CEMENT CONCRETE (M 25 GRADE)

PP = POLYPROPELENE

54

ETP FLOW DIAGRAM

55

PRODUCT WISE EXPECTED CHARACTERISTICS OF WASTE WATER

SR.

No. Parameter Unit

Product Wise Characteristics

Ketoconazole Ketoconazole A

(Intermediate)

Ketoconazole B

(Intermediate)

Ketoconazole C

(Intermediate)

Ketoconazole D

(Intermediate)

Quantity (KLD) 1.90 0.88 1.95 0.35 0.29

1 pH pH Unit 8-10 8-10 6-8 8-10 8-10

2 TSS mg/L 150 150 250 200 250

3 TDS mg/L 25984 15788 16468 15446 25448

4 BOD mg/L 20487 20578 15478 20489 22478

5 COD mg/L 70450 68794 50468 64750 70456

6 Ammo.

Nitrogen mg/L Nil Nil 150 100 150

SR.

No. Parameter Unit


Meloxicam A

(Intermediate)

Meloxicam B

(Intermediate) Chloroxazone

Aripiprazole {1-

(2, 3

Dichlorophenyl)

Piperazine

Hydrochloride }

1-(4-Methoxy-

Phenyl)-4-(4-

Nitro-Phenyl)-

Piperazine

N-Methyl-1-

Napthalene

methylamin

eHydrochlor

ide

Ambroxol

HCL

1-[2-(2-

Hydroxyetho

xy)ethyl]pipe

razine

Quantity (KLD) 0.47 0.21 0.95 0.32 0.29 0.72 2.82 0.16

1 pH pH Unit 8-10 6-8 8-10 8-10 3-5 8-10 3-5 6-8

2 TSS mg/L 175 205 150 150 250 150 250 150

3 TDS mg/L 24800 25400 24654 25984 8458 15788 8458 24658

4 BOD mg/L 19285 21570 20549 20487 10248 20578 10248 21556

5 COD mg/L 69720 59655 55457 70298 35425 68794 35425 68689

6 Ammo.

Nitrogen mg/L Nil Nil Nil Nil Nil Nil 100 Nil

56

SR. No. Parameter Unit


1-(3-


1-[2-(2-

Hydroxyethyl)Ethoxy]Piper

azine



Hydrochloride

1-(2-Methoxyphenyl)

Piperazine Hydrochloride

Quantity (KLD) 4.0 3.76 2.04 3.21

1 pH pH Unit 8-10 8-10 6-8 8-10

2 TSS mg/L 150 150 250 200

3 TDS mg/L 25984 15788 16468 15446

4 BOD mg/L 20487 20578 15478 20489

5 COD mg/L 70898 68794 50468 64750

6 Ammo.

Nitrogen mg/L Nil Nil 200 150

SR.

No. Parameter Unit

Stream from other utilities

Characteristics Worst Case from Process

Worst Case from Process(

After Solvent Stripper) Composite

Effluent

After Primary

treatment Boiler Cooling Washing

1-(3-


1-(3-


Quantity (KLD) 0.4 0.2 1.0 4.0 3.92 6.42 6.42

1 pH pH Unit 6-8 6-8 6-8 8-10 8-10 6-8 6-8

2 TSS mg/L 56 87 150 150 150 150 50

3 TDS mg/L 2100 2500 4588 25984 25984 15900 20500

4 BOD mg/L <50 <80 800 20487 17875 11300 6550

5 COD mg/L <100 <250 2500 70898 40500 39500 11500

6 Ammo.

Nitrogen mg/L Nil Nil Nil Nil Nil

<25

(1-(2-

Methoxyphenyl)

Piperazine

Hydrochloride)

<25

57

ANNEXURE-VI

DETAILS OF HAZARDOUS WASTE GENERATION, HANDLING & DISPOSAL

SR.

NO

TYPE OF

HAZ.WASTE SOURCE

CATEGORY

&

SCHEDULE

QTY.

MT/Annum MODE OF DISPOSAL

1 Used oil Maintenance Activities 5.1/SCH-I 0.500

Collection, Storage,

Transportation & Disposal by

selling to Authorised re-refiners

2 Inorganic Salt

Mfg. Process

Meloxiam A- (2-Amino-5-

Methyl Thiozol)

28.1/SCH-I 63.00


Transportation & Disposal at

TSDF OR sent to cement

industries for as Gypsum.

3 ETP Sludge ETP 35.3/SCH-I 36.00


Transportation & Disposal at

TSDF.

4 Spent Carbon Purification of product 28.3/SCH-I 4.00 Collection, Storage,

Transportation & Disposal by

selling to cement industries for

co-processing OR

by incineration at CHWIF.

5 Distillation residue Spent solvent distillation 36.1/SCH-I 38.00

6 Spent Solvent

Mfg. Process

(Ketoconazole 1A-Cis-

Tosylate) 28.6/SCH-I

10232.00


Transportation & subjected to

distillation assembly to recover

the solvent & Reuse within

premise. Solvent Stripper 22

7

Discarded,

containers, barrels,

Liners, plastic Bags

Material Handling and

Storage 33.1/SCH-I 2.5


Transportation & Sell to

Authorised Recyclers ( under

Rule-9)

8 Liquor Ammonia

Solution (22-25%)

Scrubber

(Ketoconazole -Inter- CIS

Bromo Benzoate)

28.1/SCH-I 274.08 KL

Collection, Storage & Reuse in

Mfg. Process of Cis-Bromo

benzoate (210.0 KL/year) and

Ambroxol HCl (64.08 KL/Year)

9 HCl solution

(8-10%)

Scrubber

Mfg. Process

(2-Chloro Ethyl Amine

Hydrochloride)

28.1/SCH-I 330.0 KL

Collection, Storage and allow for

Neutralization in ETP.

10 Sodium Bisulphite

Solution (22-25%)

Scrubber

28.1/SCH-I 250.0 KL


Transportation & Sell to end

users having permission Rule-9

11 Dilute NaBr

Solution (20-22%)

Scrubber

(1-(3-Chloropropyl)-4-(3-


Hydrochloride)

28.1/SCH-I 183.0 KL

12 Manganese

Dioxide(MnO2)

Mfg. Process

(Ambroxol HCL) 28.1/SCH-I 863.0

13

Aluminum Soln.

(20-25%)

Mfg. Process

2,4-Dichloro

Acetophenone

28.1/SCH-I 536.0 KL

58

ANNEXURE-VII

DETAILS OF STACK AND VENTS

FLUE GAS EMMISION

PROCESS GAS EMISSION

SR.NO. VENT

ATTACHED TO

HEIGHT

FROM

GROUND

LEVEL

DIAMETER EXPECTED

POLLUTANTS

AIR POLLUTION

CONTROL SYSTEM

1 Reaction vessel

(Bromination) 11 m 0.2 HBr < 30 mg/Nm3

Two Stage Alkali

Scrubber

2 Reaction vessel

(Chlorination) 11 m 0.2 HCl < 20 mg/Nm3

Two Stage Water

Scrubber

3 Reaction vessel

(Sulfonation) 11 m 0.2 SO2 < 40 mg/Nm3

Two Stage Alkali

Scrubber

4 Reaction vessel 11m 0.2 NH3 < 175

mg/Nm3

Two Stage Water

Scrubber

Fugitive emission details with its mitigation measures.

- Whole process will be carried out in close loop.

- Pipe line will be having minimum flange.

- Pump with double mechanical seals

- Proper ventilation.

VOC emission sources and its mitigation measures

Sources - Charging Materials

Measures

- Enclose Process

- Minimum flanges & joints

- Handled by pump with double mechanical seals

- Proper Ventilation

- Adequate PPEs

Sr.

No.

Stack attached

to

Stack

Height

(Meter)

Fuel Consumption APCM Concentration of

Pollutants

1. Boiler

(2 TPH) 15

Bio Coal/

Briquette/ Coal

7 MT/Day

or

Natural Gas

3600 SCM/Day

MCS& Bag Filter

&

Adequate Stack

Height

PM < 150 mg/Nm3

SOX<100 ppm

NOX<50 ppm 2.

Thermo pack

(2LKC/Hr.) 15

Bio Coal/

Briquette/Coal

1.5 MT/Day

or

Natural Gas

800 SCM/Day

MCS& Bag Filter

&

Adequate Stack

Height

3.

DG Set

125 KVA

(Stand by)

9 Diesel = 20 lit/Hr. Adequate

Stack height

59

ANNEXURE-VIII

STORAGE DETAILS OF HAZARDOUS CHEMICALS

Sr.

No.

Name of

Material

Max. Quantity to

be stored (MT)

Max.

storage

Capacity

Storage Condition

DRUM

1 Methanol 1.0 200 Lit x 5 ATP

2 Toluene 1.0 200 Lit x 5 ATP

3 Acetone 1.0 200 Lit x 5 ATP

4 IPA 1.0 200 Lit x 5 ATP

5 Phosphoric Acid 1.0 200 Lit x 5 ATP

6 Ethyl acetate 1.0 200 Lit x 5 ATP

7 Xylene 1.0 200 Lit x 5 ATP

8 Ethylene

Dichloride 1.0 200 Lit x 5 ATP

9 Hydrogen

Peroxide 0.500

Carbous

50 Lit x 10 ATP

10 Dimethyl

sulfoxide 1.0 200 Lit x 5 ATP

TANK

11 Hydrochloric

Acid (HDPE) 2.0 KL - ATP

12 Caustic Lye

(HDPE) 2.0 KL - ATP

13 Liq. Ammonia 1.0 KL - ATP

14 Sulphuric Acid 2.0 KL - ATP

Bottle

15 Bromine 50 Box

(1 Box = 18 liters) - ATP

60

Properties of Hazardous Chemicals

SR.

NO. RAW MATLS State

FP

deg C

BP

deg C LEL% UEL%

SP.GR.

20 deg C

VD

vs air

V.P

kPa

LD50

mg/kgs

Oral

LC 50

ppm

IDLH

ppm

TLV Antidotes

STEL

TWA

1 Methanol Liquid 12-16 64.5 6 36.5 0.7915 1.11 12.3 5628

[Rat] 64000 6000 250 ppm

260

mg/m3

Oxygen, Ethanol, Novasine Eye

Drops

2 Toluene Lquid 6 110.6 1.1 7.1 0.8636 3.1 3.8 636

[Rat] 49000 500 200 ppm

300

ppm

Milk of Magnesia, Oxygen,

Novasine Eye Drops

3 Acetone Liquid -9 56.2 2.6 12.8 0.79 2.0 24 5800 50100 2500 750 500

The cyanide antidote kit first

uses a small inhaled dose of

amyl nitrite followed by

intravenous sodium nitrite

4 IPA Liquid -24 82.5 2 12.7 0.84 2.07 4.4 5045 - 2000 1230 983 Medical attention immediately

5 Phosphoric

Acid

Liquid - 300 - - 2.0 - 0 - - 250 3 ppm 1 ppm -

6 Ethyl acetate Liquid 7.2 77 2.2 9 0.902 3.04 12.4 5620 45000 2000 - 400 Medical attention immediately

7 Xylene Liquid 27 139.5 1 7 0.870 3.7 1 2000 6350 900 150 100

8 Ethylene

Dichloride Liquid 13 84 6.2 16 3.4 81.3 2000 1000 50 2 1

9 Hydrochloric

Acid Liquid 11 57 - - 1.16 1.26 16

900

(rabbit) 1108 50

5

ppm

8

mg/m3

Eno, Milk of Magnesia, Cordinol

Tab, Eye Drops

10 CS Lye Solid - 1388 - - 2.13 - - - - 10

mg/m3 -

2

mg/m3

-

11 Liq. Ammonia Liquid - 36 15 28 0.826 - 857.3 350 2000 300 35 25

12 Sulphuric Acid Liquid - 290 - - 1.84 3.4 - 2140 510 19.94 3

mg/m3

1

mg/m3

-

13 Hydrogen

Peroxide

Liquid -33 108 - - 1.13 - 23 2000 2160 75 1 ppm 2 ppm -

14 Dimethyl

sulfoxide

Liquid 87 189 2.6 42 0.847 2.7 59.4 14500 5330 - - 250

-

15 Bromine Liquid -7.2 58.8 - - - 7.14 2600 2700 3 0.2 ppm 0.1 ppm

61

ANNEXURE-IX

GIDC PLOT ALLOTMENT LETTER

62

63

ANNEXURE-X

MEMBERSHIP OF COMMON MEE, TSDF AND CHWIF

64

ANNEXURE-XI

TOPO SHEET

65

ANNEXURE-XII

GIDC WATER SUPPLY LETTER

66

ANNEXURE-XIII

DETAILS OF SOLVENT RECOVERY AND REUSE

Sr.

No. Product

Spent

Solvent B.P. °C

Qty./

Month

Reuse /

Recovered Loss

%

Recovery

1

Ketoconazole

DMF 153 2.55 2.3 0.25 90.20

IMD 256 47.56 39 8.56 82.00

Ethyle

acetate 77.1 269.46 258.68 10.78 96.00

Toluene 110 115.03 103.5 11.53 89.98

MDC 39.6 269.43 261.34 8.09 97.00

Methanol 64.7 130.12 124.92 5.2 96.00

Dimethyl

sulphoxide 189 58.13 53.46 4.67 91.97

Acetone 56 23.33 22.63 0.7 97.00

1A Ketoconazole A

IMD 256 40.43 33.15 7.28 81.99

Ethyle

acetate 77.1 99.54 95.6 3.94 96.04

Toluene 110 97.77 87.99 9.78 90.00

MDC 39.6 166.8 161.79 5.01 97.00

Methanol 64.7 83.13 79.8 3.33 95.99

1B Ketoconazole B Toluene 110 80.3 72.27 8.03 90.00

Methanol 64.7 101.4 97.34 4.06 96.00

1C Ketoconazole C Toluene 110 140 126 14 90.00

1D Ketoconazole D Toluene 110 140 126 14 90.00

Methanol 64.7 175 168 7 96.00

2 2-Chloro Ethyl Amine

Hydrochloride EDC 83.47 65.63 63 2.63 95.99

3 Meloxicam Toluene 110 216.18 194.56 21.62 90.00

Methanol 64.7 154.41 148.23 6.18 96.00

3A Meloxicam A Toluene 110 32.81 29.52 3.29 89.97

3B Meloxicam B

DMF 153 13.1 11.79 1.31 90.00

xylene 138.4 9.7 8.73 0.97 90.00

Methanol 64.7 9.7 9.31 0.39 95.98

IPA 82.5 69 66.24 2.76 96.00

4 Chloroxazone Methanol 64.7 105 100.8 4.2 96.00

5

Aripiprazole {1-(2, 3

Dichlorophenyl)


}

Xylene 138.4 175 157.5 17.5 90.00

Acetone 56 175 169.75 5.25 97.00

6

1-(4-Methoxy-Phenyl)-4-

(4-Nitro-Phenyl)-

Piperazine

DMF 153 87.5 78.75 8.75 90.00

7

N-Methyl-1-

Napthalenemethylamineh

ydrochloride

Methanol 64.7 140 134.4 5.6 96.00

Acetone 56 87.5 84.87 2.63 96.99

Acetic Acid 118.1 87.5 84 3.5 96.00

MDC 39.6 140 135.8 4.2 97.00

8 Ambroxol HCl Toluene 110 270.45 243.4 27.05 90.00

67

Methanol 64.7 119.39 114.61 4.78 96.00

THF 66 62.33 59.84 2.49 96.01

IPA 82.5 113.11 108.58 4.53 96.00

9

1-[2-(2-

Hydroxyethoxy)Ethyl]Pipe

razine

Methanol 64.7 14.5 13.92 0.58 96.00

12 1-(3-

Chlorophenyl)Piperazine Toluene 110 80.15 72.13 8.02 89.99

13

1-[2-(2-

Hydroxyethyl)Ethoxy]Pipe

razine

Methanol 64.7 83.42 80.08 3.34 96.00

14



Hydrochloride

IPA 82.5 72.51 69.61 2.9 96.00

Toluene 110 96.66 86.98 9.68 89.99

15 1-(2-Methoxyphenyl)


Toluene 110 66.5 59.85 6.65 90.00

IPA 82.5 66.5 63.84 2.66 96.00

68

ANNEXURE-XIV

DETAILS OF PROJECT COST AND EMS BUDGET

Estimated Project Cost

Total Project Cost for project activity is Rs. 400 Lakhs.

Details Approximate Capital Cost

(Rs. in Lacs)

Land 37.0

Building 110.0

Plant & Machinery 200.0

ETP, APCS & HWM 50.0

Green Belt Development 1.00

Occupational Health 2.00

Total 400.00

EMS Budget

Sr.

No. Item

Capital Cost

in Lakhs

Recurring Cost in

lakhs/Annum

1 Air Act

Air Pollution Control Equipment/Chimney 30 2.0

Operation & Maintenance 1.0

Total 30 3.0

2 Water

Act

Primary Treatment Facility 3 2.5

Treatment Charges of CMEE 0.50 60

Total 3.5 62.5

3

Haz

Waste

Rule

Membership Fees for TSDF facility 0.5 NIL

Haz Waste Transportation NIL 2.0

Disposal Charges NIL 8.0

Membership Fees for Incineration Facility 0.5 NIL

Incineration Charges NIL 40.0

Total 1.0 50.0

4 AWH Environmental Monitoring expenses 1.5 0.10

5 OH &

Safety

Environment & Safety training

Fire Fighting,

PPEs,

Other Risk Minimise Action

2.0 1.00

6 Green

Belt Greenbelt development 1.0 2.0

Total 39.0 118.6

69

ANNEXURE-XV

HON’BLE NGT ORDER FOR CRITICALLY POLLUTED AREA & ITS COMPLIANCE BY CPCB

Compliance of Hon’ble NGT Order by CPCB

70

71

72

73

74

75

76

77

78

79

80

81

LIST OF ANNEXURESenvironmentclearance.nic.in/writereaddata/Online/TOR/26_Oct_2019_185545677DUCW4LCS...11 list of annexures sr. no. name of annexure i list of products with their production

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