annexure-i list of products filem/s. metachem industries, khambhat 1 annexure-i list of products sr....

M/s. Metachem Industries, Khambhat 1

Annexure-I

List of Products

Sr. NO. Name of the Product MT/Month

(A) Reactive Dyes 1 Reactive Blue 198. 50 2 Reactive Blue FNG. 50 3 Reactive Blue 19. 40 4 Reactive Blue 49. 50 5 Reactive Blue 220 50 6 Reactive Blue 221 50 7 Reactive Blue 222 50

Total (A) 340 (B) Dyes Intermediates

8 PNCBOSA 30 9 Chloranil Condense 30 10 Blue HEGN (198) Base 25 11 Aniline 2:4 DSA. 30 12 Aniline 2:5 DSA 30 13 Oxy-Sulphone 30 14 M. Acid 20 15 Blue - 49 BASE 20 16 Metanillic acid 20 17 4-Sulpho Anthralinic Acid 50 18 4-Sulpho Hydrazone 50 19 Sulpho O.A.V.S./ Sulpho V.S./ Sulpho J- Acid/

Sulpho Gamma Acid 30

20 3;5 DABA 10 Total (B) 375

Total (A + B) 715


List of Raw Materials

Sr. no.

Product name Raw Materials Name MT/Month

1 Reactive Blue 198 (HEGN)

Blue HEGN (198) W/C 54.50 Soda Ash 21.0 Aniline 2:4 DSA 10.0 Cy. Chloride 8.25 S.B.C. 4.75 Celsolin Oil 0.50

2 Reactive Blue FNG Blue Base 198 W/C 63.50 Soda Ash 30.0 Aniline 2: 5 DSA 14.0 Cynuric Chloride 10.40 Celsolin Oil 0.50 MBVS Ester 15.0 Sodium Bicarbonate 11.50

3 Reactive Blue 19 Oxy Sulphone 31.0 Oleum (23%) 32.0 Sulfuric Acid (98%) 7.6 Salt 34.8 CaCO3 6.4 Oxilic Acid 3.6 Soda Bicarbonate 4.0

4 Reactive Blue 49 Blue 49 W/C 27.5 Soda Ash 10.0 Cy. Chloride 5.0 Metanilic Acid 5.0

5 Reactive Blue 220 Sulpho OAVS 13.5 Sodium Nitrite 3.5 HCl (30%) 27.5 4-Sulpho Hydrazone 19.5 Caustic Lye (48%) 4.5 Soda Ash 5.0

6 Reactive Blue 221 6-Acetyl OAPSA 11.5 CS Lye (48%) 2.0 HCl (30%) 61.5 Sodium nitrite 3.5 Sulphamic acid 0.1 Sodium acetate 5.0 Soda Ash 10.0 4-Sulpho Hydrazone 15.0 Copper sulphate 12.5 CS Flakes 16.0 Salt 32.5


Cyanuric Chloride 7.5 Tamol 0.4 N-Ethyl MBVS 12.8 Soda Bi Carb 7.8 Dicamol 2.3

7 Reactive Blue 222 MPDSA 6.8 Cyanuric Chloride 6.6 Soda ash 6.5 Celsolin Oil 0.2 M.B.V.S. 10.0 NaHCO3 6.5 NaNO2 5.0 HCl (30%) 18.0 H-Acid 10.5 Sodium Acetate 14.8 S. T. A. 10.0

Dyes Intermediates 8 PNCBOSA PNCB 21.5

65% Oleum 23.6 Salt 30.0

9 Chloranil Condense

E.D.A. 150.0 PNCBOSA 30.0 SBC 16.2 HCl (30%) 45.0 Ac. Acid 3.0 C.I.P. 15.0 Soda Ash 15.0 Chloranil 12.0

10 Blue HEGN (198) Base

Sulfuric Acid (98%) 9.4 Oleum (23%) 70.0 Chlo. Cond. 25.0 Sodium per Sulfate 18.8

11 Aniline 2, 4 DSA Sulphanilic Acid 25.5 Oleum 23% 75.0

12 Aniline 2, 5 DSA Metanilic Acid 25.5 Sulfuric Acid (98%) 30.0 Oleum 65% 36.0 Hyflow 0.3 Activated Carbon 1.4 Sodium Sulphate 25.5

13 Oxy Sulphone Bromamine Acid 25.5


M.B. V.S. Acid 16.5 Soda Bi carbonate 25.5 CUCl2 0.3 Celsolin Oil 0.3 Copper Bronze 0.2 HCl (30%) 60.0 Salt 7.5

14 M. Acid Macitinline Acid 11.4 H2SO4 56.0 W.N.A. 17.6 NaOH 3.0 Iron Powder 30.0 Ac. Acid 7.0 Soda Ash 7.0 Ac. Carbon 0.5 HCl 30.0 Hydro Powder 0.3

15 Blue 49 Base Bromamine Acid 20.0 M-Acid 32.5 Soda Ash 13.6 Cuprous Oxide 2.0 Celsolin Oil 0.3 Coomon Salt 7.6 Dicamol 0.8 N2 Gas 1.3 HCl (30%) 54.0

16 Metanilic Acid Nitro benzene 18.0 Oleum (65%) 19.6 Soda Ash 1.0 Lime Stone Powder 22.0 Iron Powder 2.5 HCl (30%) 2.0 Soda Ash 3.5 Sulphuric Acid 1.8

17 4 SulphoAnthranilic Acid

O.N.T. 90.0 Oleum (65%) 99.0 Sulfuric Acid (70%) 175.0 NaOH 107.5

18 4 Sulphohydrazene

4 SulphoAnthranilic Acid 50.0 HCl (30%) 110.0 Sodium Nitrite 15.0 Sodium bisulphite 42.5 Caustic Soda 24.0 Benzaldehyde 30.0

19 Sulfo OAVS OAVS 37.5 Oleum Acid (65%) 66.4 Sulphuric Acid 54.4


KCl 19.5 20 3,5 DABA Benzoic Acid 12.0

Nitric Acid 10.9 Sulphuric Acid(98%) 23.4 Iron Powder 16.4 HCl (30%) 19.5 Soda Ash 9.0


Annexure-II

Manufacturing Process

(A) Reactive Dyes

1. Reactive Blue 198 Manufacturing Process:

Blue 198(HEGN) base W/C condensate with Cynuration of aniline 2:4 DSA& then

clarify, standardize& spray dryer.

Chemical Reaction:


Mass Balance:

INPUT KG OUTPUT KG

Blue HEGN (198) W/C 1090Soda Ash 50Water 3700

Aniline 2:4 DSA 200Soda Ash 120Cy. Chloride 165S.B.C. 95Celsolin Oil 10Ice 1800Water 1000

Soda Ash 250

RO permeate reuse 4180

Drying loss 3300Reactive Blue 198 (HEGN) 1000

Total 8480 8480

Mass Balance of Reactive Blue 198 (HEGN)

Base Slurry

Cyanuration

Condensation

Spray Drying

R/O


2. Reactive Blue FNG

Manufacturing Process: Blue 198 base W/C condense with Cynuration of aniline 2:5 DSA & then cond. With M.B.V.S ester then clarify & std. & spray dryer. Mass Balance:

INPUT KG OUTPUT KG

Blue Base 198 W/C 1270Soda Ash 55Water 3500

Aniline 2: 5 DSA 280Soda Ash 270Cynuric Chloride 208S.B.C. 150Celsolin Oil 10Ice 1750Water 1000

Soda Ash 275

MBVS Ester 300Sodium Bicarbonate 80Water 550



Total 9698 9698

Spray Drying

Mass Balance of Reactive Blue FNG

Base Slurry

Cyanuration

2nd Condensation

R/O

1st Condensation

M B V S Solution


3. Reactive Blue 19

Manufacturing Process: Esterification of Oxy-sulphonedry powder in presence of Oleum (23%) & sulphuric Acid (98%) at 35 ͦC for 36 hrs. When reaction is over dump ester/mass in brian solution at 0 ͦC to 2 ͦC slowly. After dumping over check PPT & then filter in F.P. check spot of filtrate. After filtration give air to tight press cake. Dump press cake in reaction with water of 10 ͦC. Then take pH 4.0 to 4.5 by CaCO3. Then filter slurry. Collect filtrate in another vessel. Charge oxilic acid &take pH 4.0 to 4.5 by soda bi carbonate. Then clarify slurry and collect filtration in R/O & then spray dryer. Mass Balance:

INPUT KG OUTPUT KG

Oxy Sulphone 775Oleum (23%) 800 SO2 Gas 350Sulfuric Acid (98%) 190

Water 3550 Effluent to ETP 3200Salt 870

Water 3250 Gypsum Sludge 550CaCO3 160

Oxilic Acid 90Soda Bicarbonate 100Water 650


Drying loss 3200Reactive Blue 19 1000

Total 10435 10435

Mass Balance of Reactive Blue 19

Spray Dryer

Esterfication

Drawning & Filteration

1st Slurry

2nd Slurry

R/O


4. Reactive Blue 49

Manufacturing Process: Dump B-49 base press W/c in vessel with cold water 15 ͦC & take pH 7.0 to 7.2. Check clear solution. Check real base by N. V. Then cool to 0 ͦC to 2 ͦC by external chilling. Charge Cy. Chloride close main hole and stir for ½ hrs. Take pH 7.0 to 7.2 by soda solution and maintain for 4 hrs. Check N. V. of solution. It is 0.2%. If okay then charge metanilic acid clear solution as fast as possible. Maintain pH 7.0 to 7.2 by soda solution. If pH stable start slowly heat up to 35 ͦC to 40 ͦC. check sample and clarify. Chemical Reaction:

Blue 49

O

O

NH2

SO3H

HN NH2

SO3H

CH3

CH3CH3

+Cl

Cl

ClN

NN

O

O

NH2

SO3H

HN NH

SO3H

CH3

CH3CH3

Cl

Cl

N

NN

0 °C - 2 °C

O

O

NH2

SO3H

HN NH

SO3H

CH3

CH3CH3

Cl

Cl

N

NN

+

SO3H

NH2

+

NH2

SO3H

0 °C - 5 °C

O

O

NH2

SO3H

HN NH

SO3H

CH3

CH3CH3

Cl

N

NN

NH

(50%) (50%)

SO3H


Mass Balance:

INPUT KG OUTPUT KG

Blue 49 W/C 550Soda Ash 200Cy. Chloride 100Metanilic Acid 100Water 2000

Water 200 Solid Waste 10


Total 3150 3150


Condensation

Clarifier

Spray Drying


5. Reactive Blue 220 Manufacturing Process: 4 sulphohydrazine is coupled with sulpho OAVS ester Diazo and product is complexed with copper sulphate and spray dryer. Mass Balance:

INPUT KG OUTPUT KG

Sulpho OAVS 270Sodium Nitrite 70HCl (30%) 550Water 1400Ice 1900

4-Sulpho Hydrazone 390Caustic Lye (48%) 90Soda Ash 100Ice 1250Water 1050

Copper sulphate 150Steam 350



TOTAL 7570 7570

Mass balance of Reactive Blue 220

R/O

Spray Drying

Diazotization of Supho OAVS

4 - Sulpho Hydrazone Solution

Coupling


6. Reactive Blue 221 Manufacturing Process: 4 SulphoHydrazone is coupled with 6-Acetyl OAPSAdiazo and product is complexed with copper sulphate. Then mass is filtered and w/cake is hydrolysis & base is condensed with N-ethyl meta base ester and spray dryer. Chemical Reaction:


Mass Balance:

INPUT KG OUTPUT KG

6-Acetyl OAPSA 230CS Lye (48%) 40HCl (30%) 580Sodium nitrite 70Sulphamic acid 2Sodium acetate 100Soda Ash 50Water 750Ice 850

4-Sulpho Hydrazone 300HCl (30%) 650Soda ash 100Ice 800Water 700

Copper sulphate 250CS Flakes 320Hot water 580

Salt 650 Effluent 3400Soda ash 50

Cyanuric Chloride 150Tamol 7Water 2000

N-Ethyl MBVS 255Soda Bi Carb 155

Dicamol 45 Solid waste 100



Total 9684 9684

Mass Balance of REACTIVE BLUE 221

Condensation

Clarifier

Spray Drying

Diazotization of 6-Acetyl OAPSA

4-Sulpho Hydrazone Solution

Coupling

Isolation & Filteration

Base Cyanuration

R/O


7. Reactive Blue 222 Manufacturing Process: MPDSA is cynurated with cynuric chloride at 5 ͦC& further condensed with M.B.V.S. Ester. Then this product diazotized & coupled with H-acid to getcoupling mass-1. S.T.acid is diazotized & further coupled with coupling mass-1 to get coupling mass-2 which spraydried. Chemical Reaction:


Mass Balance:

INPUT KG OUTPUT KG

MPDSA 135Cyanuric Chloride 132Soda ash 60Celsolin Oil 3Water 750Ice 750

M.B.V.S. 200NaHCO3 60Water 400

NaHCO3 70

NaNO2 50HCl (30%) 300Ice 750

H-Acid 210Soda Ash 70Ice 210Water 380

Sodium Acetate 145

S. T. A. 200HCl (30%) 60NaNO2 50Ice 380Water 380

Sodium Acetate 150



Total 5895 5895


H-Acid Cle. Solution

Coupling 2

Spray Drying

Cyanuration of MPDSA

M. B. V. S. Cle. Solution

Condensation 1

Diazotization of Cond. Mass

Coupling 1

S.T.A. Diazotization

R/O


(B) Dyes Intermediates

8. PNCBOSA Manufacturing Process: PNCB is sulphonated in presence of Oleum (65%) at 120 ͦc to 125 ͦC. Maintain for 8 hrs. then dump s/mass in water & salting & filter &C.F. Mass Balance:

INPUT KG OUTPUT KG

PNCB 715 SO2 Gas 8065% Oleum 785

Ice 1200 Spent Acid (30 - 35%) 2500Water 2800

Salt 1000 Effluent 3795

Water 1400

1525

Total 7900 7900

Wet Cake of PNCBOSA

Mass balance of PNCBOSA

Sulphonation

Dumping

PNCBOSA (As is real basis 1000 Kg)

Isolation


9. Chloranil Condense Manufacturing process:

PNCBOSA is condensed with E.D.A. at 116ͦC& the mass is then isolate with HCl. Product obtain is then reduction with C.I.P. when reaction is over filter red. Mass & collect liq. This liq. Clarify & further condense with chloranil at 60ͦC. When reaction over filter the mass & dry & Pulv. final product obtained. Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

E.D.A. 5000PNCBOSA 1000 E.D.A. Recovered 4400SBC 250Water 1800

HCl (30%) 1500 Effluent 6990Water 2500

Ac. Acid 100C.I.P. 500 Iron Sludge 1250Soda Ash 500Water 3500

Chloranil 400 Effluent 4500SBC 290Water 2000

Drying Loss 1200Chloranil Condensate 1000

Total 19340 19340

Mass balance of Chloranil Condense

E.D.A. Condensation

Reduction

Drying

Isolation

Chlo. Cond.


10. Blue HEGN (198) Base Manufacturing process: Chlo. Cond is cyclisation in presence of Oleum (23%), Sulphuric acid (98%) & sodium per sulphate at 18 ͦC, when reaction over dump this mass in cold water (20'c)as fast aspossible. Then temp. goes up to 50ͦC. When dumping over stir for 15minutes & start filter. Then wash with tap water up to congo paper faint. Then dump press cake invessel & take pH 5.0 to5.5by soda ash & then spray dry and final product obtain. Chemical Reaction:

(I) Cyclisation:-

O

O

O

NH

NH

NH2CH2CH2NH

OSO3Na

SO3NaNHCH2CH2NH2

( Chlo. Cond )

+

NH2CH2CH2NH

SO3H

NH

NH2

O

O

CL

CL

O

O

NH

NH2

SO3H

NHCH2CH2NH2

[ Blue HEGN (198) Base ]


Mass Balance:

INPUT KG OUTPUT KG

Sulfuric Acid (98%) 375Oleum (23%) 2800 SO2 Gas 90Chlo. Cond. 1000Sodium per Sulfate 750

Ice 2500 Effluent 11305Water 3000

Water 3000Soda Ash 150


Total 13575 13575

Mass Balance of Blue HEGN (198) Base

Cyaclization

Drawning

Slurry Preparation

Drying


11. Aniline 2,4 DSA Manufacturing process: Sulphalinic Acid is sulphonated with Oleum (23%) at different temp. & then this mass is dump in water. Aniline 2:4 DSA is isolated & cool. Filter slurry in Nutch & wash & C.F. Chemical Reaction:

NH2

SO3H

+ H2S2O7

NH2

SO3H

SO3H

+ H2O SO3+

Sulphanilic Acid

Oleum

Aniline 2, 4-Disulphonic Acid

Water Sulphur Trioxide

Mass Balance:

Input KG Output KG

Sulphanilic Acid 850Oleum 23% 2500 SO2 Gas 50

Water 3000

Spent sulfuric acid(45-50%) 4200Water 1000 Effluent 1450

1650

Total 7350 7350

Mass balance of Aniline 2, 4 DSA

Sulphonation

Drawning

Filtration & Washing

Wet Cake of Aniline 2:4 DSA

Aniline 2:4 DSA (As is real basis 1000 Kg)


12. Aniline 2,5 DSA Manufacturing process: Metalinic acid is sulphonated with sulphuric acid &Oleum(65%). Then mass is dump in water give tri sulphonic acid is hydrolised to get aniline 2:5 DSA. It is isolatedwith salt & filter & wash &C.F. Chemical Reaction:

++

H2SO 4

H2S2O7+ H2O + SO 3

+H2O + H2SO 4

Metanilic Acid Aniline 2, 4, 5-Trisulphonic Acid

Water Sulphur Trioxide

Aniline 2, 4, 5-Trisulphonic Acid

Aniline 2, 5-Disulphonic Acid

Sulphuric Acid

NH 2

HO 3S

SO 3H

SO 3H

NH 2

HO 3S

SO 3H

SO 3H

NH 2

HO 3S

SO 3H

NH 2

HO 3S

Mass Balance:

Input KG Output KG

Metanilic Acid 850Sulfuric Acid (98%) 1000 SO2 Gas 80Oleum 65% 1200

Hyflow 10Activated Carbon 45 Spent Acid 5185Steam 850Water 3100

Water 1600 Solid waste 250

Sodium Sulphate 850Steam 700

Effluent 3070

1620

Total 10205 10205

Wet Cake of Aniline 2:5 DSA

Mass balance of Aniline 2, 5 DSA

Sulphonation

Hydrolysis

Clarification

Isolation

Filtration & Centrifuge

Aniline 2:5 DSA (As is real basis 1000 Kg)


13. Oxy Sulphone Manufacturing process: Bromamine acid is condense with meta base cond. & cuprous chloride & S.B.C. at 72 ͦC for 10 hrs. When reaction over transfer cond. / mass in MS + RL+BL vessel. Then charge HCl to get pH 1.5 to 1.0. Then heat 90 C for boil up. Then cool to 70 C and filter slurry in F. P. when filter over. Give wash of 5% salt solution gradually. Then give air and dump F. P. Take water and charge press cake & spray dryer. Final Powder obtain. Chemical Reaction:

(I) Bromamine Condensation:-

O

O

SO3H

NH2

Br

( Bromamine Acid )

+

NH2

SO2CH2CH2OH

( M. Base Condense )

+ NaHCo3

CuCl2

O

O

SO3HNH2

NH

SO2CH2CH2OH

( Oxy. Sulphone )


Mass Balance:

Input KG Output KG

Bromamine Acid 850M.B. V.S. Acid 550Soda Bi carbonate 850CUCl2 10Celsolin Oil 10Copper Bronze 5Water 1000

HCl (30%) 2000Salt 250 Effluent 7275Water 2000

Water 2000

Drying Loss 1250Oxy Sulphone 1000

Total 9525 9525

Drying

Mass balance of Oxy Sulphone

Bromamine Condensation

Isolation

Slurry


14. M. Acid Manufacturing process:

Macitinline acid is nitrated by nitric acid & H2SO4. Then isolate N. Mass in chilled water. Filter &C.F. Nitro w/cake. Then this nitro w/cake reduction in presence of C.I.powder & acetic acid at 80 ͦC. Then filter reduction Mass & collect amino solution. Check N.V.& set N.V. 7.0 to7.5%. Isolate by HCl (30%) at 3.0 to3.5pH. Check f/l. Then heat 75 ͦC& check f/l 0.2% to0.3%. Chemical Reaction: (I) Sulphonation:-

CH3

CH3H3C

( Mesitylene Acid )

+H2S2O7

H2SO4

CH3

CH3H3C

SO3H

+ H2SO4

(II) Nitration:-

CH3

CH3H3C

SO3H

+2(HNO3)H2SO4

CH3

CH3H3C

SO3H

NO2

O2N+ 2(H2O) + H2SO4

(III) Reduction:-

CH3

CH3H3C

SO3H

NO2

O2N

+Fe/HCl/H2ONa2CO3

CH3

CH3H3C

SO3HH2N

2,4,6 Trimethyl m Phenylene diamine

[M-Acid]

NH2


Mass Balance:

Input KG Output KG

Macitinline Acid 570H2SO4 2800 NO2 200W.N.A. 880

Water 1500Ice 2200

Spent Acid 4500

NaOH 150Water 1500

Iron Powder 1500 Iron Sludge 2900Ac. Acid 350Soda Ash 350Ac. Carbon 25Water 650

HCl 1500 Effluent 4540Hydro Powder 15

Drying Loss 850M Acid 1000

Total 13990 13990

Drying

Mass balance of M. Acid

Nitration

Isolation

Filteration & C. F.

Nitro slurry

Reduction

Isolation

Filteration & C. F.


15. Blue 49 Base Manufacturing process: Bromammine acid is condense with M. Acid at 8.5 to 9.0pH in presence of copper oxide & nitrogen gas purging. At 72ͦC slowly by slowly external heating. The reaction take 12 to 15hrs.check unreacted bromamine content. If nil then charge common salt & Dicamol & stop stirrer. Filter mass & wash press cake by hot water. Collect filtrate in another vessel. Charge HCl (30%) to get pH 4.0 to 4.2 to isolate M-acid. Start filter in F.P. &collect filtrate in another vessel. (Press cake is recover m-acid use for next batch). Check volume & take pH 1.0 by HCl(30%) charging. Check spot & startfilter. Give wash of 30% HClsolution gradually.Give slow air & dump F.P. Cake in vessel with water. Take pH 4.5 by soda ash & spray dryer. Chemical Reaction: (I) Bromamine Condensation:-

O

O

SO3H

NH2

Br

( Bromamine Condensation )

+NH2H2N

CH3

CH3H3C

SO3H

+ CuO + N2 gas + Na2Co3

O NH2

O

SO3Na

NH

CH3

NH2

CH3

SO3Na

H3C

( Blue 49 Base )

( M- Acid )


Mass Balance:

INPUT KG OUTPUT KG

Bromamine Acid 1000M-Acid 1625Soda Ash 500Cuprous Oxide 100Celsolin Oil 15Coomon Salt 380Dicamol 40N2 Gas 65Water 3200

Wash Water 1500 Solid Waste 950

HCl (30%) 1500 Recovered M-Acid 1150Wash Water 2500

HCl (30%) 1200 Waste Water 11850Wash Water 2200

Water 1800Soda Ash 180

Drying loss 2855Blue 49 Base 1000

Total 17805 17805

Mass Balance of Blue 49 Base

2nd Isolation

Slurry

Spray Drying

Condensation of Bromamine Acid

Filteration

1st Isolation


16. Metanilic Acid Manufacturing process: Nitro Benzene reacted with Oleum (65%) at 105 ͦCfor 4 hrs. Maintain Check TLC & acidity. Then dump S/mass water + lime powder + Soda ash solution slowly at 60 C to 80 C. Take pH 7.0 by lime powder & stir for 1 hrs. Filter slurry in nutch & wash with hot water. Collect nitro solution. Check N V and real. Then reduction of nitro solution in presence of iron powder & HCl. Heat mass up to 95 C and check clear spot and A. R. + B. R. by N. V. ok. Then charge soda ash to get pH 8.5 to 9.0 to –Ve test. Filter mass in F. P. and wash with hot water and receive amino solution & check N. V. & real charge sulphuric acid slowly to get pH 1.5 Material isolate. Check F/L & filter slurry in nutch. Then C. F. & Dry in SFD

Chemical Reaction: (I) Sulphonation:-

NO2

+H2S2O7

H2SO4

NO2

SO3H

+ Na2CO3

NO2

SO3Na

(II) Reduction:-

NO2

SO3Na

+ 2Fe + HCl Fe2O3+ + NaCl + CO2 + H2O

( Aniline 2 Sulphonic Acid ) Metalinic Acid

NH2

SO3Na


Mass Balance:

INPUT KG OUTPUT KG

Nitro benzene 900 SO2 Gas 40Oleum (65%) 980

Soda Ash 50Lime Stone Powder 1100 CO2 Gas Evap. 150Water 500

Hot Water 500 Gypsum Sludge 3120

Iron Powder 125HCl (30%) 100 CO2 Gas Evap. 50Soda Ash 175Water 750

Hot water 700 Iron Sludge 450

Sulphuric Acid 90 CO2 Gas evap. 25Water 2400

Wastewater to ETP 2385

Drying loss 1150Metanilic Acid 1000

Total 8370 8370

Isolation

Drying

Mass Balance of Metanilic Acid

Sulphonation

Drawning

Filteration

Reduction

Filteration

Filteration & Centrifugation


17. 4 SulphoAnthranilic Acid Manufacturing process: O.N.T. is sulphonated with sulphuric acid (98%) and leum (65%) at 65 C maintain for 12 hrs. Then S/mass is dilute in water and hydrolyze by NaOH and water. Then clarify it, isolate material by 70% sulfuric acid then filter & C.F.

Chemical Reaction:

CH3

NO2

+ H2SO4 + H2SO4.SO3

Ortho Nitro Toluene

Hydrolysis

COOH

NH2

SO3H

CH3

NO2

SO3H

4-Sulpho Anthranilic Acid

Sulphonation-2SO3

-2H2OOleumSulphuric Acid

Mass Balance:

Input KG Output KG

O.N.T. 1800Oleum (65%) 1980Sulfuric Acid 1000

Water 2700 Dil Sul. Acid (40-45%) 4850

Water 3500NaOH 2150

Sulfuric Acid (70%) 2500

Wash Water 1800 Spent Acid (32-35%) 10430

Drying Loss 11504 Sulpho Anthranilic Acid 1000

Total 17430 17430

Drying

Filteration & Centrifugation

Mass balance of 4 Sulpho Anthranilic Acid

Sulphonation

Dumping

Hydrolysis

Isolation


18. 4 SulphoHydrazone Manufacturing process: 4 Sulpho Anthranilic Acid is diazotize by sodium nitrite and HCl. Then it is coupled by S. B. S. in presence of C. S. Lye (48%). Then mass is reacting with benzaldehyde & HCl to get product. Chemical Reaction:

(I) Diazotisation:-

COOH

NH2

SO3H

( 4- Sulpho Anthralanic Acid )

+ NaNo2 + 2(HCl)

SO3H

COOH

N=NCL

(II) Reduction:-

SO3H

COOH

N=N-CL + SBS + NaOH

SO3H

COOH

NHNH2

(III) Condensation:-

SO3H

COOH

NHNH2

+

CHO

(Benzaldehyde)SO3H

COOH

N=N-CH

( 4- Sulpho Hydrozone )


Mass Balance:

Input KG Output KG

4 Sulpho Anthranilic Acid 1000HCl (30%) 1200Sodium Nitrite 300Ice 1700

Sodium bisulphite 850Caustic Soda 480

Benzaldehyde 600 SO2 Gas 300HCl (30%) 1000 CO2 Gas 250Ice 1900

Wash Water 480 Effluent 6830

Drying Loss 11304 Sulpho Hydrozene 1000

Total 9510 9510

Drying & Packing

Mass balance of 4 Sulpho hydrazene

Diazotization

Coupling

Benzolation



19. Sulpho OAVS / Sulpho VS / Sulpho J Acid / Sulpho gamma Acid Manufacturing process: OAVS is sulphonated with Sulphuric acid (98%), oleum (65%) at 140 ͦC then dump s. mass in cold water below 10 ͦC to 15 ͦC. Then salting by KCl & check F/L& filter & C.F. Chemical Reaction: Sulpho OAVS

(I) Sulphonation:-NH2

OCH3

SO2CH2CH2OSO3H

( OAVS )

+ H2S2O7

H2SO4

NH2

OCH3

SO2CH2CH2OSO3HHO3S

( Sulpho OAVS )

Sulpho VS

(I) Sulphonation:-

SO2CH2CH2OSO3H

NH2

+H2S2O7

H2SO4

SO2CH2CH2OSO3H

NH2

SO3H

( Sulpho V.S )

Sulpho J Acid

(I) Sulphonation:-

OH

H2N SO3H

( J. Acid )

+H2S2O7

H2SO4

OH

H2N SO3H

SO3H

( Sulpho J- Acid )


Sulpho gamma Acid

(I) Sulphonation:-

NO3S

OH

NH2

( Gamma Acid )

+H2S2O7

H2SO4

OH

NH2

SO3H

( Sulpho Gamma Acid )

HO3S

Mass Balance:

INPUT KG OUTPUT KG

OAVS 1250 SO2 282Oleum Acid (65%) 2212Sulphuric Acid 1812

KCl 650Water 1500Ice 2500

Wash water 1500 Spent acid (32-35%) 9642

1500

Total 11424 11424

Mass Balance of Sulfo OAVS

Sulphonation

Dumping


Wet cake of Sulpho OAVS

Sulpho OAVS (As is real basis1000 Kg)


20. 3:5 DABA Manufacturing process: Benzoic acid is nitrated in presence of Nitric acid & Sulphuric acid. When reaction over transfer n/mass in water & isolated. Filter & C.F. Then reduction of nitro compound in presence of iron powder &HCl (30%). Then maintain temp up to reduction over. When reduction overcharge soda ash to -ve iron test. Then filter mass in F.P. & wash with water. Collect amino in isolation vessel. Isolate by HCl (30%) &filter & get final product. Chemical Reaction:

COOH

+

(I) Nitration:-

HNO3

H2SO4

COOH

NO2

(II) Reduction:-

NO2

COOH

+Fe/HCl/H2O

Na2CO3H2N NH2

COOH

( 3:5 DABA )

O2N

O2N


Mass Balance:

INPUT KG OUTPUT KG

Benzoic Acid 1200Nitric Acid 1090 NO2 Gas 180Sulphuric Acid(98%) 2336

Water 2500

Wash Water 1000 Spent Acid(35-40%) 3744Effluent 1500

Iron Powder 1636HCl (30%) 1000 Iron Sludge 4000Soda Ash 900Water 1800

HCl (30%) 950 Waste water to ETP 2952

Drying loss 10363,5 DABA 1000

Total 14412 14412


Drying

Mass Balance of 3,5 DABA

Nitration

Drawning


Reduction

Isolation


Annexure-III Water Balance Diagram

Total Volume 233

Dyes 89

RO 83

Spray drying

for product recovery

Dyes Intermediates

144

77

Domestic 5.0

Soak pit 4.0

Drying Loss 12.0

Ice 30

4.0 Steam

Water retained with RM 71

Process 128

Permeates water 44

6.0

Scrubber 10.0

7.0 SBS (30-35%)

3.0

Boiler 10.0

Cooling 40

Utility 50.0

Spray Dryer 56.0

Salt 1.75

Evaporation loss 54.25

10 Bleed

off

Permeates water 85.0*

50

Drying Loss 39

RO 141

Total fresh water consumption 233.0 KLD (123 KLD Fresh water + 110 KLD recycle)

Greenbelt 15.0

Washing 25.0*

1.0 Blow down

Water/steam loss

25

25

25

ETP 77+ 3.0 + 25.0 +25.0 + 1.0+ 10 =141

Spent H2SO4

55


Break up of Water Consumption& Waste Water Generation

Sr. No.

Source Water Consumption

(KLD)

Waste Water generation

(KLD) 1. Domestic 5.0 4.0

2. Green Belt 15 --

3. Industrial

A Process 128 102

B Scrubber 10 3.0

C Boiler 10 1.0

D Cooling 40 10

E Washing 25 25

Total Industrial 213 141

Total (1 +2 + 3) 233 145

Less recycle 110 --

Actual fresh water consumption

123 --


Annexure-IV

Hazardous waste details

Sr. No.

Type of Waste

Category No. as per

HWM rules, 2016

Quantity Proposed

Method of Disposal

1. ETP Waste 35.3 200 MT/month Collection, Storage, Transportation, Disposal at TSDF site.

2. Salt ofSpray Dryer

35.3 46 MT/month Collection, Storage,Transportation, disposal at TSDF site.

3. Process Iron Sludge

26.1 145 MT/month Collection, Storage, Transportation, disposal at TSDF site or to Cement industries for co-processing.

4. Process Gypsum Waste

26.1 84 MT/month Collection, Storage, Transportation, disposal at TSDF site or to Cement industries for co-processing.

5. Sodium Bi sulfite (30-35%)

26.3 182 KL/Month

Collection, Storage and partly reuse in-house and partly will be sold to actual users under Rule-9.

6. UsedOil 5.1 0.5 KL/Year Collection, Storage,Transportation,sell to registered re-processors or use for lubrication within premises.

7. Discarded Containers/ Liners/Bag

33.3

600 Nos./month

1.0 MT/month

Collection, Storage,Transportation, Sell to registered recyclers.

8. Spent Acid B-15 1430 MT/month

Collection, Storage,Transportation and will be sold to actual users under Rule-9.


Annexure-V Details of Air Pollution

Sr. No.

Stack attached to

Fuel Type Stack Height,

in m

APC measures

Probable emission

Flue Gas Stacks 1. Steam Boiler

(2 TPH) – 2 nos. (1 stand by)

Coal/ Bio fuel 10 TPD

30 Multi Cyclone

Dust Collector

SPM<150 mg/Nm3 SO2<100 ppm NOx<50 ppm

2. Ho Air Generator – 4 Nos. (4.5 Lakhs Kcal/hr each)

Coal/ Bio fuel 2 TPD each

30 Bag Filter SPM<150 mg/Nm3 SO2<100 ppm NOx<50 ppm

3. Ho Air Generator – 2 Nos. (25 Lakhs Kcal/hr each)

Coal/ Bio fuel 14 TPD each

30 IN built Cyclone

Separator & Bag Filter

SPM<150 mg/Nm3 SO2<100 ppm NOx<50 ppm

4. D G Set (500 kVA)

HSD – 70 lit/hr. 15 -- SPM<150 mg/Nm3 SO2<100 ppm NOx<50 ppm

Process Gas Stacks 1. Process Vessel

(Sulphonation) -- 20 Two Stage

Water Scrubber &

Alkali Scrubber

SO2<40 mg/Nm3

2. Process Vessel (Nitration)

-- 20 Two Stage Alkali

Scrubber

NOx<25 mg/Nm3

3. Process Vessel (Isolation)

-- 20 Two Stage Alkali

Scrubber

SO2<40 mg/Nm3

4. Spin Flash Dryer – 4 Nos.

-- 20 In builtcyclone separator& bag filter

PM<45 mg/Nm3

5. Spray Dryer For effluent (2500 lit/hr.)

-- 30 In built cyclone

separator & bag filter

PM<45 mg/Nm3

annexure-i list of products filem/s. metachem industries, khambhat 1 annexure-i list of products sr....

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