Revised Form-1 Finalenvironmentclearance.nic.in/writereaddata/Online/... · Charge Hydantoin,...

ADDITIONAL ATTACHMENT

LIST OF PRODUCTS

S.

No. Name of Products

Production Capacity (MT/Month)

Existing Proposed Total

1. Sodium Silico Fluoride 300 - 69 231

2. Alpha Keto Isoleucine Calcium Salt - 3.0 3.0

3. Alpha Keto Leucine Calcium Salt. - 3.0 3.0

4. Alpha Keto Phenylalanine Calcium Salt. - 3.0 3.0

5. Alpha Keto Valine Calcium Salt. - 3.0 3.0

6. Alpha Hydroxy Methionine Calcium Salt. - 3.0 3.0

7. Iron Sucrose - 2.0 2.0

8. Phenyl Acetic Acid - 40.0 40.0

9. Diacerein - 3.0 3.0

10. Tolfenamic Acid - 2.0 2.0

11. Diosmin - 3.0 3.0

12. T.P.O - 10.0 10.0

13. Ferric carboxy Maltose - 1.0 1.0

14. Sucroferric oxyhydroxide - 5.0 5.0

15. Couple Amines - 2.0 2.0

Total 300 14 314

By-Products

1. Acetic Acid - 36.29 36.29

2. Methyl Iodide - 1.29 1.29

DETAILS OF MANUFACTURING PROCESSES

EXISTING

1. SODIUM SILICO FLUORIDE

Manufacturing Process Charge Hydro Fluoro Silicic Acid in a rubber lined reactor. Charge soda ash and sodium chloride

in to reactor to precipitate Sodium Silico Fluoride. The precipitate is then centrifuged and washed

with water to remove hydrochloric acid completely. The filtrate containing about 1% to 3% HCL is

collected in the storage tank of ETP.The neutralized and washed precipitate is dried or keeps wet as

per requirement. Then the product is packed in HDPE/PP bags.

Chemical reaction

H2SiF6 + Na2Co3 Na2SiF6 + H2O + CO2

(144.08) (106) (188.08) (18) (44)

H2SiF6 + 2 NaCl Na2SiF6 + 2 HCl

(144.08) (117) (188.08) (73)

Process Flow Diagram

Material Balance

Input Qty.

Output Qty

HFS Acid 4.33

Supernatant to ETP 0.25

Sodium Carbonate 0.08

Effluent to ETP 7.15

Sodium Chloride 0.59

Product 1

Water 3.4

8.4

8.4

PROPOSED

2. ALPHA KETO ISOLEUCINE CALCIUM SALT

Manufacturing Process Charge Hydantoin, Monoethanol amine and Methyl ethyl ketone in a SS Reactor, Heat the reaction

mass up to reflux and completely distill out methyl ethyl ketone and reuse for next batch. Cool the

reaction mass and charge DM water and sodium Hydroxide. Adjust the pH to 6-7 with hydrochloric

acid and charge calcium chloride in to SS reactor. Heat the reaction mass up to reflux. Distill out

water and cool the reaction mass. Filter the isolated solid and dry it, mill it and blend. Pack the

material in paper drums.

Chemical reaction

REACTOR

CENTRIFUGE

REACTOR

TRAY DRYER

SODIUM SILICO

FLUORIDE

CENTRIFUGE

HFS Acid

Sodium Carbonate

Sodium Chloride

Water

Supernatant to

ETP

Effluent to ETP

Effluent to ETP

Product


Material Balance

Input Qty. Output Qty

Hydantoin 1.43 MEK Distillation 2.29

Methyl Ethyl Ketone 2.3 ML to ETP 8.74

Ethanol Amine 0.87 Ditilled water for

boiler 8.57

DM water 11.83 Washing Solvent 0.7

Sodium Hydroxide 1.1 Drying Loss 0.14

Hydrochloric acid 2.07 Product 1

Calcium Chloride 1.13

MeOH Washing 0.71

21.44 21.44

3. ALPHA KETO LEUCINE CALCIUM SALT

Manufacturing Process Charge DM water and sodium hydroxide in the reactor under stirring. Charge Hydantoin, Glycine

and Isobutyraldehyde. Heat to reflux, maintain till reaction will be completed. Distil out

Isobutyraldehyde completely and reuse for next batch. Cool the reaction mass and charge DM water

and sodium Hydroxide. Adjust the pH 6 to 7 with Hydrochloric acid and charge DM water and

calcium chloride in SS reactor and heat the reaction mass up to reflux. Distil out water completely

and cool the reaction mass. Filter the isolated solid and dry, mill and then blend. Send the filtrate to

ETP.

Chemical reaction


(Continuation from previous page.......)

Material Balance


water 10.29

Isobutyraldehyde

Distillation 1.76

sodium hydroxide 1.01 ML 7.73

hydantoin 1.18 Ditilled water for boiler 7.06

glycine 0.88 Washing Solvent 0.66

Isobutyraldehyde 1.82 Drying Loss 0.12



MeOH Washing 0.71

18.33 18.33

4. ALPHA KETO PHENYLALANINE CALCIUM SALT

Manufacturing Process

• Charge Glycine, DM water and Acetic anhydride in glass line reactor and stir the mass for 1hr.

Filter the isolated solid and transfer the wet material for next stage and the filtrate (40% acetic

acid) keep for selling.

• Charge Dimethyl formamide, stage-I, sodium acetate, acetic anhydride, benzaldehyde in glass

line and heat the reaction mass up to reflux. Distil out acetic anhydride and DMF completely

under vacuum and add DM water in reaction mass. Cool it and add Hydrochloric acid in the glass

line reactor. Heat the reaction mass up to reflux. Separate out the salt to TSDF for land filling.

Cool the reaction mass and add calcium chloride, triethylamine and methanol in the glass line

reactor and stir at room temperature. Distil out methanol and reuse for next batch. Filter the

isolated solid and send the salt to TSDF site for land filling. The isolated solid of Ca salt of Alpha

keto phenylalanine is then undergone drying, milling, blending and packing.

Chemical reaction


Material Balance


glycine 1.33 ML 7.63

Acetic anhydride 3.33 Drying Loss 0.12

water 1.34

Acetic Acid 4

Benzaldehyde 2.13 Distil out DMF 3.31

Sodium Acetate 0.4 salt 0.4

DMF Fresh 3.34 Recovery of MeoH 1.29


Methanol 1.33

TEA 0.83 Calcium Chloride 0.52

17.75 17.75

5. ALPHA KETO VALINE CALCIUM SALT

Manufacturing Process Charge Hydantoin, Glycine, Acetone, Sodium hydroxide and DM water in SS Reactor, Heat the

reaction mass up to reflux and completely distill out acetone and reuse for next batch. Cool the

reaction mass and charge DM water and sodium Hydroxide and adjust the pH to 6-7 with

hydrochloric acid. Charge DM water and calcium chloride in to SS reactor. Heat the reaction mass

up to reflux. Distill out water and cool the reaction mass. Filter the isolated solid and send the

filtrate to ETP. Dry the material, mill it and blend. Pack the material in paper drums.

Chemical reaction


Material Balance


water 13.34 Acetone 2.08

hydantoin 1.33 ML 11.69

glycine 1 Ditilled water for boiler 8

Acetone 2.13 Washing Solvent 0.51

sodium hydroxide 1.29 Drying Loss 0.13



MeOH Washing 0.53

23.41 23.41

6. ALPHA HYDROXY METHIONINE CALCIUM SALT

Manufacturing Process Charge Methionine acid and methanol in the glass line reactor. Distill out methanol and reuse for

next batch. Charge sodium hydroxide and adjust pH between 6.5 to 7.0 and add carbon. Filter

through sparkler and add calcium chloride and centrifuge. Charge methanol and heat up to reflux.

Filter the isolated solid and dry, mill and blend .Pack the material in fiber drums.

Chemical reaction


Reactor

Reactor

DM Water

Ferric Chloride

Reactor

Sucrose

Reactor

Filtration by

Centrifuge

Centrifuge DM Water

Reactor

Hydrochloric acid

Caustic soda flakes

ML to ETP

Sucrose

Material Balance


Methionine Acid 1.39 Activated Carbon 0.03

sodium hydroxide 0.31 Hyflow 0.04

Activated Carbon 0.03 ML to ETP 1

Hyflow 0.04 Washing solvent 0.67

Calcium Chloride 0.42 Drying Loss 0.14

Methanol wash 0.69 Product 1

2.88 2.88

7. IRON SUCROSE

Manufacturing Process Ferric chloride hexahydrate is dissolve in DM water and react with 20% sodium hydroxide solution at 20-

25°C in form of ferric hydroxide. Centrifuge the gelatinous precipitate of ferric hydroxide and collect the

wet lumps. Charge DM water, Ferric hydroxide lumps, sucrose and 20% sodium hydroxide solution in the

reactor. Heat it up to reflux. Concentrate the reaction mass by distilling of water and chill the residue in form

of Iron Sucrose. Dry the wet cake in the dryer, mill then pack.

Chemical reaction


Filtration by

Sparkler

Hyflow

Reactor

Reactor

Centrifuge

Tray Dryer

Hyflow

Activated carbon

Reactor Activated Carbon

Reactor Caustic Soda

Distil out water

MeOH

Methanol reuse for next

batch.

Drying Loss

Product

Milling

Sifter

Blender

IRON SUCROSE

50ºC

(Continuation from previous page.......)

Material Balance


DM Water 1.6 ML to ETP 2.53

Ferric chloride 0.4 Hyflow 0.07

Sucrose 0.8 Activated carbon 0.07

Hydrochloric acid 0.12

Ditilled water for

boiler 1.39

Caustic soda flakes 0.23 recovered methanol 3.93

DM Water 0.6 Drying Loss 0.13

Sucrose 1.2 Product 1

Caustic soda flakes 0.04

Activated Carbon 0.07

Hyflow 0.07

MeOH 4

9.13 9.13

8.PHENYL ACETIC ACID

Manufacturing Process Charge Sodium salt of phenyl acetic acid solution in the reactor. Cool the liquid and charge

hydrochloric acid to the reactor. Centrifuge the isolated solid. Send the ML to ETP

Chemical reaction


Material Balance

Input Qty.

Output Qty

Na salt Phenyl acetic

acid 2.86

Ditilled water for

boiler 1.72

HCl / H2SO4 0.52

ML 0.36

Drying Loss 0.3

Product 1

3.38

3.38

9. DIACEREIN


Aloe-emodin is reacted with acetic anhydride at temperature 90 to 94°C in presence of sodium

acetate. After reaction completion acetic anhydride is distilled out completely under vacuum from

reaction mass, water is added in degassed mass. Isolated product is undergone for centrifuge. Tri

acetyl Aloe-emodin (Stage-1) oxidized with Chromium trioxide solution in mixture of Acetic acid

and acetic anhydride at 57 to 62°C to get Diacerein Crude (Diacerein stage-2). Reaction mass is

centrifuged. Water slurry of wet cake is prepared and centrifuged. Crude material is washed with

N,N Dimethylacetamide and then with water.Wet cake is dried in tray dryer ,mill and then pack.

Reactor

Reactor

Na salt Phenyl acetic acid

Hydrochloric Acid/ Sulphuric

Filtration by

Centrifuge

Tray Dryer

Phenyl Acetic

ML to ETP

Distilled out water for use

in utilities

ML to ETP

Drying Loss

Reactor

Reactor

Acetic Anhydride

Aloe-emodine

Sulfuric Acid

Reactor Chromium trioxide

Centrifuge Distil out ML

Reactor

Reactor

Water Slurry wash

N,N Dimethylacetamide

Filtration by

Centrifuge

ML to ETP

Acetic Acid

Acetic Acid reuse

Distillation residue

ML reused for next batch

ML to ETP Water

Drying Drying Loss

Milling

Sifter

Diacerein

Chemical reaction

OH O

O

OH

OH

O

CH3

O

CH3

O

O

O

OO

CH3

O

Aloe-emodinM. Wt.= 270.2

Tri acetyl Aloe-emodin

M. Wt.= 396.3

Acetic anhydride

Sodium acetate anhrdrous


Material Balance

Input Qty.

Output Qty

Acetic anhydride 7.15

Acetic acid sellable or

reuse 8.09

Aloe-emodine 1

Distillation residue

Incineration 0.1

Sulfuric acid 0.015

ML reuse for next batch 25

Acetic acid 15

Effluent to ETP 15

Chromium Trioxide 1.13

Drying loss 0.1

Water Slurry wash 10

Product 1

N,N

Dimethylacetamide 10

Water 5

49.29

49.29

10. TOLFENAMIC ACID


Part A – Tolfenamic Acid Crude

Process Stage-I: Manufacturing of potassium salt of o-Chlorobenzoic acid Ortho chloro benzoic acid is reacted with potassium hydroxide in presence of methanol gives

Potassium salt of ortho chloro benzoic acid.

Process Stage-II: Condensation of potassium salt of o-Chlorobenzoic acid with 3-Chloro 2-

Methyl aniline to form crude Tolfenamic acid. Further methanol is distilled and degassed. Solid mass of potassium salt of ortho chloro benzoic

acid reacts with 3-Chloro 2-Methyl Aniline in presence of DMF and calcium carbonate by

adding catalyst, further reaction mass is charcolized and filtered.

The liquid reaction mass is further precipitated by adding HCl which forms crude Tolfenamic

Acid. Wet crude Tolfenamic acid is slurry washed in water and dehydrated in toluene by

azeotropic distillation and dried.

Part B – Tolfenamic Acid

Purification of crude Tolfenamic acid The crude Tolfenamic acid is dissolved in Dimethyl Formamide, Charcoalized and filtered.

Further material is crystallized by applying chilling. Crystallized material is filtered and dried in

vacuum tray dryer to get pure Tolfenamic acid.

Chemical reaction

Part A: Tolfenamic Acid Crude

Process Stage I: Conversion of o-Chlorobenzoic acid to the corresponding potassium salt.

Process Stage II : Condensation of potassium salt of OCBA with CMA to give crude

Tolfenamic Acid.

Part B: Purification of crude Tolfenamic Acid to give the final active substance Tolfenamic

Acid


Reactor

Reactor

N,N

Dimethylformamide

Orthochlorobenzene

Reactor Water

Centrifuge ML for Distillation

Drying

Reactor

Sparkler

Drying loss

Hydrochloric Acid

Residue

DMF reuse for next batch

Hyflow & Carbon disposed to

TSDF & Incinerator Activated Carbon

Drying

Milling

Blending

3-Chloro methyl aniline

Cat-TNA

Water Reuse

in utilities

N,N

Hyflow Supercel

Centrifuge ML for Distillation Residue

Reuse for next

Drying loss

Sifting

Tolfenamic Acid

O C H3

PH O H O

O H O

O O

O

O

O H O C H 3

O H

O H O H H O

O O

O

O

O HOC H 3

O H

O H O H H O

O C H 3

H O H O

O H O

+ I2 + N a O H

Hesperidi

n

Diosmi

n

Material Balance

Input Qty.

Output Qty

N,N

Dimethylformamide 4.31 Water reuse in washing 10

Orthochlorobenzene 1.71

salt TSDF 0.69

Potassium Carbonate 0.81

DMF 4.31

3-Chloro methyl

aniline 0.81 Drying loss 0.75

Cat-TNA 0.02

carbon (inci.) 0.04


Distilation residue 0.2

Water 8.5

ML to distillation 7.4

N,N

Dimethylformamide 7.5 Drying loss 0.2

Activated Carbon 0.04

Product 1

Hyflow Supercel 0.13

Hyflow 0.13

Water 0.5

24.73

24.73

11. DIOSMIN


Hesperidin reacts with iodine in presence of sodium hydroxide and pyridine as a solvent. The

reaction is carried out at 98 to 103°C.

After reaction completion the reaction mass is cooled. Pyridine is distilled out completely under

vacuum. Methanol is charged in the reactor. The reaction mass is heated to reflux to get the uniform

mixture. After completion of the reflux, reaction mass is cooled. Solid cake (crude Diosmin) is

isolated by centrifugation.

The wet cake of crude Diosmin is charged into the solution of sodium Thiosulphate in De-ionised

water. The mixture is stirred well to become homogenous. Solution of sodium hydroxide is added

to get a clear solution. This solution is filtered over hyflow bed and clear filtrate is collected in

reactor. Wash the hyflow bed with de-ionized water and collect the washings along with the filtrate

in reactor and water is distilled out. Further mass is filtered through sparkler filter. Cool the filtrate,

precipitate out the Diosmin by adding concentrated Sulphuric acid. The reaction mass is stirred well

to get optimum precipitation of the product. The resulting solid is isolated by centrifugation. The

cake in the centrifuge is washed with purified water.The wet cake is taken in purified water in the

reactor. The slurry is heated and stirred well. The solid is isolated by centrifugation. The isolated

solid cake in the centrifuge is washed with warm purified water to free of sulphates.The above

obtained pure Diosmin is dried in vacuum tray dryer. The product is milled, blended and sifted on a

sieve.

Chemical reaction


Material Balance

Input Qty.

Output Qty

Pyridine 6.68

Distil Out Pyridine 5.5

Hesperidin 1.586

Distil out Methanol 5.15

Sodium hydroxide 0.57

Methyl Iodide 0.43

Iodine 0.49

salt To TSDF 0.5

Methanol 8.89

WaterDistillation 4

De-ionised Water 4

Salt ToTSDF 0.1

Sodium Thiosulphate 0.114

ML to ETP 9.63

Sodium Hydroxide 0.5

Drying loss 0.05

Hyflow 0.15

Product 1

Sulphuric Acid 0.53

Hyflow 0.15

Purified Water 3

26.51

26.51

Reactor

Centrifuge

Pyridine

Hesperidin

Sodium

Methyl Iodide

Sparkler

Hyflow & Salt to TSDF Hyflow

Sparkler Filter

Reactor

Centrifuge

Iondine

Methanol

Reactor Water Distillation & reuse

Salt to TSDF

Tray Dryer

Milling

Reactor De-ionised Water

Sodium Thiosulphate

Sodium Hydroxide

Sulphuric Acid

Purified Water ML to ETP

Drying Loss

Vacuum Tray

Sifter

Blender

Diosmin

Distill Out Pyridine &

H2N C

O

NH2 + H2N NH2 . H2O

Urea Hydrazine Hydrate Semicarbazide

+ H2O NH3 +

MethanolHydrochloric Acid

. HCl

Semicarbazide Hydrochloride

H

H2N

NH2

N O

H2N

NH2

N OH

N

C l

NH2

NH

O

NH2

NN H

N

O

Semicarbaz ide Hydrochloride

+H Cl

2-Chloro-pyridine

TPO (C rude)

2- Ethoxy ethanol

Catalyst

NN

N

O

HN

N

N

O

H

TPO (Crude) TPO (Pure)

Water slurry

12. 1,2,4 TRIAZOLO [4,3-A] PYRIDIN-3-ONE (T.P.O)


Urea reacted with hydrazine hydrate in presence of water at temperature 105 to 110°C to give

semicarbazide. Water is distilled out under vacuum and degas. Methanol is added to dissolve it.

Further concentrated Hydrochloric acid is added to precipitate semicarbazide as hydrochloride salt.

Semicarbazide hydrochloride reacted with 2- Chloro pyridine in presence of catalyst , using 2-

ethoxy ethanol as a solvent to give TPO, followed by water crystallization with chilling,

centrifugation and dried. Crude TPO is purified by water slurry to remove the salts to give pure

TPO, which is isolated by centrifuging and further wet cake is dried.

Chemical reaction

Methanol

Salt Hydrochloric Acid

Methanol reuse

Water to ETP

Drying Loss

2-Chloro

Sulfuric Acid

Water

100º

Reactor

Reactor

Urea

Hydrazine Hydrate

Water

Centrifuge

Drying

Reactor

Reactor

ML

Reactor

Reactor

Sparkler

2-Ethoxy

Centrifuge

Dryer

Milling

Sifting

Heat

Chill

Heat

Cool & Chill Ethoxy

Salt

ML to ETP

Drying Loss


Material Balance

Input Qty.

Output Qty

Urea 1.89

ML 2.46

Hydrazine Hydrate 1.97

salt 0.02

Methanol 5

Methanol reuse 4.8


ML 4.84

2-Ethoxy Ethanol 4.23

Drying loss 0.12

2-Chloro Pyridine 1.28

Ethoxy Ethanol 4.2

Sulfuric Acid 0.02

salt 0.05

Water 2

ML 2

drying loss 0.1

product 1

19.59

19.59

1, 2, 4-Triazolo (4, 3-a) Pyridine-3-

one

13. FERRIC CARBOXY MALTOSE


Charge ferric chloride in to a reactor containing DM water under constant stirring.Charge sodium

carbonate solution and adjust the pH between 5.0 and 6.0.Centrifuge the mass and wash with water

to remove excess chloride. Collect the wet mass and dissolve it in DM water. Charge maltodextrin

and sodium hypochlorite in this mass. Charge Sodium bromide, stir and adjust the pH between

11.00 to 11.50 by adding sodium hydroxide solution. Heat the reaction mixture , maintain for four

hrs and cool down. Adjust pH of the mixture between 5.5 to 6.5 by dilute HCl. Filter the mass

through sparkler filter. Add this solution dropwise to a reactor containing methanol under stirring.

Centrifuge the isolated product and wash with methanol. Dry the wet cake, mill and then pack the

product HDPE drum.

Chemical reaction Ferric chloride Hexahydrate + Sodium carbonate + Purified water (Double

Pass Reverse Osmosis Water)

FeCl3.6H2O Na2CO3 H2O

(M. Wt. 270.2) (M.Wt. 105.99) (M. Wt. 18)

Ferric Hydroxide + Sodium Chloride + Carbon dioxide

Fe (OH )3 NaCl CO2 (M. Wt. 106.86) (M.Wt. 58.44) (M.Wt 44.00)

Fe(OH)3 + C6nH [10n+2]0[5n+1] + NaBr + NaOCl

(Ferric hydroxide) Maltodextrin Sodium Bromide Sodium Hypochlorite

[FeOx(OH)y(H2O)z]n [{(C6H10O5)m(C6H12O7)l}k


Contd..

Material Balance

Input Qty.

Output Qty

DM Water 8.33

ML to ETP 26.67

Ferric chloride 1.67

Salt TSDF 0.08


Water Reuse for Next

Batch 3.23

Water wash 16.67

Distillation residue 0.08

DM Water 0.83

Methanol 16.33

Maltodextrin 0.62

Drying Loss 0.17

Sodium Hypochlorite 1.47

Product 1

Sodium Bromide 0.01

Sodium Hydroxide 0.08

Hydrochloric Acid 0.05

Methanol 15

Methanol 1.67

47.57

47.57

14. SUCROFERRIC OXYHYDROXIDE


Charge ferric chloride in to reactor containing DM water under constant stirring. Charge sodium

carbonate solution and adjust the pH between 5.0 and 6.0.Centrifuge the mass and wash with water

to remove excess chloride. Collect the wet mass and dissolve it in DM water. Charge Sucrose and

Starch. Charge Acetone to the reactor. Centrifuge the isolated product and ml reuse for next batch.

Dry the wet cake, mill and then pack the product HDPE drum.

Chemical reaction

Contd..


Contd..

Material Balance

Input Qty.

Output Qty

DM Water 6.94

ML to ETP 11.25

Ferric chloride 0.69

Distil Out Water 1.39


ml reuse for next batch 1.36

Water 3.47

Drying Loss 0.14

DM Water 1.39

Product 1

Sucrose 0.28

Starch 0.28

Acetone 1.39

15.13

15.13

15. COUPLE AMINE HYDROCHLORIDE


2- Chlorophenyl glycinate is taken in methanol thionyl chloride is added at chilled condition in 90to 120

min. Reaction mass is maintained for 30 min at chilled condition. Then heated to 60 to 65°C and maintain

temp. 60 to 65°C for 5 hours at room temp.

Then product is taken in MDC by extraction at by liq. NH3 basic PH. After MDC extraction organic layer is

washed by water followed by NACL treatment. MDC distilled out atmospherically then traces removed by

vacuum. Oily syrup of 2- Chlorophenyl glycinate is obtained.

Tartaric acid solution in methanol is prepared and addition of stage-I plus acetone solution is done up to

40°C. Reaction is maintained for 30 hrs at 32±2°C. After reaction confirmation product is isolated by

filtration followed by chilled methanol washing. Wet cake is obtained is dried for 4 hrs at 55 to 60°C. Crude

stage –II is obtained. Crude StageII is then washed with chilled methanol .

1, 2- Thiopene ethanol is taken in Methylene dichloride and Triethyl amine is charged then socl2

is added slowly at chilled condition. Reaction mass is heated to reflux after reflux of 3hrs. Cooled

to 25to 35°C. Water is charged, and then sodium carbonate solution is added to ph 8 to 8.5. After

stirring, layer separation and twice water washing. Methylene dichloride is distilled out at

atmospherically then degassed under vacuum. Crude stage is obtained.

Product Distillation:-

Pure stage –III is isolated by high vacuum distillation by removing I, II and main fraction of pure

stage –III.Ester free base of (+) Tartaric salt of stage –II is prepared at chilled condition in

Methylene dichloride by adding 10% sodium bicarbonate solution. After stirring and layer

separation aqueous layer is extracted by Methylene dichloride till product absence in aqueous layer.

After water washing and NACL treatment MDC is removed under vacuum up to 35°C.

Ester free base is couple with stage-III in presence of acetonitrile, Na2 Co3 KI (adding lot wise) and

TBAB maintaining 96 hrs at reflux. After reaction confirmation cooled to RT and excess Na2 CO3,

salts removed by filtration followed by acetonitrile washing.

REACTOR

Methanol

2-Chlorophenyl glycine

Thionyl Chloride

HCL to Scrubber

Distil Methanol + Socl2

reuse for next batch

REACTOR

Water

Liq. Ammonia

Methylene Dichloride

Aqueous layer to ETP

REACTOR Sodium Chloride Solution


Methylene chloride

Distilled and reuse. REACTOR

Stage-I

REACTOR Acetone

Stage-I

Base is isolated removing acetonitrile under vacuum up to 45°C Base is dissolved in toluene. Then conc.

HCL is added to organic layer at chilled temperature. Reaction mass stirred for 2 hrs at RT. Product is

isolated by filtration. Finally, the wet cake is dried at 55 to 60°C for 8 hrs.

Chemical reaction


REACTOR

Methanol

Tartaric acid

CENTRIFUGE Chilled Methanol

Methanol + Acetone ML

TRAY DRYER Dry Losses

Stage-II

REACTOR Methanol

Stage-II

REACTOR Chilled Methanol

Methanol Reused

TRAY DRYER Dry Losses

Product

Water

Methylene dichloride

2-Thiophene ethanol

Triethyl Amine

Thionyl chloride

Water

Sodium Carbonate

REACTOR Aqueous layer to ETP

REACTOR Distilled MDC reused

Stage-III

Ist

Cut

IInd

Cut

Residues

Product[Stage III]

REACTOR

Crude Stage-III

REACTOR

Water

Stage-II

Methylene Dichloride

Sodium Bicarbonate soln


REACTOR Sodium Chloride Soln

REACTOR


Methylene Chloride

Distilled

Acetonitrile

Sodium Carbonate

Potassium Iodide

TBAB

Stage III

REACTOR

CENTRIFUGE Acetonitrile Salts to Discard

REACTOR

REACTOR

REACTOR HCl

Acetonitrile Distilled

and reuse

Toluene

CENTRIFUGE Toluene ML

DRYER Drying Loss

Product

MILLING

SIFTING

COUPLE AMINE HYDROCHLORIDE

Material Balance

Input Qty.

Output Qty

Methanol 5.2

HCL to Scrubber 0.18

2-Chlorophenyl

glycine 2.13

Distil Methanol + Socl2 and

reuse for next batch 1

Thionyl Chloride 2.04

aqueous layer to ETP 35.81

Water 6.51

Methylene chloride Distilled

and reuse. 7.22

Liq.Ammonia 1

Methanol + Acetone ML 3.58

Methylene Dichloride 8.8

Dry Losses 0.13

Sodium Chloride Sol 2.54

Methanol ML reuse for next

batch 2.13

Acetone 1

Distill MDC & Reuse 1.2

Tartaric acid 0.95

Ist

Cut 0.013

2-Thiophene ethanol 0.81

IInd

Cut 0.19

Triethyl Amine 0.97

Residue 0.096

Thionyl chloride 0.97

Salts to Discard 0.4

Sodium Carbonate 5.26 Acetonitrile Distilled and

reuse 1.06

Sodium Bicarbonate

soln 14.6 Toluene ML 2.37

Acetonitrile 0.77 Drying Loss 0.02

Potassium Iodide 0.12 Product 1

TBAB 0.03

Toluene 2.4

Hydrochloric Acid 0.3

56.4 56.4

LIST OF RAW MATERIALS

SR.NO NAME OF RAW MATERIAL MTPM MODE OF

TRANSPORT

EXISTING RAW MATERIALS

1. HFS Acid 770

By Road 2. Sodium Carbonate 14

3. Sodium Chloride 105

PROPOSED RAW MATERIALS

4. Hyflow Supercel 0.26

By Road

5. Ferric chloride 7.19

6. Benzaldehyde 6.39

7. Ethanol Amine 2.61

8. Isobutyraldehyde 5.46

9. Sulfuric acid 0.045

10. 2-Chloro Pyridine 12.8

11. 2-Chlorophenyl glycine 4.26

12. 2-Ethoxy Ethanol 42.3

13. 2-Thiophene ethanol 1.62

14. 3-Chloro methyl aniline 1.62

15. Acetic acid 45

16. Acetic anhydride 32

17. Acetone 19.51

18. Acetonitrile 1.54

19. Activated Carbon 0.31

20. Aloe-emodine 3

21. Calcium Chloride 12.69

22. Cat-TNA 0.04

23. Caustic soda flakes 0.54

24. Chromium Trioxide 3.39

25. DMF Fresh 10.02

26. Ferric chloride 0.8

27. Glycine 9.63

28. Hesperidin 3.42

29. Hydantoin 11.82

30. Hydrazine Hydrate 19.7

31. Hydrochloric acid 80

32. Hyflow 0.71

33. Iodine 1.47

34. Liq.Ammonia 2

35. Maltodextrin 0.62

36. MeOH 123

37. Methionine Acid 4.17

38. Methyl Ethyl Ketone 6.9

39. Methylene Dichloride 17.6

40. N,N Dimethylacetamide 53.62

41. Na salt Phenyl acetic acid 114.4

42. Orthochlorobenzene 3.42

43. Potassium Carbonate 1.62

44. Potassium Iodide 0.24

45. Pyridine 20.04

46. Sodium Hydroxide 0.08

SR.NO NAME OF RAW MATERIAL MTPM MODE OF

TRANSPORT

47. Sodium Acetate 1.2

48. Sodium Bicarbonate soln 29.2

49. Sodium Bromide 0.01

50. Sodium Carbonate 17.21

51. Sodium Chloride Sol 5.08

52. Sodium hydroxide 15.15

53. Sodium Hypochlorite 1.47

54. Sodium Thiosulphate 0.342

55. Starch 2

56. Sucrose 6.24

57. Sulfuric Acid 22

58. Tartaric acid 1.9

59. TBAB 0.06

60. TEA 2.49

61. Thionyl Chloride 6.02

62. Toluene 4.8

63. Triethyl Amine 1.94

64. Urea 18.9

DETAILS OF SOLID & HAZARDOUS WASTE GENERATION DURING OPERATION

S.

No.

Name of The

Waste

Cat.

No. Existing Proposed Total

Method of Storage

and Disposal

1. Discarded

Containers/Barrel

s/liner

33.1 0.12 MT/Y

5.0 MT/Y

or

(100

No./M)

5.12 MT/Y

or

(100

No./M)

Collection, storage

and send to

authorized recycler

after

decontamination.

2. Process Waste 28.1 -- 4.76 MT/M 4.76

MT/M

Collection, storage

and transport to

TSDF site.

3. Used oil 5.1 -- 200

Lit/Year

200

Lit/Year

Collection, storage

and reuse as

lubricants in the

machineries within

the premises only or

send to authorized re-

processors

4. ETP Sludge 35.3 1.5 MT/M 8.5 MT/M 10 MT/M

Collection, storage

and transport to

TSDF site.

5. Distillation

Residue 36.1 -- 0.98 MT/M

0.98

MT/M

Collection, Storage

and send for

incineration.

6. Spent Solvent 28.6 -- 250

MT/Month

250

MT/Month

Collection, Storage,

Recovered and

reused.

7. Spent Carbon 28.3 -- 0.31

MT/Month

0.31

MT/Month

Collection, Storage

and send for

incineration.

8. Hyflow 28.1 -- 0.97

MT/Month

0.97

MT/Month

Collection, storage

and transport to

TSDF site.

EMISSIONS FROM COMBUSTION OF FOSSIL FUELS FROM STATIONARY OR MOBILE

SOURCES

S.

No. Stack Attached To Fuel Used

Stack

Height

Pollution

Control System Final Concentration

Existing - Nil

Proposed

1.

Steam Boiler

(1000 Kg/Hr)

Natural Gas

800 m3/Day

11

meter

Natural is used as

fuel, adequate stack

height is provided

SPM ≤ 150 mg/nm3

SO2 ≤ 100 ppm

NOX ≤ 50 ppm

Steam Boiler

(600 Kg/Hr)

TFH

(2 Lac Kcal/Hr)

2. D. G. Set

(250 KW + 93 KW)

HSD

20 Lit/Hr

9

meter Adequate stack

height is provided

SPM ≤ 150 mg/nm3

SO2 ≤ 100 ppm

NOX ≤ 50 ppm

PROCESS EMISSION

S.

No.

Stack Attached

To Stack Height

Pollution Control

System Final Concentration

Existing - Nil

Proposed

1. Reactor 20

meter

Alkali Scrubber

followed by Water

Scrubber

HCl ≤ 20 mg/Nm3

WATER CONSUMPTION

No. Purpose WATER CONSUMPTION (KL/Day)


(A) Domestic 2 2 4

(B) Industrial

1. Processing 34 2.74 36.74

2. Boiler - 4 4

3. Cooling - 4 4

4. Washing 2 1 3

5. Scrubbing - 1 1

6. Others 3 -3 0

(B) Total Industrial 39 9.74 48.74

(C) Green Belt 0 6 6

Total (A+B+C) 41 17.74 58.74

WASTE WATER GENERATION

No. Purpose WASTE WATER GENERATION (KL/DAY)


(A) Domestic 1 1.5 2.5

(B) Industrial

1 Processing 74 -1.98 72.02

2 Boiler - 0.2 0.2

3 Cooling - 0.1 0.1

4 Washing 2 1 3

5 Scrubbing - 1 1

6 Others 3 -3 0

Total (B) 79 -2.68 76.32

(C) Green Belt - - -

Total (A+B+C) 80 -1.18 78.82

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