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BHARAT RASAYAN LIMITED MOKHRA BHARAT RASAYAN LTD. 1 Annexure List Annexures Subject Annexure-1. Product List Annexure-2. Site Location Map Annexure-3. Site Layout Annexure-4. Manufacturing Process Annexure-5. Raw Material & Products Storage Details Annexure-6. Waste Water Generation Annexure-7. Waste Water Treatment Annexure-8. Water Consumption Annexure-9. Fuel Consumption Annexure-10. Hazardous Waste Generation Annexure-11. Stack Details
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Page 1: Annexure List Annexures Subjectenvironmentclearance.nic.in/writereaddata/Online/TOR/0_0...BHARAT RASAYAN LIMITED – MOKHRA BHARAT RASAYAN LTD. 1 Annexure List Annexures Subject Annexure-1.

BHARAT RASAYAN LIMITED – MOKHRA

BHARAT RASAYAN LTD. 1

Annexure List

Annexures Subject

Annexure-1. Product List

Annexure-2. Site Location Map

Annexure-3. Site Layout

Annexure-4. Manufacturing Process

Annexure-5. Raw Material & Products Storage Details

Annexure-6. Waste Water Generation

Annexure-7. Waste Water Treatment

Annexure-8. Water Consumption

Annexure-9. Fuel Consumption

Annexure-10. Hazardous Waste Generation

Annexure-11. Stack Details

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BHARAT RASAYAN LIMITED – MOKHRA

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Annexure -1 Product List

Product List

Sr. No.

Name of Product Quantity in MT/Year

Existing After Product Mix

1 Alpha Cypermethrin Technical 0 100

2 Bifenthrin Technical 0 120

3 Clodinafop Technical 0 100

4 Cypermethrin Technical 600 350

5 Fenvalerate Technical 900 300

6 Fipronil Tech. 0 100

7 Lambda Cyhalothrin Tech. 0 300

8 Metaphenoxy Benzaldehyde 960 1800

9 Permethrin Tech. 0 100

10 Safener (Cloquintocet Mexyl) 0 30

11 Thiamethoxam 0 300

12 Diafenthiroun Tech. 0 150

13 Difenconazole Tech. 0 50

14 Propanil Tech. 0 50

15 Pyrazosulfuron Tech. 0 20

16 Para Chloro Phenyl isopropyl Acetic acid 0 200

17 Para chloro benzyl cyanide 480 100

18 Myclobutanil Technical 0 15

19 Tebuconazole Technical 0 50

20 Imiazethapyre Technical 0 25

Total 2940 4260

By Product List

Sr. No. Byproducts Quantity in MT/Year

Existing After Product Mix

1 Alum 5086.08 9536.4

2 Pot. Chloride 2001.6 5036.5

3 Spent acid 1125.9 824.95

4 Hydrochloric Acid 28% 1946.58 2212.31

5 Sodium sulphite 1523.7 1403.8

6 Potassium bromide (soln.) 1850.88 3726.7

7 Sodium Bromide (soln.) 948.6 758.6

Total 14483.34 23499.26

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Annexure: Site Location Map

Figure 1: Site Location Map in Haryana

Annexure - 2

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Annexure – 3 ( Site Lay out )

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Annexure:4 Manufacturing Process

Existing

1. Cypermethrin Technical

Process Description

Meta phenoxy Benzaldehyde & cypermethric acid chloride reacted with aqueous sodium cyanide in

presence of a catalyst & produce Cypermethrin .Hexane & ethylene dichloride is used as a solvent . recovered hexane ethylene dichloride is reused.

1. Fenvalerate Technical

Process Description

Stage – 1

Parachloro Toluene reacted with Chlorine in presence of a catalyst and produced para chlorobenzylchloride. This para chlorobenzyl chloride reacted with Aqueous sodium cyanide and produced

para chlorobenzyl cyanide. A catalyst is used in this reaction.

Stage-2

Para chlorobenzyl cyanide reacted with Isopropyl bromide, caustic soda and a phase transfer catalyst and

produced 2-(4-chlorophenyl)-methyl butyro nitril (CPIN).

Stage – 3

CPIN is hydrolyzed in dil. sulphuric acid to get CPIA. CPIA reacted with Thionyl chloride in presence of

Hexane & EDC solvent and produced parachloro phenyl iso valeryl chloride. Para chloro phenyl iso valeryl

chloride and meta phenoxy benzaldehyde reacted with Aqueous sodium cyanide a phase transfer catalyst to used in this reaction. Soda ash is used as pH booster & recovered hexane & EDC is reused.

2. Metaphenoxy Benzaldehyde

Process Description

Stage-1

Benzaldehyde reacted with bromine and chlorine in presence of Aluminum chloride, Ethylene di chloride is

used as a solvent in above reaction. The Brominated mass quenched in water and washed. After washing organic mass is distilled and recovered Ethylene di chloride is reused in bromination. Distilled meta bromo

benzaldehyde taken for second stage reaction.

Stage-2

Metabromo benzaldehyde reacted with Mono ethylene glycol and produced meta bromo Benzal acetal.

This meta bromo benzalacetal react with KOH and phenol in presence of Toluene solvent and produce

metaphenoxy benzalacetal which on hydrolysis with sulphuric acid and water give Meta phenoxy Benzaldehyde and MEG water is neutralized with caustic lye and recovered water and mono ethylene

glycol is recycle in next batch.

3. Prachloro Benzyl Cyanide

Process Description

Stage – 1

Parachloro Toluene reacted with Chlorine in presence of a catalyst and produced para chlorobenzyl chloride. This para chlorobenzyl chloride reacted with aqueous sodium cyanide and produced para

chlorobenzyl cyanide. A catalyst is used in this reaction

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1. Alpha Cypermethrin Technical

Process Description

Meta phenoxy Benzaldehyde & cypermethric acid chloride reacted with aqueous sodium cyanide in presence of a catalyst & produce Cypermethrin .Hexane & ethylene dichloride is used as a solvent .

recovered hexane ethylene dichloride is reused. Cypermethrin reacted with a tri ethyl amine & produced

Alpha cypermethrin, which is acidified with acid &crystallized in hexane. Solvent is filtered & product dried in drier. Recovered Hexane, & TEAS is reused.

Process flow diagram of Alpha Cypermethrin

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CHEMICAL REACTION OF ALPHACYPER METHRIN

H3C CH3

C CHO

H COCl + + NaCN + H2O CH C CMAC MPB Cl MW=227.5 MW=198 Cl H3C CH3

C

Cl H C=HC COO C + NaCl+NaCN +H2O Cl CN

Cypermethrin Technical

MW = 416.3

H3C CH3

C

Cl H C=HC COO C + CH3COOH+TEA Cl CN Acetic acid

Cypermethrin Technical

MW = 416.3

H3C CH3

C

Cl H C=HC COO C + TEA Acetate Cl CN

Alpha Cypermethrin Technical

MW = 416.3

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Material Balance of Alphacypermethrin

S. No. Input/Ton of Product Total Consumption to

produce 1KG. of Alpha

Cypermethrin Technical Raw Materials

1 Metaphenoxy Benzaldehyde 0.71

2 Cypermethic Acid Chloride 0.83

3 Sodium cyanide 0.20

4 Catalyst 0.02

5 Ethylene Dichloride (Fresh + Recovered) 0.08

6 Hexane (Fresh + Recovered) 3.62

8 Soda Ash 0.02

9 TEA (Fresh + Recovered) 0.13

10 Acetic acid 0.109

11 Caustic Lye 47% 0.176

12 Sodium hypochlorite for washing 0.183

12 Water 4.855

Total 10.934

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Alpha

Cypermethrin - - 1 - Product

2 Rec Ethylene

Dichloride - - 0.08 - Recovered for Reuse

3 Rec Hexane - - 3.46 - Recovered for Reuse

4 Rec Cyper. - - 0.39 - Recovered for Reuse

5 Rec. TEA - - 0.08 - Recovered for Reuse

6 EDC - 0.00 - - Loss

7 Hexane - 0.08 - - Loss

8 Operation Loss - 0.08 - - Loss

9 Spent Cyanide

Aq. 1.813 - - -

To ETP through detoxification

10 Water+acetic

acid +salt 3.775 - - - To ETP

11 Ventury soln 0.176 To ETP

Total

(Ton)

5.764 0.16 5.01

10.934

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2. Bifenthrin Technical

Process Description

Bifenthrin alcohol is reacted with thionyl chloride to form bifenthrin chloride which was further reacted

with lambda cyhalothric acid [2-(IR, S)-cis-2,2-dimethyl-3-(2,2-chloro,3,3,3-trifloro-1-propargyl) cyclopropane Carboxylic acid] to form Bifenthrin (T) Product is purified in suitable solvent.

Process Flow Diagram

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CHEMICAL REACTION BIFENTHRIN

+ SOCl2 + SO2 + HCl

Thionyl chloride [119] [64] [36.5]

CH3 CH2OH CH3 CH2Cl

Bifenthrin Alcohol [198 ] Bifenthrin Chloride

[216.5 ]

Cl

+ C = CH COOH Catalyst

CF3 +K2CO3 + TBAB

CH3 CH2Cl CH3 CH3 Pot.Carbonate [138]

Bifenthrin Chloride Cyhalothric Acid

[216.5] [242.5]

Cl

C = CH C O

CF3 O CH2 + HCl + KCl

CH3 CH2 Hydrochloric Acid Pot. Chloride

CH3 [ 36.5 ] [ 74.5 ]

Bifenthrin [ 422.5 ]

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Material Balance of Bifenthrin

S. No. Input/Ton of Product Total Consumption to

produce 1KG. of Bifenthrin Technical Raw Materials

1 Bifenthrin Alcohol 0.57

2 SOCl2 0.34

3 Ethylene dichlride(Fresh + Recovered) 1.0

4 Lambda Cyhalothric Acid 0.63

5 Caustic Soda lye 47% 0.486

6 Potassium Carbonate 0.36

7 Dimethyl Formamide (DMF) (Fresh + Recovered) 1.13

8 Hexane (Fresh + Recovered) 1.170

9 Water 3.657

Total (Ton) 9.34

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Bifenthrin - - 1.000 - Product

2 Sodium Sulfite

(19%) - - 2.11 - Byproduct

3 Hydrochloric

Acid (30%) - - 0.348 - Byproduct

4

Potassium

Chloride

solution

- 2.405 - Byproduct

5

Recovered

Ethylene dichloride

- - 0.960 - Recovered for Reuse

6 Recovered DMF - - 1.09 - Recovered for Reuse

7 Recovered

Hexane - - 1.12 -

Recovered for Reuse

8 Uncondensed

vapor - 0.192 - - Loss

9 Water - - - - To ETP

10 Residue - - - 0.12 To incinerator

Total

(Ton)

0 0.192 9.03 0.12

9.34

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3. Clodinafop Propargyl Technical

Process Description

Stage-1

Propargyl alcohol reacted with thionyl chloride & produced Propargyl chloride.

Stage-2

5-chloro-2,3 di chloro pyridine, potassium carbonate, 2-(4-hydroxyphenoxy propionic acid) and propargyl chloride reacted and produced Clodinafop propargyl tech. DMF is used for reaction in above reaction and

Methanol is used as a solvent for crystallization. Recovered DMF & methanol reused in process.

Process Flow Diagram of Clodinafop

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CHEMICAL REACTION - CLODINAFOP PROPARGYL

CH C – CH2OH + SOCl2 CH C - CH2Cl + HCl + SO2

Propargyl alcohol Thionyl Propargyl Chloride Hydrochloric Sulpherdioxide

56 Chloride 74.5 Acid [36.5] [64]

Stage-2 119

CH3 CH3

a)

C COOH C COOK

H

H + K2 CO3

+ KHCO3

+ DMF

OH OH

2-( 4-Hydroxy phenoxy Pot.Salt of HPPA - 220

Propionic acid ) -182 ( HPPA )

CH3

b) C -- COOK

H

Cl F

Pot.Salt of HPPA

+ K2CO3 +

N

F Pot. Carbonate OH

[138] MW=220

5-chloro-2,3-difloropyridine

[ 149.5]

Cl F

[100]

CH3 Pot.bicarbonate

N O C – COOK + KF + KHCO3

H

2 -[4-(5chloro-3-floro pyridin-2 oxy)phenoxy] Pot.Propionate +Pot.Floride

[349.5] [ 58]

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Remaining part of Clodinafop Propargyl reaction.

( C )

Cl F

CH3

N O C – COOK +CH C-CH2Cl

H

2 -[4-(5chloro-3-floropyridin-2 oxy)phenoxy ] Pot.propionate +Propargyl chloride

[349.5] [74.5]

Cl F

CH3

N C COO CH2 C CH + KCl

H Pot. Chloride

[ 74.5 ]

Clodinafop Propargyl

[ 349.5 ]

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Material Balance of Clodinafop Propargyl

S. No.

Input/Ton of Product Total Consumption to produce 1KG. of Clodinafop Technical Raw Materials

1 Propargyl Alcohol 0.300

2 Thionyl chloride 0.642

3 Dimethyl Formamide (DMF) (Fresh + Recovered) 2.74

4 Caustic Soda Lye 0.918

5 2-(4-hydroxy phenoxy propionic Acid) (HPPA) 0.61

6 5-Chloro 2,3 difluoro pyridine (CDFP) 0.52

7 Potassium carbonate 0.97

8 Methanol (Fresh + Recovered) 0.54

9 Toluene (Fresh + Recovered) 0.54

10 Water 6.86

Total (Ton) 14.64

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Clodinafop - - 1 - Product

2 HCl (30%) - - 0.656 - Byproduct

3 Sodium

Sulfite(24%) - - 2.527 - Byproduct

4 Recovered

DMF - - 2.628 - Recovered for Reuse

5 Recovered

Methanol - - 0.516 - Recovered for Reuse

6 Recovered

Toluene - - 0.52 - Recovered for Reuse

7 DMF - 0.108 - - Loss

8 Methanol - 0.024 - - Loss

9 Toluene - 0.02 - - Loss

10 Salt + Water - - 6.366 - To ETP

11 Residue - - - 0.275 To Incinerator

Total (Ton) - 0.152 14.213 0.275

14.64

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4. Cypermethrin Technical

Process Description

Meta phenoxy Benzaldehyde & cypermethric acid chloride reacted with aqueous sodium cyanide in presence of a catalyst & produce Cypermethrin .Hexane & ethylene dichloride is used as a solvent .

recovered hexane ethylene dichloride is reused.

Process Flow Diagram of Cypermethrin

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CHEMICAL REACTION OF CYPERMETHRIN

H3C CH3

C

CHO

H COCl + + NaCN + H2O

Cl CH

C Cypermethric Acid chloride sodium cyanide

Cl MW=227.5 [49 ]

MPB

198

H3C CH3

C O

H

Cl

C HC COO C + (NaCl+ NaCN +water)

Cl Spent Sod. Cyanide

CN

Cypermethrin Technical

MW=416.3

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Material Balance of Cypermethrin

S. No. Input/Ton of Product Total Consumption to produce

1 KG. of Cypermethrin

Technical Raw Materials

1 Metaphenoxy Benzaldehyde 0.503

2 Cypermethic Acid Chloride 0.585

3 Sodium cyanide 0.146

4 Catalyst 0.014

5 Ethylene Dichloride (Fresh + Recovered) 0.06

6 Hexane (Fresh + Recovered) 1.248

7 Sodium Hypo Chlorite 0.05

8 Soda Ash 0.02

9 Water 2.107

Total (Ton) 4.733

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Cypermethrin - - 1 - Product

2 Recovered Ethylene

Dichloride

- - 0.058 - Recovered for Reuse

3 Recovered

Hexane - - 1.190 - Recovered for Reuse

4 Ethylene Dichloride

- 0.002 - - Loss

5 Hexane - 0.058 - - Loss

6 Spent Cyanide 1.225 - - - To ETP through

Detoxification

7 Water +hypo 1.200 - - - To ETP

Total

(Ton)

2.425 0.06 2.248 0.00

4.733

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5. Fenvalerate Technical

Process Description

Stage – 1

Parachloro Toluene reacted with Chlorine in presence of a catalyst and produced para

chlorobenzylchloride. This para chlorobenzyl chloride reacted with Aqueous sodium cyanide and produced

para chlorobenzyl cyanide. A catalyst is used in this reaction.

Stage-2

Para chlorobenzyl cyanide reacted with Isopropyl bromide, caustic soda and a phase transfer catalyst and

produced 2-(4-chlorophenyl)-methyl butyro nitril (CPIN).

Stage – 3

CPIN is hydrolyzed in dil. sulphuric acid to get CPIA. CPIA reacted with Thionyl chloride in presence of

Hexane solvent and produced parachloro phenyl iso valeryl chloride. Para chloro phenyl iso valeryl chloride and meta phenoxy benzaldehyde reacted with Aqueous sodium cyanide a phase transfer catalyst

to used in this reaction. Soda ash is used as pH booster & recovered hexane & EDC is reused.

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CHEMICAL REACTION OF FENVALERATE

Stage – 1

CH3 CH2Cl

i

a) + Cl2 + Catalyst-I + HCl

AZDN Hydrochloric acid

Chlorine [36.5]

Cl Cl

Parachloro Toluene Para chlorobenzylchloride

MW=126.5 MW=161

CH2 – Cl CH2CN

b) + H2O + NaCN + Catalyst-II + NaCl

TEA Sod. Chloride

[58.5]

Cl Cl Para chlorobenzyl

Cyanide

Para chloroBenzylchloride + Sodium Cyanide (PCBCN)

Stage –2 MW=151.5

CH3 CH3

a) CH

CH2CN CH3 HC—CN

+ CH3 CH – Br + NaOH + Cat-III TEBA

+ NaBr+H2O

Sod.bromide [103]

Cl Cl

ParachloroBenzyl cyanide + Isopropylbromide + Sodium hydroxide 4 -chloro phenyl isovaleryl nitril

MW=123 MW=40 MW=193.5

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Remaining part of Fenvalerate reaction

b)

CH3 CH3 CH3 CH3

CH CH

HC –CN HC COCl

+ SO2

+ H2SO4 + H2O + Cat-IV DMF+ SOCl2 + Hexane +HCl+H2O

Sulphuric Thionyl

Cl Acid Chloride Cl

MW=98 MW=119

4-chlorophenyl Isovaleryl Nitirile

c)

CH3 CH3

CH

HC – COCl

+ NaCN (Aq.) + OHC + Catalyst-V TEBA

Sodiumcyanide MPB

Cl

Para chlorophenyl Isovaleryl chloride

MW=231.5

CH3 CH3

CH H

HC COO C

+ Spent sodium cyanide for detoxification +NaCl

CN

Fenvalerate Technical

Cl MW=419

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Material Balance of Fenvalerate

S. No. Input/Ton of Product Total Consumption to produce

1KG. of Fenvalerate Technical Raw Materials

1 Para chloro Toluene 0.415

2 Chlorine 0.237

3 Catalyst I (Fresh + Recovered) ( AZDN) 0.002

4 Catalyst -II(TEA) 0.011

5 Sodium Cyanide 0.300

6 Isopropyl Bromide (Fresh + Recovered) 0.345

7 Caustic Soda Lye 0.762

8 Caustic Soda flakes 0.15

9 Catalyst III & V ( TEBA) 0.019

10 Sulphuric Acid 0.811

11 Sulphuric Acid 70% Wash 0.05

12 Dimethyl Formamide (DMF) 0.005

13 Thionyl chloride 0.356

14 Hexane (Fresh + Recovered) 1.160

15 Ethylene Dichloride (Fresh + Recovered) 0.03

16 Metaphenoxy Benzaldehyde 0.500

17 Soda Ash 0.01

18 Sodium hypo chlorite 0.05

19 Water 7.577

Total (Ton) 12.79

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Fenvalerate - - 1 - Product

2 HCl 30% - - 0.765 - Byproduct

3 Spent acid - 1.251 - Byproduct

4 Sod. Sulphite Soln. (22%)

- - 1.693 - Byproduct

5 Catalyst - - 0.00184 - Recovered for Reuse

6 Isopropyl

bromide - - 0.01 - Recovered for Reuse

7 Hexane - - 1.12 - Recovered for Reuse

8 Ethylene Dichloride

- - 0.028 - Recovered for Reuse

9 Hexane - 0.040 - - Loss

10 Ethylene Dichloride

- 0.002 - - Loss

11 Uncondensed

Vapour 0.0656 - - Loss

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12 Spent Sod. Cyanide aq.

Soln.

1.9944 - - - To ETP through

detoxification unit

13 NaBr. Soln. 1.054 - - - To ETP through bromine recovery

15 Water 3.677 - - - To ETP

16 Residue - - - 0.04 To Incineration

17 Spent sod

hypochlorite 0.05 - -

-

TO ETP

Total (Ton)

6.78 0.108 5.87 0.04

12.79

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6. Fipronil Technical

Process Description

Trifluoromethane Sulfinyl chloride is reacted with 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoro methyl

phenyl)-1H-pyrazole to form Fipronil.Ethylene dischloride is used as solvent, which is recovered & reused.

Process Flow Diagram of Fipronil

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CHEMICAL REACTION OF FIPRONIL

CF3

S CN

CN

N

N + F3C S Cl Cat-B NH2 N + HCl

H2N N Sulfinyle chloride Cat –C MW=36.5

Cl Cl [152.5] Cl Cl

CF3 CF3

5-amino-3-cyano-2,6 – dichloro 4-trifluoromethyle Fipronil [ 437 ]

Phenyl pyrazole [ 321 ]

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Material Balance of Fipronil

S. No. Input/Ton of Product Total Consumption to

produce 1kg of Fipronil Technical Raw Materials

1 5-amino-3-cyno-1-(2,6-dichloro-4-trifluoro methyl phenyl)-1H-pyrazole

0.93

2 Ethylene Di Chloride (EDC) (Fresh + Recovered) 3.730

3 Tri floro metthane sulfinyl chloride 0.492

4 Trmethyl amine hydrochloride 0.492

5 4- DMAP 0.033

6 Ammonia solution 0.003

7 Water 8.60

Total (Ton) 14.28

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Fipronil - - 1 - Product

2 Ethylene Dichloride

- - 3.545 - Recovered reused

3 Ethylene

Dichloride - 0.185 - - Loss

4 Hydrochloric

acid -30% - - 0.3925 - Bi-product

5 Washing +salt 8.853 - - - To ETP

6 Residue - - - 0.3045 To Incineration

Total

(Ton)

8.85 0.19 4.94 0.30

14.28

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7. Lambda Cyhalothrin Technical

Process Description

Stage- 1

Lambda cyhalothric acid reacted with thionyl chloride & produced Lambda Acid Chloride.

Stage-2

Lambda acid chloride, meta phenoxy Benzaldehyde, Aq. Sodium cyanide and a catalyst reacted and

produced cyhalothrin technical. Hexane is used as a solvent in this reaction. Spent sodium cyanide is sent detoxification plant. Recovered hexane is reused then Cyhalothrin is epimerized with IPA and

catalyst to form Lambda Cyhalothrin Tech.

Process Flow Diagram of Lamda Cyhalothrin

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CHEMICAL REACTION OF LAMBDA CYHALOTHRIN

CF3 + SOCl2 C F3

C = CH COOH C = HC COCl + HCl+SO2

Cl Cl

Lambda Acid Lambda Acid Chloride + Hydrochloric acid

MW=242.5 MW=261

CHO

CF3

C = CH COCl +

Cl O + NaCN + H2O

Lambda Acid chloride + MPB Sodium Cyanide Water

198

O +NaCN +NaCl

CF3

C = CH COO + CH -

Cl CN

Cyhalothrin Technical

MW=450

+ DIPA + IPA

Diisopropyl amine Isopropryl alcohol

O

CF3

C = CH COO CH + DIPA + IPA

Cl CN Di Isopropyl amine+ Isopropyl Alcohol

Lambda Cyhalothrin Technical

MW=450

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Material Balance of Lambda Cyhalothrin

S.

No.

Input/Ton of Product Total Consumption to produce 1KG. of Lambda Cyhalothrin

Technical Raw Materials

1 Lambda Acid 0.555

2 Thionyl chloride 0.290

3 Dimethyl Formamide (DMF) 0.002

4 Caustic Soda Lye 0.54

5 Metaphenoxy Benzaldehyde 0.44

6 Sodium Cyanide 0.124

7 Catalyst 0.01

8 Soda Ash 0.03

9 Hexane 2.60

10 Sodium Hypo Chlorite 0.490

11 Acetic Acid 0.115

12 Isopropyl Alcohol 0.79

13 Di isopropyl Amine 0.04

14 Lambda powder (seeding) 0.02

15 Sodium bicarbonate (NaHCO3) 0.01

16 Caustic Soda Flakes 0.098

17 Water 6.756

Total (Ton) 12.91

S.

No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Lambda

Cyhalothrin - - 1 - Product

2 Sodium Sulphite

Solution (22%)

- - 1.35 - Byproduct

3 Hydrochloric Acid (28%)

- - 0.3 - Byproduct

4

Recovered

Isopropyl Alchohol

- - 0.75 - Recovered for Reuse

5

Recovered Di

iso Propyl Amine

- - 0.03 - Recovered for Reuse

6 Recovered

Hexane - - 2.50 - Recovered for Reuse

7 Isopropyl Alcohol

- 0.039 - - Loss

8 Di iso Propyl

Amine - 0.012 - - Loss

9 Hexane - 0.10 - - Loss

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10 Spent Cyanide

Solution 0.79663 - - -

To ETP through

Detoxification

11 Caustic Solution

0.221 - - - To ETP

12 Water 5.81 To ETP

Total (Ton) 6.82 0.151 5.93 0.00

12.91

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8. Metaphenoxy Benzaldehyde

Process Description

Stage-1

Benzaldehyde reacted with bromine and chlorine in presence of Aluminum chloride, Ethylene di chloride is

used as a solvent in above reaction. The Brominated mass quenched in water and washed. After washing organic mass is distilled and recovered Ethylene di chloride is reused in bromination. Distilled meta bromo

benzaldehyde taken for second stage reaction.

Stage-2

Metabromo benzaldehyde reacted with Mono ethylene glycol and produced meta bromo Benzal acetal.

This meta bromo benzalacetal react with KOH and phenol in presence of Toluene solvent and produce

metaphenoxy benzalacetal which on hydrolysis with sulphuric acid and water give Meta phenoxy Benzaldehyde and MEG water is neutralized with caustic lye and recovered water and mono ethylene

glycol is recycle in next batch.

Process Flow Diagram of Metaphenoxy Benzaldehyde

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CHEMICAL REACTION OF METAPHENOXY BENZALDEHYDE

Stage – 1

CHO CHO-- AlCl3

a) + AlCl3 + Br2 + Cl2 + EDC at + HCl

Br. Benzaldehyde + Aluminium Chloro +bromine + Chlorine - Complex + hydrochloric acid

MW=106

CHO – AlCl3 CHO

b) + H2O + HCl + ( Al2O3 + H2O + HCl ) (Alum)

Br. Br.

Stage – 2 Meta bromo benzaldehyde MW=185 O--CH2

CHO CH

O--CH2 CH2OH Cat-D PTSA

a) + CH2OH + H2O

Br. Br.

Meta bromo Benzaldehyde Mono ethylene glycol Meta bromo benzal acetal (MBBA)

MW=185 MW=62 MW=229 O—CH2 O—CH2

CH CH O— CH2 O—CH2

OH

b) + KOH + + Tol. CuCl + KBr.

Br. 56 Phenol Catalyst-E

94 +Pot. MBBA + Pot.Hydroxide Metaphenoxy Benzal Acetal (MPBA) bromide

c)

O — CH2 CHO CH

O— CH2 CH2OH +

+ H2O + H2SO4 CH2OH + H2SO4

Sulphuric acid MEG

MPBA 242 Metaphenoxybenzaldehyde

MW=198

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Material Balance of Metaphenoxy Benzaldehyde

S. No. Input/Ton of Product Total Consumption to produce

1KG. of Metaphenoxy

Benzaldehyde Raw Materials

1 Ethylene dichloride 2.726

2 Benzaldehyde 0.7130

3 Alluminium chloride 1.1760

4 Bromine 0.590

5 Chlorine 0.250

6 Formic acid 0.025

7 Thiosulphate 0.0142

8 Hydrochloric Acid (HCl) 0.428

9 PTSA ( Cat-D) 0.001

10 Caustic Soda lye 0.159

11 Mono Ethyl Glycol 0.800

12 Catalyst-E ( CuCl) 0.00310

13 Toluene (Fresh + Recovered) 1.726

14 Potassium Hydroxide (KOH) 0.390

15 Phenol 0.590

16 Sulphuric Acid 0.032

17 Water 6.296

Total (Ton) 15..919

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery Solid Waste

1 Metaphenoxy Benzaldehyde

- - 1 - Product

2 Aq. Alum - - 5.298 - Byproduct

3 HCL 30% - - 0.818 - Byproduct

4 Rec. EDC - - 2.591 - Recovered for

Reuse

5 Catalyst ( PTSA)

- - 0.001 - Recovered for Reuse

6 Rec. MEG - - 0.76 - Recovered for

Reuse

7 Rec. Toluene - - 1.657 - Recovered for

Reuse

8

Water

recovered from MBBA

reaction

- - 0.1085 - Reused

9

Water recovered

from MPBA reaction

- - 0.1085 - Reused

10 Water from

KOH 0.039 - Reused

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11

Water

recovered from spent

MEG

-- - 0.476 - Recovered & reused

12 EDC - 0.14 - - Loss

13 MEG - 0.04 - - Loss

14 Toluene - 0.07 - - Loss

15 Water 0.380 - - - To ETP

16 Effluent for

ventury 0.243 - - - To ETP

17 KBr. Soln.

- 1.928 - To ETP through bromine recovery

18 Residue - - - 0.167 To incineration

19 Sod. Sulphate 0.058 - - -

To incineration

Total

(Ton)

0.717 0.25 14.785 0.167

15.919

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9. Permethrin Technical

Process Description

DV acid chloride reacted with Meta-phenoxybezyl alcohol & produced Permethrin tech. which is washed

with water & water is flushed under vacuum. Hydrogen chloride gas evolve is scrubbed in water.

Process Flow Diagram of Permethrin

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CHEMICAL REACTION OF PERMETHRIN

H3C CH3

CH2OH

Cl

+ C HC COCl

Cl

Metaphenoxy Benzyl alcohol + DV Acid Chloride

MW=200 MW=227.5

H3C CH3

H

Cl H

C C COO C + HCl

Cl

H

Hydrochloric Acid

Permethrin Technical

MW=391

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Material Balance of Permethrin

S. No. Input/Ton of Product Total Consumption to produce

1 KG. of Permenthrin Technical Raw Materials

1 Cypermethric Acid chloride 0.60

2 Metaphenoxy Benzyl alcohol 0.52

3 Caustic Soda Lye 0.03

4 Soda Ash 0.02

5 Acetic Acid 0.01

6 Water 1.31

Total (Ton) 2.49

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Permethrin

Tech. - - 1 - Product

2 HCl Soln.

(31%) - - 0.32 - Byproduct

3 Ventury

Soln. 0.152 - - - To ETP

4 Water 1.014 - - - To ETP

Total

(Ton)

1.166 - 1.32 -

2.49

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10. Safener (Cloquintocet Mexyl)

Process Description

Stage – 1

Monochloro acetic acid reacted with 2-heptanol and produced -2-chloroheptyl acetate. Toluene is used as

solvent. Recovered Toluene is reused in process.water formed in reaction is removed azeotropically.

Stage – 2

2-choro heptyl acetate reacted with 8-hydroxy 5-chloroquinoline and pot. Carbonate and produced

cloquintocet mexyl. N – methyl pyrolidone(NMP) is used as solvent.Recoverd NMP is reused.

Process Flow Diagram

MCA

2- HEPTANOL Recovered Toluene

Toluene Water

Residue for

Inceneration

Potassium Carbonate

Toluene Recovered NMP

NMP Recovered Toluene

Water Effluent Water 5-Chloro 8- Hydroxy

quinolene

DRYING

Safener Packaging

PREPARATION OF 2-

CHLOROHEPTYL

ACETATE

CONDENSATION

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CHEMICAL REACTION OF SAFENER

Stage -1

Cl- CH2 - COOH + HO - CH2 – CH – CH2CH2 - CH3CH3 + Toluene

MCA

94.5 CH3 2-heptanol MW=116

Cl – CH2 – COO – CH2 – CH- CH2 – CH3 – CH2 – CH3 + H2O

2-Chloro heptyl acetate [192.5]

CH3

Stage-2

2)

Cl 5 chloro -8-hydroxy quinoline

2 chloro-heptyl acetate

+ Cl – CH2 – COO - CH2-CH-CH2-CH2-CH2 + ½ K2CO3 + Tol.+NMP

Pot.carbonate

N CH3 CH3 138

H

179.5

Cl

CH3

N

CH2 - COOCH2 – CH - CH2 - CH2 - CH2 CH3

+ KCl + H2O + CO2

Potassium Chloride

Cloquintocet Mexyl 74.5

(Safener)

335.5

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Material Balance of Safener

S. No.

Input/Ton of Product Total Consumption to

produce 1 KG. of Safener (Cloquintocet Methyl)

Technical Raw Materials

1 Toluene (Fresh + Recovered) 1.48

2 2-Heptanol 0.38

3 Mono chloro Acetic Acid 0.31

4 5-chloro-8-hydroxy quinolone 0.56

5 n- methyl pyrolidone (NMP) 1.48

6 Potassium carbonate 0.49

7 Water 3.8

Total (Ton) 8.50

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Safener - - 1 - Product

2

Pot. Chloride

K2CO3+KHCO3 +water

- - 3.4 - By-product

3 Rec. Toluene - - 1.42 - Recovered for Reuse

4 Rec. NMP - - 1.41 - Recovered for Reuse

5 NMP - 0.07 - - Loss

6 Toluene 0.06 Loss

7 Uncondensed

Vapor - 0.04 - - Loss

8 Water 1.062 - - - To ETP

9 Impurities - - - - To Incineration

10 Residue - - - 0.038 To Incineration

Total (Ton)

1.062 0.17 7.23 0.038

8.50

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11. Thiomethoxam Technical

Process Description

3-methyl-4-nitro perhydro-1,3,5-oxadiazine is reacted with 2-chloro-5-chloromethyl-1,3-thiazole in

presence of suitable solvent and base to form Thiamethoxam.

Process Flow Diagram Thiomethoxam

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CHEMICAL REACTION OF THIOMETHOXAM

N NO2

Cl S C

CH2Cl

+ NaOH + HN N CH3

N

O

2-chloro-5-chloromethyl thiazole 3-methyl-4-nitroperhydro,1,2,5 oxadiazene

MW=168 Sod.hydroxide MW=160

MW=40

N NO2

Cl S

CH2

N N CH3 + NaCl + H2O

N Sod.chloride

MW= 58.5

Thiomethoxam

MW=291.5

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Material Balance of Thiomethoxam

S. No. Input/Ton of Product Total Consumption to

produce 1 KG. of

Thiomethoxam Technical Raw Materials

1 2-Chloro-5 –chloromethyl thiazole (CCMT) 0.70

2 3-methyl-4-nitro per hydro, 1,2,5 oxadiazene (MNPO) 0.70

3 Dimethyl Formamide (DMF) 3.69

4 Methanol 1.06

5 Caustic Flakes 0.18

6 Hydrochloric acid -30% 0.035

7 Sodium hypochlorite 0.150

8 Water 2.640

Total (Ton) 9.155

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item

Liquid Effluent

Air Emission

Recovery Solid

Waste

1 Thiomethoxam - - 1 - Product

2 Recovered DMF - - 3.51 - Recovered for Reuse

3 Recovered Methanol

- - 1.01 - Recovered for Reuse

4 Uncondensed

vapour - 0.24 - - Loss

6 Sodium Chloride 0.26 - - - To ETP

7 Unreacted

Caustic (100%) 0.01 - - - To ETP

8 Unreacted MNPO 0.07 - - - To ETP

9 Water 2.90 - - - To ETP

10 Residue - - - 0.16 To incinerator

Total (Ton)

3.24 0.24 5.52 0.16

9.155

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12. Diafenthiuron

Process Description

1-(2,6-diisopropyl-4-phenoxy phenyl)-thiourea continuously reflux in presence of xylene as a solvent till

conversion into 1,2-diisopropyl-2-isothiocynato-5-phenoxybenzene which is an isothiocynate derivative.

Organic layer is separated. Organic layer having 1,3-diisopropyl-2-isothiocynato-5-phenoxybenzene

obtained in step-II is then condensed with tertiary butyl amine to form Diafenthiuron.

Process Flow Diagram Diafenthiuron

O-Xylene Water

Thio-urea O-Xylene

Catalyst - MR

Tertiary Butyl amine

IPA

Water Aqueous to ETP

IPA

Isomerization

Condensation

Layer separation

Filtration & Drying

Packing

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CHEMICAL REACTION OF DIFENTHIURON

CH3 CH3

CH3 + Xylene + Cat-MR + CH3 C NH2

S CH3

NH2-C-NH

CH3 CH3 Tertiary Butyl amine

[ 73]

1-(2,6-Diisopropyl-4-phenoxyphenyl Thiourea

MW=328.6

CH3

CH3 C

CH3

CH3 – C – N – C N

CH3 H S H C + NH3

CH3 CH3 AMMONIA (17)

Diafenthiuron

[ 384.6 ]

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Material Balance Difenthiuron

1 Xylene 0.99

2 2,6 Di-isopropyl phenoxy phenyl thio urea 0.97

3 Catalyst MR 0.003

4 Tertiary butyl Amine 0.23

5 Isopropyl alcohol (IPA) 1.58

6 Water 0.200

Total (Ton) 3.98

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Difenthiuron - - 1 - Product

2 Xylene

recovered - - 0.95 - Recovered & reused

3 IPA recovered - - 1.51 - Recovered & reused

4 Xylene - 0.049 - - Recovered & reused

5 IPA - 0.078 - - Loss

6 Water + TBA 0.22 - - - To ETP

7 Residue - - - 0.19 For incineration

Total (Ton)

0.22 0.13 3.45 0.19

3.98

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13. Difenconazole

Process Description

2-(4-(4-chlorophenoxy)-2-chlorophenyl)-2-bromomethyl-4-methyl-1,3-dioxolone is reacted with 1,2,4-triazole in presence of potassium carbonate as acid scavenger. DMF is used as a solvent in the reaction. Crude Difenconazole is purified by methanol to get pure Difenconazole (T)

Process Flow Diagram of Difenconazole

Pot.Carobonate

Bromo OxolaneDerivative KBr.soln.as by product

DMF

Water

1,2,4-Triazole DMF Recovered

Methanol

Recd.Methanol for recycling

Reactor

Filtration

Purification

Drying and Packing

Diafenconazole

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CHEMICAL REACTION OF DIFENCONAZOLE

N N + + 1 K2CO3 N 2 Pot.carbonate N C H CH2Br [ 69 ] [ 138l/2 69 ] [ 418 ] 2-(4-(4-chlorophenoxy)-2-chlorophenyl) 1,2,4 triazole -2-bromomethyle-4-methyl-1,3-dioxolone

N Carbondioxide + KBr + 1 CO2 + 1 H2O (water) Pot.bromide 2 2 N CH2 N [ 119 ] [ 44/2 22 ] [18 /2 9 ] [ 406 ] N Difenconazole

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Material Balance of Difenconazole

1 2-(4-(4 chloro phenoxy )2-chloro phenyl )-2 bromo methyl 4 methyl -1 ,3dioxalone

1.29

2 1,2,4 triazole 0.25

3 Dimethyl formamide 4.00

4 Potassium carbonate 0.64

5 Methanol 2.500

6 Water 4.000

Total (Ton) 12.68

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Difenconazole

Technical - - 1.00 - Product

2 Recovered DMF

- - 3.80 - Recovered & reused

3 Recovered Methanol

- 2.40 - Recovered & reused

4 Carbon dioixide - 0.068 - - Loss

5 Uncondensed vapor

0.30

6 Potassium Bromide

- 4.791 - For Bromine Recovery

7 Unreacted Potassium

Carbonate

- - - - To ETP

8 Water - - - - To ETP

9 Unreacted

1,2.4 -triazole 0.04 - - - To ETP

10 Water formed in reaction

0.03 - - - To ETP

Residue 0.25 Incineration

Total

(Ton)

0.07 0.37 11.99 0.25

12.68

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14. Propanil Technical

Process Description

3,4-dichloro aniline is refluxed with excess propionic acid to form Propanil.

Excess propionic acid is recovered under reduced pressure and crude propanil is flushed

under reduced pressure to remove traces of propionic acid.

Process Flow Diagram of Propanil

Propionic Acid

3,4 dichloro aniline

Catalyst-H

Propionic acid recd. & reuse

Propanil Packing

Condensation

Distillation

Flushing

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CHEMICAL REACTION OF PROPANIL

NH2 NH – C – CH2CH3

Cat-H

+ CH3CH2COOH + H2O + Propionic

Cl Cl Acid

Cl Cl

Propionic Acid Propanil MW=74 MW=218 3,4-Dichloro aniline MW=162

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Material balance of Propanil

1 3,4- Dichloro aniline 0.752

2 Propionic acid 1.030

3 Catalyst 0.01

Total (Ton) 1.79

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Propanil - - 1 - Product

2 Recovered

Propionic acid - - 0.66 - Recovered & reused

3 Propionic acid - 0.04 - - Loss

4 - - - -

5 Water to ETP+

catalyst 0.09 - - - ETP

6 Residue - - - -

Total (Ton)

0.09 0.04 1.66 -

1.79

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15. Pyrazolsulfuron Tech.

Process Description

Ethyl-1-methyl-5-Sulfenamideisocyanate-1H-pyrazole-4-carboxylate is reacted with 2-amino-4,6-dimethoxy pyrimidine in presence of Toluene. Crude Pyrazosulfuron is purified by methanol to get pure Pyrazosulfuron (T)

Process Flow diagram of Pyrazolsulfuron

Ethyl-1-methyl-5-sulfenamide

isocyanate-1H-

Pyrazole 4-carboxylate

2-amino-4,6 dimethoxy

Pyrimidine

Toluene

Recd.Tolune

Methanol Recd. Methanol

Pyrazosulfuron

Reactor

Filtration

Purification

Drying & Packing

Packing

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CHEMICAL REACTION PYRAZOLSULFURON

CH3 NH2 N S - N = C= N N Toluene N + C– – CH2CH3 CH3O OCH3 2-amino-4,6-dimethoxy pyrimidine [ 155 ] Ethyl-1-methyl-5-sulfenamide isocyanate-1H-pyrazole-4-carboxylate MW=259 CH3 N OCH3 N N N S – NH – C – NH - N OCH3 C – 0 – CH2CH3 Pyrazosulfuron MW=414

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Materia Balance Pyrazolsufuron

1 Ethyl-1-methyl -5-sulphanamide isocyanide- 1-H pyrazole-

4-carboxylate 0.80

2 2- amino -4,6-dimethoxy pyrimidine 0.490

3 Toluene 3.00

4 Methanol 2.00

Total (Ton) 6.29

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Pyrazosulfuron

Tech. - - 1.00 - Product

2 Toluene - - 2.90 - Recovered & reused

3 Methanol - - 1.93 - Recovered & reused

4 Uncondensed vapor

(Toluene)

- 0.17 - - Loss

5 Uncondensed vapor

(Methanol)

- - - - Loss

6 Residue 0.292 Incinerator

Total (Ton)

00 0.17 5.83 0.292

6.29

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16. Parachlorophenyl alpha isopropyl acetic acid (PCA)

Process Description

Stage – 1

Parachloro Toluene reacted with Chlorine in presence of a catalyst and produced para

chlorobenzylchloride. This para chlorobenzyl chloride reacted with Aqueous sodium cyanide and produced

para chlorobenzyl cyanide. A catalyst is used in this reaction.

Stage-2

Para chlorobenzyl cyanide reacted with Isopropyl bromide, caustic soda and a phase transfer catalyst and

produced 2-(4-chlorophenyl)-methyl butyro nitril (CPIN).

Stage – 3

CPIN is hydrolyzed in dil. sulphuric acid to get CPIA.CPIA then dissolve in hexane crystalysed &

fiter.Materail dried & packed.

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Process Flow Diagram PCA

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CHEMICAL REACTION OF PCA

Stage – 1

CH3 CH2Cl

i

a) + Cl2 + Catalyst-AZDN + HCl

Chlorine

Cl Cl

Parachloro Toluene Para chlorobenzylchloride

MW=126.5 MW=161

CH2 – Cl CH2CN

b) + H2O + NaCN + Catalyst-TEA + NaCl

Sod.chloride [58.5]

Cl Cl Para chlorobenzyl

Cyanide

Para chloroBenzylchloride + Sodium Cyanide (PCBCN)

Stage –2 MW=151.5

CH3 CH3

a) CH

CH2CN CH3 HC—CN

+ CH3 CH – Br + NaOH

+ NaBr+H2O

Sod.bromide

Cl Cl [103]

ParachloroBenzyl cyanide + Isopropylbromide + Sodium hydroxide 4 -chloro phenyl isovaleryl nitril

MW=123 MW=40 MW=193.5

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Remaining part of PCA reaction

b)

CH3 CH3 CH3 CH3

CH CH

HC –CN H C COOH

+ H2SO4 + H2O + Hexane + H2SO4+H2O

Sulphuric +(NH4)2SO4

Cl Acid Cl Amm.sulphate

MW=98 Parachlorophenyl [132]

4-chlorophenyl Isovaleryl nitrile Isopropyle acetic acid

[ 193.5] [ 212.5]

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Material Balance of PCA

S. No. Input/Ton of Product Total Consumption to produce

1 KG.Of parachloro phenyl alpha isopropyl acetic acid Raw Materials

1 Para chloro Toluene 0.810

2 Chlorine 0.463

3 Catalyst –I ( AZDN) 0.004

4 Sodium Cyanide 0.318

5 TEA – II Catalyst 0.017

6 Caustic Lye for ventury + Alkyl 0.521

7 Isopropyle bromide 0.673

8 TEBA Catalyst – III 0.018

9 Caustic Soda Flakes 0.287

10 Sulphuric Acid 1.588

11 Hexane 1.76

12 Water 6.464

Total (Ton) 12.92

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 CPIA - - 1 - Product

2 HCl 30% - - 0.781 - Byproduct

3 Spent acid - - 2.25 - Byproduct

4 Isopropyl bromide

- - 0.02635 - Recovered for Reuse

5 Hexane - - 1.677 - Recovered for Reuse

6 Hexane - 0.083 - - Loss

7 Uncondensed

Vapor - 0.08 - - Loss

8

Spent Sod.

Cyanide aq. Soln.

1.54 - - - To ETP through

detoxification unit

9 NaBr. Soln. 2.014 - - - To ETP through

bromine recovery

10 NaCl+C.S Lye 0.129 - - - To ETP

11 Water 3.173 - - - To ETP

12 Impurities - - - To Incineration

13 Residue - - - 0.165 To Incineration

Total

(Ton)

6.855 0.163 5.732 0.165

12.92

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17. Para chloro benzyl cyanide (PCBCN)

Process Description

Stage – 1

Parachloro Toluene reacted with Chlorine in presence of a catalyst and produced para chlorobenzylchloride. This para chlorobenzyl chloride reacted with Aqueous sodium cyanide and produced

para chlorobenzyl cyanide. A catalyst is used in this reaction.

Process Flow Diagram of PCBCN

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CHEMICAL REACTION OF PCBCN

Stage – 1

CH3 CH2Cl

i

a) + Cl2 + Catalyst-I AZDN + HCl

Chlorine

Cl Cl

Parachloro Toluene Para chlorobenzylchloride

MW=126.5 MW=161

CH2 – Cl CH2CN

b) + H2O + NaCN + Catalyst-II TEA + NaCl

Cl Cl Para chlorobenzyl

Cyanide

Para chloroBenzylchloride + Sodium Cyanide (PCBCN)

[161] [49] [151.5]

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Material Balance of PCBCN

S. No. Input/Ton of Product Total Consumption to produce

1 KG. Of PCBCN Raw Materials

1 Para chloro Toluene 1.022

2 Chlorine 0.584

3 Catalyst (AZDN)- I 0.005

4 Sodium Cyanide 0.401

5 Catalyst (TEA) – II 0.014

6 Caustic for ventury 47% 0.037

7 Water 3.57

Total (Ton) 5.632

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 PCBCN - - 1 - Product

2 HCl 30% - - 0.985 - Byproduct

3 Catalyst -I 0.005 Reused

4 Uncondese

vapour - 0.1037 - Loss

5 Spent Sod. Cyanide aq.

Soln.

1.938 -

- -

To ETP through

detoxification unit

6 NaCl+C.S

Lye+water 0.16 -

- To ETP

7 Water 1.37168 - - - To ETP

8 Residue - - - 0.06896 To Incineration

Total (Ton)

3.47 0.1037 1.99 0.069

5.632

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18. Myclobutanil

Process Description

Parachloro benzyl cyanide is reacted with butyl bromide in presence of base to form 2-(4-chlorophenyl)hexane nitrile.

2-(4-chlorophenyl)hexane nitrile is then reacted with excess dichloro methane in presence of base to form 1-chloro-2-(4-chlorophenyl)-2-cyanohexane.

1-chloro-2-(4-chlorophenyl_-2-cyanohexane is reacted with 1-Sodium-1,2,4-H triazole in presence of base to form Myclobutanil.

Process flow diagram of Myclobutanil

Butyl Bromide

PCBCN Sod. Bromide Soln.

Caustic Soda Soln.

Dichloromethane

Caustic Soda Soln. Sodium Chloride Soln.

1,2,4-Triazole

DMF Sodium Chloride

Caustic Soda Flakes

Water Recd. DMF

Water as Effluent

Myclobutanil

Condensation

Condensation

Condensation

Recovery & Washing

Drying & Packing

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CHEMICAL REACTION OF MYCLOBUTANIL

CH2CH2CH2CH3

CH2CN H – C - CN + CH3CH2CH2CH2Br + NaOH + NaBr + H2O Sod.hydroxide [40] Sod.bromide [103] Cl Cl PCBCN Butyl bromide 2-(4-chloropheny)hexane nitrile MW=151.5 MW = 137 MW = 207.5 CH2CH2CH2CH3 CH2CH2CH2CH3

H – C – C N Cl – CH2- C - CN + Cl – CH2 -Cl + NaOH + NaCl + H2O dichloromethane MW=85 Cl Cl 2-(4-chlorophenyl)hexane nitrile 1-chloro-2-(4-chlorophenyl)-2-cyano hexane MW = 207.5 MW= 256 CH2CH2CH2CH3 CN N

Cl-CH2-C-CN CH3CH2CH2CH2- C –CH2-N N N + N + NaOH + NaCl + H2O N H Cl Cl 1,2,4-Triazole Myclobutanil MW = 256 MW=69 MW=288.5

1-chloro-2-(4-chlorophenyl)-2-cyano hexane

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Material Balance of Myclobutanil

S. No.

Input/Ton of Product Total Consumption to

produce 1 kg Of parachloro

pheny alpha isopropyl acetic acid

Raw Materials

1 Parachloro benzyl cyanide 0.68

2 Butyl Bromide 0.61

3 Dichloro Methane 1.10

4 1,2,4- triazole 0.29

5 Dimethyl formamide 3.00

6 Sodium hydroxide 0.51

7 Water 6.20

Total (Ton) 12.40

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Mucobutanly Tech. - - 1.00 - Product

2 Sodium Bromide Soln.

2.64 - - - Byproduct

3 Recovered Dicloro

Methane - - 0.72 - Recovered & reuse

4 Uncondensed vapour

of dichlor methane - 0.04 - - Loss

5 Recovered DMF - 2.85 - Recovered for

Reuse

6 Uncondensed vapor

of DMF - 0.15 - Loss

7 Sodium chloride - - 0.20 To landfill site

8 Water wash –I 1.64 - - - To ETP

9 Water wash-II 3.16 - - - To ETP

Total (Ton)

7.44 0.19 4.57 0.20

12.40

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19. Tebuconazole Tech.

Process Description

2-[2[(4-chlorophenyl)ethyl]-2-(1,1-dimethyl-ethyl)oxirane is reacted with 1,2,4-Triazole in presence of base using Dimethyl formamide as a solvent to form Tebuconazole.

Dimethyl formamide is recovered and crude product is formed slurry with water and filtered.

Wet cake is dried and packed in suitable packing.

Process flow diagram Tebuconazole

2-[2[(4-chlorophenyl)

Ethyl]-2-(1,1dimethyle-ethyle)Oxirane

1,2,4-Triazole

Sod. Hydroxide

DMF

Recovered DMF

Water

Waste Water to Effluent

Condensation

Filtration & Drying

Washing

Recovery

Tebuconazole

Packing

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CHEMICAL REACTION OF TEBUCONAZOLE

H

N

+ N + NaOH

Cl C N Sod.hydroxide [40 ]

C CH3 1,2,4-Triazole [69]

CH3

CH3

2-[2[(4-chlorophenyl) ethyl]-2-(1,1-dimethyl-ethyl)

Oxirane [ 238 ]

OH CH3

Cl CH CH2 C C CH3 + NaOH

CH2 CH3

N

N

N

Tebuconazole

MW = 307.5

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Material Balance of Tebuconazole

S. No. Input/Ton of Product Total Consumption to produce

1 KG.Of parachloro pheny

alpha isopropyl acetic acid Raw Materials

1 2-[2[(4-chlorophenyl)ethyl]-2-(1,1 dimethyl-ethyl)oxirane 0.86

2 1,2,4-Triazole 0.30

3 Sodium Hydroxide 0.17

4 DMF 4.00

5 Water 3.00

Total (Ton) 8.33

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent

Air

Emission Recovery

Solid

Waste

1 Tebuconazole

Tech. - - 1.00 - Product

2 Recovered DMF - - 3.80 - Recovered and

reuse

3

Unreacted

Sodium

Hydroxide

0.144 - - - To ETP

4 1,2,4-Triazole

Sodium Salt 0.07 - - - To ETP

5 Water formed 0.01 - - - To ETP

6 Impurities 0.11 - - - To ETP

7 Uncondensed

DMF - 0.200 - - Loss

8 Water 3.00 - - - To ETP

Total (Ton)

3.33 0.200 4.80 00

8.33

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20. Imiazethapyre Tech.

Process Description

Diethyl – 5 ethyl pridine -2,3-dicarboxylate and 2-amino-2,3-dimethyl butyramide is reacted with in presence of sodium methoxide. Product is obtained as sodium salt of Imazethapyr then acidified with

HCl to get IMAZETHAPYR (T)

Process Flow diagram Imiazethapyre

Diethyl 5-ethyle

Pyridine-2,3 dicarboxylate

2-amoni-2,3 dimethyl Effluent

Butyramide

Toluene

HCl

Reactor

Filtration & Drying

Imiazethapyre

Packing

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CHEMICAL REACTION OF IMIAZETHAPYRE

NH2 CH3 CH3 COOC2H 5 Sod.methoxide [108] + C – C – CH + 2CH3ONa + 2 HCl Hydrochloric acid N NH2 CH3 (36.5×2) COOC2H5 Diethyl -5-ethyl pyridine – 2 2-amino-2,3-dimethyl -3-dicarboxylate butyramide [ 251] [130] COOH N CH3 N + 2C2H5OH + 2 CH3OH + 2 NaCl Ethanol Methanol Sod.chloride

HN [46 x 2 ] [32x2] [58.5 x 2]

[92] [64] [117]

[289 ]

Imiazethapyr

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Material Balance

S. No. Input/Ton of Product Total Consumption to produce

1KG. Of PCBCN Raw Materials

1 Diethyl-5-ethyl pyridine-2,3-dicarboxylate 1.09

2 2-amino-2,3-dimethyl butyramide 0.59

3 Sodium Methoxide 0.58

4 Toluene 3.50

5 HCl (28%) 1.39

Total (Ton) 7.15

S. No.

Output in Ton /Ton of Product Disposals / ETP

Offsite Recycling Item Liquid

Effluent Air

Emission Recovery

Solid Waste

1 Imazethapyre

Tech. - - 1.00 - Product

2 Toluene - - 3.40 - To ETP

3 Uncondensed vapour

(Toluene)

- 0.100 - - To ETP

4 Ethanol 0.4 - - - To ETP

5 Methanol 0.343 - - - To ETP

6

Unreacted

2-amino-2,3-dimethyl

butyramide

0.030 - - - To ETP

7 Water 1.01 - - - To ETP

8 Sodium

Chloride 0.63 - - - To ETP

9 Residue - 0.25 Incinerator

Total (Ton)

2.40 0.100 4.40 0.25

7.15

Bromine Recovery

Potassium or sodium bromide solution obtained from different products are acidified with hydrochloric acid or sulphuric acid as per requirement & acidified aqueous is taken for bromine recovery by passing chlorine

at higher temperature.

Detoxification of Spent Sodium Cyanide Aqueous

Caustic soda lye & spent sodium cyanide is charged in vessel, then chlorine is passed at low temperature,

sodium hypo chlorite is formed in citu which reacts with sodium cyanide &destroy to nitrogen ,sod

chloride & sodium carbonate.

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Annexure 1: Raw Material & Products Storage Details

Table 1: Details of Raw Material & Product

Sr. No

Chemical State Consumption, (MT/Annum

Hazard Involved Means of Storage

Operating Condition (Storage)

No of Drum

or Vessel

Packing size

Max. Storage Capacity

(MT) Press

(Kg/Cm2) Temp (0C)

Raw Materials

1

2(4(chlorophenyl )-2-chlorophenyl) 2-

bromomethyl-4methyl -1,3 dioxolone

Liquid 64.50 Non-Hazard M.S. Drum Ambient Ambient 100 200 kg. 20

2

2-[2[(4-chlorophenyl)ethyl]-2-(1,1-

dimethyl-ethyl)oxirane Liquid 43.00 Non-Hazard M.S. Drum Ambient Ambient 100 200 kg. 20

3 1,2,4-triazole Solid 31.85 - Fiber Drum Ambient Ambient 400 50 Kg. 20

4 5-amino-3-cyno-1-(2,6-dichloro-4-trifluoro methyl

Pheny)-1H-pyrazole

Solid 9.30 Lachrymator Fiber Drum Ambient Ambient 280 25 Kg. 7

5 2-amino-4,6-dimethoxy

pyrimidine Solid 9.82 - Fiber Drum Ambient Ambient 160 50 Kg. 8

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Sr.

No. Chemical State Consumption,(MT/Annum

Hazard

Involved

Means of

Storage

Operating

Condition

(Storage) No of

Drum

or Vessel

Packing size

Max.

Storage

Capacity (MT)

Press

(Kg/Cm2)

Temp

(0C)

6 3,4-dichloroaniline Solid 37.50 - Poly Bag Ambient Ambient 800 25 Kg. 20

7 Dichloromethane Liquid 16.50 Flammable MS storage

tank Ambient Ambient 1 10 KL 10

8 Diethyl-5-ethyl pyridine-2,3-

decarboxylate Solid 27.25 Non-Hazard Fiber Drum Ambient Ambient 400 50 Kg. 20

9 Ethyle-1-Methyl-5-sulfinamide isocyanate-

H,pyrazole-4-carboxylate

Solid 16.00 Toxic Fiber Drum Ambient Ambient 240 50 Kg. 12

10 2-amino-2,3-dimethyl

butyamide Solid 14.75 Non-Hazard Fiber Drum Ambient Ambient 200 50 Kg. 10

11 2-Heptanol Liquid 11.40 Toxic MS Drum Ambient Ambient 58 170 Kg. 9.86

12 5-chloro-8-hydroxy

quinolone Solid 16.8 Non-Hazard HDPE bags Ambient Ambient 416 30 kg. 12.48

13 2-chloro-5-chloromethyl thiazole (CCMT)

Liquid 210.00 Lachrymator HDPE drum Ambient Ambient 80 250 Kg. 20

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 75

Sr.

No. Chemical State

Consumption,(MT/An

num

Hazard

Involved

Means of

Storage

Operating

Condition

(Storage)

No of

Drum

or Vessel

Packing size

Max.

Storage

Capacity (MT)

Press (Kg/Cm2)

Temp (0C)

14

3-methyl-4-nitro per

hydro,1,2,5

oxadiazene(MNPO)

Solid 210.00 - Fiber Drum Ambient Ambient 800 25 Kg. 20

15 2(4-hydroxy phenoxy

propionic Acid)HPPA) Solid 61.00 Fiber Drum Ambient Ambient 400 50 Kg. 20

16 5-Chloro 2,3 difluro pyridine (CDFP)

Liquid 52.00 - M.S. Drum Ambient Ambient 100 200 20

17 Copouros chlorite Solid 5.58 - HDPE bags Ambient Ambient 100 20 2

18 4-dimethyl amino pyridine Solid 3.000 Lachrymator Fiber Drum Ambient Ambient 80 25 Kg. 2

19 Methanol Liquid 537.00 MS storage

tank Ambient Ambient 1 30 KL 30

20 Acetic Acid Liquid 144.50 - HDPE drum Ambient Ambient 25 200 Kg. 5

21 Ammonia ( solution 20% ) Liquid 0.30 - HDPE drum Ambient Ambient 4 50 Kg. 0.2

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 76

Sr.

No. Chemical State

Consumption,(

MT/Annum

Hazard

Involved

Means of

Storage

Operating Condition

(Storage) No of

Drum or Vessel

Packing size

Max. Storage

Capacit

y (MT) Press

(Kg/Cm2) Temp (0C)

22 Aluminium Chloride Liquid 2116.80 Evalution of

HCl gas bags Ambient Ambient 1000 25 Kg. 25

23 Benzaldehyde Liquid 1283.40 HDPE drum Ambient Ambient 200 200 Kg. 40

24 Bifenthrin Alcohol Solid 68.40 bags Ambient Ambient 800 25 Kg. 20

25 Bromine Liquid 1062.00 Toxic Glass Bottle Ambient Ambient 6666 3 kg. 19.98

26 Butyl Bromide Liquid 9.15 Inflammable MS Drum Ambient Ambient 30 250 kg. 7.5

27 Catalyst MR liquid 0.45 - HDPE drum Ambient Ambient 5 50 Kg. 0.25

28 Catalyst –H Liquid 0.15 - HDPE drum Ambient Ambient 1 100 kg. 0.1

29 Caustic Soda Flakes Solid 462.85 Corrosive HDPE bags Ambient Ambient 200 50 kg. 10

30 Caustic Lye ( 47%) Liquid 709.02 Corrosive MS storage

tank Ambient Ambient 2 20 KL 36

31 Chlorine Gas 671.50 Toxic Cylinder Ambient Ambient 22 900 kg. 19.8

32 Azobis Isobutaronitrile

Solid 1.90 Fiber Drum Ambient Ambient 50 20 kg. 1

33 Cypermethrin Acid

Chloride Liquid 347.750 -

Plstic coated

MS. Drums Ambient Ambient 72 250 kg. 18

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 77

Sr.

No. Chemical State

Consumption,(MT/A

nnum

Hazard

Involved

Means of

Storage

Operating Condition

(Storage) No of Drum

or Vessel

Packing size

Max. Storage

Capacity (MT)

Press (Kg/Cm2)

Temp (0C)

34 Di isopropyl Amine Liquid 12.00 - MS Drum Ambient Ambient 35 140 kg. 4.9

35 Di isopropyl phenoxy

phenyl thio urea Solid 145.50 - HDPE bags Ambient Ambient 400 50 Kg. 20

36 Dimethyl Formamide (DMF) Liquid 1963.70 - MS Drum Ambient Ambient 150 200 kg. 30

37 Ethylene Dichloride (EDC) Liquid 5386.80 Toxic MS storage tank Ambient Ambient 1 40 KL 30

38 Hexane Liquid 2656.20 Fire hazard MS storage tank Ambient Ambient 2 20 KL 25

39 Formic Acid Liquid 45.00 - HDPE drum Ambient Ambient 142 35 kg. 4.97

40 Hydrochloric Acid (30%) Liquid 780.90 Corrosive HDPE storage

Tank Ambient Ambient 2 20 KL 20

41 Isoprypyl Alcohol Liquid 237.00 Fire hazard MS storage tank Ambient Ambient 1 30 KL 25

42 Isoprypyl Bromide Liquid 237.50 Toxic HDPE drum Ambient Ambient 80 250 Kg. 20

43 Lambda Acid Solid 240.60 Toxic HDPE bags Ambient Ambient 1200 25 kg. 30

44 Lambda Powder (seeding) Solid 6.00 irritated hdpe drum Ambient Ambient 125 40 kg. 5

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 78

Sr.

No. Chemical State

Consumption,(MT/A

nnum

Hazard

Involved

Means of

Storage

Operating Condition

(Storage) No of Drum

or

Vessel

Packing size

Max. Storage

Capacity

(MT) Press

(Kg/Cm2)

Temp

(0C)

45 Metaphenoxy Benzaldehyde Liquid 529.050 Toxic HDPE drum Ambient Ambient 180 200 kg. 36

46 Metaphenoxy benzalalcohol Liquid 52.00 Toxic hdpe drum Ambient Ambient 88 225 kg. 19.8

47 Monochloro Acetic Acid Solid 9.30 Toxic HDPE bags Ambient Ambient 160 50 kg. 8

48 Mono Ethyl Glycol Liquid 1440.00 Toxic MS storage

tank Ambient Ambient 1 30 KL 30

49 n-methyl pyrolidine (NMP) Liquid 44.40 Toxic HDPE drum Ambient Ambient 100 200 kg. 20

50 Orthoxylene Liquid 34.85 Fire hazard MS storage

tank Ambient Ambient 1 30 KL 10

51 Parachloro Benxyl cyanide Liquid 10.20 lachrymator HDPE drum Ambient Ambient 40 200 kg. 8

52 Parachloro Toluene Liquid 88.70 Fire hazard M.S. Drum Ambient Ambient 150 200 kg. 30

53 Paratolune sulphonic acid

(PTSA) Solid 1.80 - HDPE bags Ambient Ambient 24 50 1.2

54 Phenol Solid 1062.00 Corrosive MS storage

tank Ambient Ambient 1 30 KL 30

55 Potassium Carbonate Solid 186.90 Fire hazard HDPE bags Ambient Ambient 800 25 kg. 20

56 Potassium Hydroxide (KOH) Solid 702.00 - HDPE bags Ambient Ambient 800 50 Kg. 40

57 Propargyl alcohol Liquid 30.00 - MS Drum Ambient Ambient 111 180 kg. 19.98

58 Propionic Acid Liquid 51.50 - HDPE drum Ambient Ambient 100 200 kg. 20

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 79

Sr.

No. Chemical State

Consumption,

(MT/Annum

Hazard

Involved

Means of

Storage

Operating Condition (Storage) No of

Drum or Vessel

Packing size

Max. Storage Capacity (MT)

Press (Kg/Cm2)

Temp (0C)

59 Sodium methoxide Solid 14.5 corrosive HDPE drum Ambient Ambient 80 50 kg. 4

60 Soda Ash Solid 86.00 Toxic HDPE bags Ambient Ambient 200 50 kg. 10

61 Sodium bicarbonate

(NaHCO3) Solid 3.00 - HDPE bags Ambient Ambient 40 50 kg. 2

62 Sodium Thiosulfite Solid 25.56 Highly toxic HDPE bags Ambient Ambient 100 50 kg. 5

63 Sodium Cyanide Solid 302.00 Highly toxic MS Drum Ambient Ambient 400 50 kg. 20

64 Sodium Hypo Chlorite Liquid 242.80 - HDPE storage

Tank Ambient Ambient 1 15 KL 20

65 Sulphuric Acid 70% wash Liquid 15.00 Corrosive HDPE drum Ambient Ambient 16 250 Kg. 4

66 Sulphuric Acid Liquid 618.50 Corrosive MS storage tank Ambient Ambient 1 30 KL 30

67 Tertiary butyl amine Liquid 34.50 corrosive M.S. Drum Ambient Ambient 75 200 15

68 Thionyl chloride Liquid 286.60 Corrosive/tox

ic MS drum Ambient Ambient 100 300 kg. 30

69 Toluene Liquid 3352.70 Fire hazard MS storage tank Ambient Ambient 2 20 KL 30

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 80

Sr.

No. Chemical State

Consumption,

(MT/Annum

Hazard

Involved

Means of

Storage

Operating Condition (Storage)

No of Drum

or

Vessel

Packing size

Max. Storage

Capacity

(MT) Press

(Kg/Cm2)

Temp

(0C)

70 Triethylamine (TEA) Liquid 19.70 - MS Drum Ambient Ambient 66 150 kg. 9.9

71 Trifloromethan sulfinyl chloride

Liquid 49.00 - Coated MS

drum Ambient Ambient 400 50 kg. 20

72 Trimethyle amine hydrochloride

Solid 49.00 Toxic HDPE bags Ambient Ambient 400 25 kg. 10

73 Triethyl benzyl ammonium chloride

Solid 20.60 Lachrymator HDPE drum Ambient Ambient 25 200 kg. 5

TOTAL 29255.98 20515 1236.94

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 81

Sr. No.

Chemical State Production , (MT/Annum

Hazard Involved

Means of Storage

Operating Condition

(Storage) No of

Drum or

Vessel

Storage Capacity

Max.

Storage Capacity

(MT) Press

(Kg/Cm2) Temp (0C)

PRODUCTS

1 Alpha Cypermethrin Solid 100 Toxic Fiber Drum Ambient Ambient 100 50 Kg. 5

2 Bifenthrin Technical Solid 120 Toxic MS drum Ambient Ambient 50 200 kg. 10

3 Clodinafop Technical Solid 100 Toxic Fiber Drum Ambient Ambient 500 40 kg. 20

4 Cypermethrin Technical Liquid 350 Toxic MS Drum Ambient Ambient 180 200 Kg. 36

5 Difenthiuron Technical Solid 150 Toxic Fiber Drum Ambient Ambient 400 40 kg. 16

6 Difenconoazole Solid 50 Toxic Fiber Drum Ambient Ambient 200 50 kg. 10

7 Fipronil Technical Solid 100 Toxic Fiber Drum Ambient Ambient 125 40 kg. 5

8 Fenvalerate Technical Liquid 300 Toxic MS Drum Ambient Ambient 100 200 kg 20

9 Imiazethapyre Technical Solid 25 Toxic Fiber Drum Ambient Ambient 100 50 kg. 5

10 Lambda Cyhalothrin

Technical Liquid 300 Toxic M.S. Drum Ambient Ambient 100 200 kg.

20

11 Metaphenoxy Benzaldehyde Liquid 1800 Toxic HDPE drum Ambient Ambient 160 225 kg. 36

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 82

Sr. No.

Chemical State Consumption, (MT/Annum

Hazard Involved

Means of Storage

Operating Condition

(Storage) No of

Drum or

Vessel

Storage Capacity

Max.

Storage Capacity

(MT) Press

(Kg/Cm2)

Temp

(0C)

12 Myclobutanil Technical Solid 15 Toxic Fiber Drum Ambient Ambient 20 50 Kg. 1

13 Para Chlorophenyl isopropyl

acetic acid Solid 200 Toxic HDPE bags Ambient Ambient 40 500 kg. 20

14 Para Chloro benzyl cyanide Liquid 100 Toxic HDPE drum Ambient Ambient 90 200 kg. 18

15 Permethrin Technical Liquid 100 Toxic MS Drum Ambient Ambient 50 200 kg. 10

16 Propanil Technical Solid 50 Toxic MS Drum Ambient Ambient 50 200 kg. 10

17 Pyrizolesulfuron Technical Solid 20 Toxic Fiber Drum Ambient Ambient 40 50 2

18 Safener ( CloquintocetMexyl Solid 30 Toxic Fiber Drum Ambient Ambient 125 40 kg. 5

19 Thiamethoxam Technical Solid 300 Toxic Fiber Drum Ambient Ambient 625 40 kg. 25

20 Tebuconazole Solid 50 Toxic Fiber Drum Ambient Ambient 40 50 kg. 2

TOTAL 4260 3585 298

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BHARAT RASAYAN LTD. FORM 1

BHARAT RASAYAN LTD. 83

Sr. No.

Chemical State Consumption, (MT/Annum

Hazard Involved

Means of Storage

Operating Condition

(Storage) No of

Drum or

Vessel

Storage Capacity

Max.

Storage Capacity

(MT) Press

(Kg/Cm2) Temp (0C)

LIST OF BYPRODUCTS

1 Alum Liquid 9536.4 Corrosive HDPE

storage Tank Ambient Ambient 3 20 KL 60 KL

2 Pot. Chloride Liquid 5036.5 Corrosive HDPE

storage Tank Ambient Ambient 2 20 KL 40 KL

3 Spent Acid Liquid 824.95 Corrosive HDPE

storage Tank Ambient Ambient 2 20 KL 40 KL

4 Hydrochloric Acid 28% Liquid 2236.2 Corrosive HDPE

storage Tank Ambient Ambient 2 20 KL 40 KL

5 Sodium Sulfite Liquid 1427.1 Corrosive HDPE

storage Tank Ambient Ambient 2 20 KL 40 KL

6 Potassium bromide (soln) Liquid 3726.7 Corrosive MS storage

tank Ambient Ambient 1 40 KL 40 KL

7 Sodium Bromide (soln) Liquid 758.6 Corrosive MS storage

tank Ambient Ambient 2 20 KL 40 KL

23499.26 14 300 KL

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 84

Annexure 2: Waste Water Generation Details

S.

No. Area

Effluent Generation in KLD

Disposal Mode Existing

After Product Mix

1 Domestic 30 35 To STP & used for

Gardening

2 Industrial Process 34.43 35.62 To Pretreatment & MEE. Condensate of MEE to

ETP Washing 2.0 3.0

Cooling 4 5 Condensate of MEE and

outlet of Utilities will be treated in ETP and

finally reused in plant Boiler 5 6

Total (Industrial) 45.43 49.62

Total Waste Water

Generation KL/Day 75.43 84.62

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 85

Annexure 3: Waste Water Treatment Plant Details

Details of Existing Effluent Treatment Plant

M/s. Bharat Rasayan Limited have an Effluent Treatment Plant consisting of primary, secondary and tertiary treatment units. The effluent confirming the SPCB standards shall be collected in the tank

before it is reused.

Process Description: ETP

For the proposed pesticide manufacturing unit, the raw water will be utilized for Processing, Cooling,

Washing, Boiler, Scrubber and domestic purpose. The effluent generated from the same sources will be sent to Proposed Evaporation System. Water will be evaporated, condensed and recycled to

process/scrubber/sent to proposed ETP. After recovery of solvent from mother liquor, water will be

sent to ETP. The biodegradable effluent will be sent to ETP.

Primary Treatment:

The biodegradable effluent is first passed through the Oil & Grease tank to remove oil & grease content from the effluent. The effluent is equalized & neutralized by addition of either acid or caustic.

The pH will be adjusted to 6.5 (range 6.5 to 9.5). the mixing is provided by air diffusion. There will is a one no. of equalization tanks, then mass from equialsation tank is taken to neutralization reactor for

pH maintaining. Once pH is achieved, then the neutralized wastewater is collected into settling cum

clarifier and then transferred to sludge drying bed &water to holding tank. From holding tank water is taken to MEE for distilling water.

Secondary Treatment:

Condensed Water from MEE is taken to storage tank for it. From storage tank water is taken to

charging overhead tank. From overhead tank it is taken to aeration tank for aeration for biological

treatment. For biological treatment two no of tanks are provided. Each tanks is fitted with fine bubble diffuser & air is provided by blower. From biological tank partial mass is taken in clarifier for

decanting clarifier water in holding tank. Sludge from bottom of clarifier is recycle & partial sludge is filtered by filter bed. Sludge is send to TSDF site .

Tertiary Treatment:

For the finishing of the treated effluent getting from the overflow of the clarifier, tertiary treatment

will be introduced. The overflow of the clarifier tank is overflow by gravity to a collection tank from

where it is passed through pressure sand filter & activated carbon filter. The final treated effluent is collected in collection tank and is reused

Details of Units of ETP

Sr. No. Name of Unit Dimension No. of Units

1. Equalization Tank 8.7 x 8.7 X 2.13 1

2. Neutralization Tank with coarse diffuser

3.1 x 3.1 x 2.13 1

3. Lime Dosing Tank 5000 ltrs 1

4. Flocculation & reaction reactor 10000ltrs 1

5. Primary Clarifier – I 28000 ltrs 1

6. Intermediate Collection Tank 10.0 X6.5X2.3 1

7. Aeration Tank – I 10.0 X6.5X2.3 1

8. Aeration Tank – II 8 X 8 X 2.5 1

9. Secondary Settling tank – I 15000 ltrs 1

10. Intermediate tank 6000 ltrs 1

11. Dual Media Filter 5 m3 1

12. Carbon bed filter 2 m3 1

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 86

Sr. No. Name of Unit Dimension No. of Units

13. Treated Water tank 20000 ltr 1

14. Sludge Sump 5.1 x 5.1 x (2.5 + 0.5) 1

15. Filter Press - 1

Evaporation System

Process Description:

The feed effluent is preheated by using hot condensate coming from the evaporator. The effluent is fed to continuous multiple effect evaporator and the effluent concentrated continuously by using

steam as heating medium to the first effect. The evaporated and condensed water is recycled to Scrubbers / ETP.

The evaporation is carried till the inorganic salts is start crystallizing in the evaporator and slurry is formed. The slurry of salts and effluent is withdrawn and fed to a Nutsche Filter for separating the

solids. Two Nutsche filters will be provided to sustain continuous operation. The solids coming from the Nutsche filter will be manually scooped and dumped to GEIPL , Pali (nearest TSDF site).

Details of Effluent Treatment PlantS

PRE-TREATMENT UNITS: 1. Screening Chamber: 1 No.

Effluent generated from various production areas will be collected into a screen chamber via gravity /

pumping. Screening Chamber will be made of RCC with internal acid proof brick lining since the pH of

incoming effluent is acidic in nature. The chamber will be provided with fine screens – MS FRP lined for arresting the floating matter and large size suspended matter. From this chamber the effluent will

flow under gravity to Oil & Grease Trap Unit.

2. Oil and Grease Trap: 1 No.

Effluents from screening chamber will overflow to an Oil & Grease Trap under gravity. Oil and Grease chamber is baffle walled tank. Oil and Grease collected is removed manually by scrapping and shall

be disposed off as Hazardous wastes (waste oils) which shall form a part of Hazardous solid wastes

along with ETP Sludge.

3. Equalization cum Neutralization Tanks: 1 Nos.

Overflow from Oil & Grease Trap will be taken to Equalization cum Neutralization Tanks under gravity. The prime purpose of these tanks is for collection and storage of effluents generated and to

have proper equalization of effluents in order to have constant load onto the further treatment units.

This is designed as PROCESS for operational ease. This equalized effluent will be further subjected to lime, alum & poly dosing for neutralization cum flocculation. A reactor is used for pH adjustment /

primary treatment of flocculation and precipitation.

Course Bubble Aeration grid with Twin lobe blower system is provided in this tank for mixing the

effluents for proper equalization and keeping the tank contents into suspension.

Dosing of Lime, Alum & poly shall be carried out in the reactor for neutralization and flocculation.

From this reactor, the flocculated effluent shall be further transferred to Primary Settling Tank for

settlement of chemical sludge.

Dosing of chemicals is carried out by means of three HDPE open top dosing tanks each for lime,

alum & poly. 10% concentration of Lime, Alum & 2% Poly solution shall be prepared in these dosing tanks. The tanks are of made of HDPE / FRP

4. Primary Settling Tank - 1: 1 No.

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 87

The flocculated effluents from Equalization cum neutralization reactor will be pumped directly into

Primary Settling tank for removal of the chemical sludge by settling.

This chemical sludge falls under the Hazardous Waste Category as per the Hazardous Waste

Management and Handling Rules. The sludge will be directly taken to Sludge Drying Beds and further temporarily stored in HDPE/LDPE bag packing in the Hazardous Waste Storage Shed provided in the

ETP area. The sludge will be finally disposed off into a secured landfill site. The supernatant from the

primary settling tank will be further conveyed under gravity to the Intermediate Collection Tank.

5. Intermediate Collection Tank - 1: 1 No

An Intermediate Collection Tank – 1 will be provided for collection of supernatant from Primary settling tank. From this Feed Tank, the equalized and primarily treated effluents shall be pumped to

the 1st Unit of MEE i.e. Solvent Stripper for stripping of solvents which will further pass through Multi Effect Evaporator.

MEE System: Multi Effect Evaporator with Solvent Stripper & Nutch Filter: 50 KL Capacity – Total 1

Solvent Stripper and MEE System are proposed to evaporate the neutralized effluents of process +

washings. The Solvent Stripper removal the low boiling point solvents and the MEE will generate residue and condensate. MEE system will be designed to cater for high TDS by selection of suitable

material for Calandria Tubes. The system will be designed with Thermo Vapour Compressor with

Three to four stage of Falling Film or Forced Circulation Evaporation System. The concentrate solids will be filtered out in a nutch filter whereas the filtrate will be recycled back into the system. MEE

Condensate will be collected into the Collection Tank of Post Treatment Units.

Solids from MEE will be collected and packed in bags for intermittent storage in Hazardous Waste

Storage area in ETP. They will be further dispose off into Secured Landfill site.

POST TREATMENT UNITS:

Condensate from MEE plant is taken in a storage tank,from storage tank it is taken in charging tank from charging tank condensate is charged in biological treatment tank. Biological treant tank is fitted

with fone bubble air diffuser. These diffuser are connected with root blower. After aeration treated mass is transferred to clarifier, overflow of clarifier is collected in a tank. Sludge is transferred back

to biological tank. Part of sludge is transferred to filter. Which collected & send to TSDF.

1. Pressure Sand Filter:

Pressure Sand Filter will be provided as a form of tertiary treatment for removal of residual suspended solids. The filter is consist of different gradations of gravel & sand bed. The filter is

provided with necessary valve arrangements for inflow and outflow and backwashing of the system.

The backwash water from the system will be taken to the Equalization cum Collection tank for re-treatment.

2. Activated Carbon Filter:

Activated Carbon Filter will be provided as a form of tertiary treatment for removal of residual

organics, odor, color & organic TDS by means of adsorption process. The filter will consist of

gradations of gravel & sand sub bed and over which is provided activated carbon of high iodine value. The filter will be provided with necessary valve arrangements for inflow and outflow and

backwashing of the system. The backwash water of the system shall be taken to the Equalization cum Collection Tank for re- treatment. The sand and activated carbon filters are provided as part of

tertiary polishing treatment for catering to residual pollution load in order to meet the specified disposal norms.

Outlet of PSF and ACF will be taken to Final Collection Tank (Guard Pond) for storage to be further

use in plant .

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 88

3. Sludge Drying Beds:

The chemical sludge formed in physio-chemical treatment from primary settling tank will be directly

collected in Sludge Drying Beds.

The sludge drying beds will be divided into compartments to facilitate in easy sludge drying handling and disposal. The dried sludge falls under hazardous waste category and should be filled in

HDPE/LDPE bags and finally disposed to a secured landfill. Leachate from Sludge Drying Bed will be collected in leachate collection sump and pumped back to equalization cum collection tanks.

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 89

Block Diagram of ETP (100 KLD):

Polyelectrolyte

Lime

Plant –A+B

Plant - C

For Plant use

Oil Separator Retention Pond for treated cyanide

Skimmer

Lime sludge beds

Size: 4 x 3 x 1 m

8.6x8.6x1.7m ETP water collection Tank

MEE Plant

Pond No.2

8.6x8.6x1.7m Equalization Tank with Cost Diffuser

Neutralization R-702

Cap.10Kl

Primary settler Cap.28 KL

Pond No.3

Airation

10x6.5x1.7m

MEE distill

water 20 KL

Pond No.9

43.3x24x .4

Feed Tank

4 KL

Biological Airation

Pond No.1 – 150 KL

Biological Airation Pond No.2 (10x6.5x1.5m)

Carbon Filter Media Filter

Clear Water Holding

Tank Cap.20 KL

Pond No.10

24x3x1 Pond No.11

42x26.7x1.85

Pond No.12

42x25.5x2.85

Solid waste

Residue storage Shed (13x7x1.5)

Size:16x13x1.5

Lime Sludge Storage Shed

Size: 10 x 23 x 3

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FORM 1

BHARAT RASAYAN LTD.

BHARAT RASAYAN LTD. 90

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FORM 1

BHARAT RASAYAN LTD.

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Annexure 4: Water Consumption Details

S.

No. Area

Water Consumption in KLD

Existing After Product Mix

1 Domestic 30 35

2 Industrial Process

48.004 66.719

3 Washing 2.0 3.0

4 Cooling 20.0 30

5 Boiler 50.0 60

Total (Industrial) 150.004 194.719

Gardening 30.0 40

Total Water Consumption KL/day 180.004 234.719

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Annexure 5: Fuel Consumption

S. No.

Name of Fuel Consumption

Existing After Product Mix

1

Furnace Oil

5.5MT/Day 6.5 MT/Day

2 Coke 8.5MT /day 10 MT/Day

3 HSD* 0.85 MT/Day 1 MT/Day

*For emergency use only in DG Set

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Annexure 6: Hazardous Waste Generation

Sr. No. Type of Waste

Category

as per HW

TOTAL QUANTITY, MT/Year

Treatment / Disposal Method

Existing After

Product

Mix

1. Used Oil 5.1 0.726 1

Collection, Storage, Transportation & Disposal

by selling to registered reprocessor / reuse as

lubricant

2.

Process Waste / Waste Residue containing

Pesticides

29.1 229.42 529.22

Collection, Storage,

Incineration at common Incineration / Disposal of

Incinerable waste to Cement Industry

3. ETP Sludge 29.2 1236 1550.0

Collection, Storage, Transportation & Disposal

at nearest TSDF site (GEIPL, Pali) / Sludge from

Primary Treatment to Cement Industry

4. Date Expired / off specification

products

29.3 Nil 1.0 Collection, Storage,

Incineration at common

incineration

5. Discarded Container

33.3 3000 Nos. 5000 Nos. Collection, Storage, Decontamination,

Detoxification & sell to authorized vendor 6.

Discarded bag / liners

33.3 3 4

7.

Distillation

Residue from contaminated

organic solvents

36.4 0 0 Collection, Storage,

Incineration at common

incinerator

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Annexure 7: Stack Details

Flue Gas Stacks

Stack Attached to Sources Stack Height, m Stack Top Dia, m

Existing

Boiler 1 30 1M

DG Set–I (1250 KVA) 11 300mm

DG Set – II (275 KVA) 11 300mm

After Product Mix

Boiler 1 30 1M

DG Set–I (1250 KVA) 11 300mm

DG Set – II (275 KVA) 11 300mm

Thermic Fluid Heater 30

Process Vents

Stack Attached to Stack height in m

Existing

Process Vent – I 15

Process Vent – II 15

Process Vent- III 15

Process Vent- IV 15

After Product Mix

Process Vent – I 15

Process Vent – II 15

Process Vent- III 15

Process Vent –IV 15