Annexure-I List of Products

Transcription

1 Sr. No. Annexure-I List of Products Name of Products CAS no. Quantity (MT/Month) Existing Proposed Addition 1 Reactive Black Reactive Black HFGR Reactive Red Reactive Yellow FG Reactive Blue Reactive Blue Direct Black Direct Black Total 9 Reactive Blue Reactive Blue Reactive Blue Reactive Blue Reactive Blue Reactive Turquoise Blue Total Associated Dyestuff Pvt. Ltd., Unit-I 1

2 Sr. No. List of Raw Materials Name of product Name of raw material Quantity (MT/MT) 1 Reactive Black 5 Vinyl Sulphone Sodium Nitrite HCl Sulphamic Acid H-Acid Sodium bi Carbonate Vinyl Sulphone Reactive Black HFGR Vinyl Spulphone HCl Sodium Nitrite CS Lye H-Acid Soda bi Carb J-Acid Cyanuric Chloride Reactive Red 195 Cyanuric Chloride H-Acid 0.22 HCl CS Lye Soda Ash Soda bi Carb Sodium Nitrite 0.05 STA Sulphamic Acid Vinyl Sulphone Reactive Yellow FG Vinyl Sulphone CS Lye HCl Salt Soda bi Carb Sodium Nitrite SPCP Sulphamic Acid Reactive Blue 222 Cyanuric Chloride H-Acid HCl MPDSA Soda Ash Soda bi Carb Sodium Nitrite STA Sulphamic Acid Reactive Blue 194 VS Caustic Lye Cynuric Chloride Associated Dyestuff Pvt. Ltd., Unit-I 2

3 H-Acid HCl MPDSA Soda Ash Sodium Nitrite Direct Black 22 F.C. Acid HCl 1.2 Sodium Nitrite Sulphamic acid Gamma Acid Soda Ash Caustic Flakes MPD Soda Ash Acid Black 210 PNA Caustic Flakes DASA H-Acid HCl MPD Soda Ash Sodium Nitrite Reactive Blue 160 MPDSA HCl 0.17 Sodium Nitrite Cynuric Chloride Caustic Lye Soda Ash H-Acid Metanilic Acid Reactive Blue 198 Cyanuric Chloride Soda Ash Aniline 2:4 DSA Soda bi Carb Blue HEGN-Base HCl Reactive Blue 220 Sulpho OAVS Sulpho Hydrazone Copper Sulphate CS Lye HCl Soda Ash Soda bi Carb Sodium Nitrite Sulphamic Acid Reactive Blue 19 Meta Based Easter Sodium Nitrite HCl Associated Dyestuff Pvt. Ltd., Unit-I 3

4 Sulphamic Acid Bromamine Acid CS Flakes Salt Reactive Blue Acetyl OAPSA Sulpho Hydrazone Copper Sulphate CS Flakes CS Lye Cyanuric Chloride HCl N-Ethyl MBE Salt Soda Ash Soda bi Carb Sodium Acetate Sodium Nitrite Reactive Terq. Blue 21 Copper Pthalo Cyanine Blue Chloro Sulphonic Acid PCl Vinyl Sulphone Sodium Bi Sulphate Associated Dyestuff Pvt. Ltd., Unit-I 4

5 Annexure-II Manufacturing Process 1. Reactive Black 5 Manufacturing Process: Diazotization: VS (Para Base) charged to a reaction vessel along with water and ice to maintain temperature between 0 to 5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature 0 to 5 C throughout the diazotization reaction. Coupling: Charge H Acid to the diazotized VS and stir it keeping the temperature between 0 to 5 C by adding of ice. Clarification: The coupled mass is diluted with water and clarified in clarifier. Spray Drying: The standardized dye liquid will be transferred to the spray drying holding tank and spray dry. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauber s salt and anti dusted by anti-dusting oil. Packing: The final product is then packed in HDPE bags/m.s. Drums/ Plastic Carboys/Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 5

6 Chemical Reaction: 1. Diazotization of VS: NH 2 N=N-Cl + 2HCl + NaNO 2 Ice Temp C + 2H 2 O + 2NaCl SO 2 CH 2 CH 2 OSO 3 H SO 2 CH 2 CH 2 OSO 3 H Vinyl sulphone 2. Solution of H-acid NH 2 OH NH 2 OH SO 3 H + 2NaOH SO 3 H Ice Temp C SO 3 Na + 2H 2 O SO 3 Na H-acid Clear sodium salt solution of H-acid 3. Coupling N=N-Cl NH 2 OH + SO 2 CH 2 CH 2 OSO 3 H Diazotized vinyl sulphone SO 3 Na SO 3 Na Clear sodium salt solution of H-acid + 2NaHCO 3 Ice Temp C NH 2 OH NaO 3 SOH 2 CH 2 CO 2 S N=N N=N SO 2 CH 2 CH 2 OSO 3 Na SO 3 H SO 3 H + 2H 2 O + 2CO 2 + NaCl Reactive Black 5 Associated Dyestuff Pvt. Ltd., Unit-I 6

7 Mass Balance: Mass Balance of Reactive Black 5 INPUT KG OUTPUT KG VINYL SULPHONE 470 SODIUM NITRITE 125 HCL 220 SULPHAMIC ACID 1 WATER 800 ICE 750 Diazotization of Vinyl Sulphone H-ACID 260 SODIUM BI CARBONATE 276 ICE 650 WATER 500 Coupling of H-Acid SD-40 8 Drying loss 3060 Spray Drying Standardization & Packing Reactive Black Total Associated Dyestuff Pvt. Ltd., Unit-I 7

8 2. Reactive Black HFGR Manufacturing Process: Diazotization of Amine: Charge vinyl sulfone to a M.S.R.L reaction vessel along with water and ice to maintain temperature between 0 to 5 o C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature between 0 to 5 0 C throughout the diazotization reaction. First Coupling: Charge H-Acid slurry to the diazotized vinyl sulfone, and stir for 6 to 8 hrs keeping the temperature between 0 to 5 0 C by adding of ice. Second Coupling: Charge J. Acid Clear solution. Add Cyanuric Chloride in it keeping the temperature between 8 to 10 0 C. Check the cyanuration test. Then charge cyanurated J. Acid solution in to first coupling mass. Solution stir for 2 hrs keeping temperature between 0 to 5 0 C raise the PH of the first coupling mass be 50 kg. Sodium bicarbonate up to 6.0 Maintain temperature between 0 to 5 o C by addition of ice. Check strength, tone etc. before starting spray drying and standardize the batch before spray drying. Spray Drying: The standardized dye liquid of reactive black HFGR will be transferred to the spray drying holding tank and spray dry. Packing: The final product is then packed in HDPE bags/m.s. Drums/ Plastic Carboys/Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 8

9 Chemical Reaction 1. Diazotization of VS: NH 2 N=N-Cl + 2HCl + NaNO 2 Ice Temp C + 2H 2 O + 2NaCl SO 2 CH 2 CH 2 OSO 3 H SO 2 CH 2 CH 2 OSO 3 H Vinyl sulphone Diazotized vinyl sulphone 2. Solution of H-acid NH 2 OH NH 2 OH SO 3 H + 2NaOH SO 3 H Ice Temp C SO 3 Na + 2H 2 O SO 3 Na H-acid Clear sodium salt solution of H-acid 3. Coupling N=N-Cl NH 2 OH + SO 2 CH 2 CH 2 OSO 3 H Diazotized vinyl sulphone SO 3 Na SO 3 Na Clear sodium salt solution of H-acid + 2NaHCO 3 Ice Temp C NH 2 OH HO 3 SOH 2 CH 2 CO 2 S N=N N=N SO 2 CH 2 CH 2 OSO 3 H SO 3 Na SO 3 Na + 2H 2 O + 2CO 2 + NaCl Associated Dyestuff Pvt. Ltd., Unit-I 9

10 4. Solution of J-Acid SO 3 H NH 2 SO 3 Na NH 2 + NaOH + H 2 O OH J-Acid OH Clear Sodium Salt Solution of J-acid 5. Cyannuration of J-Acid SO 3 H OH NH 2 + Cl N C Cl C N N C Cl SO 3 Na OH NH C N N Cl C N C Cl + HCl Clear Sodium Salt Solution of J-acid Cyannuric chloride Cyannurated mass 7. Coupling N=N-Cl + SO 3 Na NH C N N Cl C N C + NaHCO 3 SO 2 CH 2 CH 2 OSO 3 H Diazotized vinyl sulphone OH Cyannurated mass Ice Cl Temp C HO 3 SOH 2 CH 2 CO 2 S SO 3 Na HO 3 SOH 2 CH 2 CO 2 S N=N Cl SO 3 Na N C NH C N N C N=N Cl OH Orange Dye Cl N C NH C N N C Cl OH Orange Dye NH 2 OH + + H 2 O + NaCl HO 3 SOH 2 CH 2 CO 2 S N=N N=N SO 2 CH 2 CH 2 OSO 3 H SO 3 Na SO 3 Na Reactive Black HFGR Associated Dyestuff Pvt. Ltd., Unit-I 10

11 Mass Balance: Mass Balance Reactive Black HFGR INPUT KG OUTPUT KG VINYL SPULPHONE 400 HCl 180 SODIUM NITRITE 100 SULPHAMIC ACID 2 WATER 1600 ICE 650 Diazotization CS LYE 60 H-ACID 140 WATER 1500 ICE 550 First Coupling SODA BI CARB 140 J-ACID 80 CYANURIC CHLORIDDE 60 WATER 1500 ICE 550 Second Coupling RO/UF w/w reuse 3000 Spray Drying Drying loss 3512 Standardization & Packing Reactive Black HFGR 1000 TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 11

12 3. Reactive Red 195 Manufacturing Process: Cyanuration: Charge cyanuric chloride in to H Acid and caustic lye solution for the cyanuration. Diazotization: Sulpho Tobias Acid charged to a MSRL reaction vessel along with water and ice to maintain temperature 0 to 5ºC. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature 0 to 5 C throughout the diazotization reaction. Coupling: Charge cyanurated H-acid to the diazotized Sulpho Tobias acid and stir it keeping the temperature 0 to 5ºC by adding of ice. Condensation: Charge Meta base VS with soda bi carb for the condensation of the coupler mass. Clarification: The final dye is clarified in Filter Press with Dicamol. Spray Drying: The final dye liquid will be transferred to the spray drying holding tank and spray dry. Standardization: The spray dried powder is then charged to the ball mill and standardize be adding Glauber s salt and anti dusted by anti-dusting oil. Packing: The final product is then packed in HDPE bags/ M.S. Drums / Plastic Carboy s/paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 12

13 Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 13

14 Mass Balance: Mass Balance Reactive Red 195 INPUT KG OUTPUT KG CYANURIC CHLORIDE 125 H-ACID 220 HCL 260 SODA BI CARB 115 CS LYE 32 WATER 1000 ICE 630 Cyanuration of H-Acid STA 205 HCL 43 SODIUM NITRITE 25 SULPHAMIC ACID 2 SODA BI CARB 115 SODA ASH 38 OCTANOL 1 Water 1000 ICE 510 Diazotization of STA SODIUM NITRITE 25 HCL 43 SULPHAMIC ACID 2 Water 1200 ICE 175 Coupling of Cyanurated of H-Acid VINYL SULPHONE 180 SODA BI CARB 25 HCL 43 Water 1200 ICE 210 Condensation of Vinyl Sulphone DICAMOL 20 solid waste 47 Clarification RO/UF w/w reuse 2880 Drying loss Spray Drying SD Standardization & Packing Reactive Red Total Associated Dyestuff Pvt. Ltd., Unit-I 14

15 4. Reactive Yellow FG Manufacturing process: Diazotization: Charge VS to a MSRL reaction vessel along with water and ice to maintain temperature between 0 to 5 o C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization is completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature between 0 to 5 o C throughout the diazotization reaction. Coupling: Charge SPCP with Caustic lye to the diazotized mass and stir it keeping the temperature between 0 to 5 o C by adding of ice. Spray Drying: The standardized dye liquid will be transferred to the spray drying holding tank and spray dry. Packing: The final product is then packed in HDPE bags/m.s. Drums/ Plastic Carboys/Paper cartoon boxes. Chemical Reaction: 1. Diazotization NH 2 N=N-Cl + 2HCl + NaNO 2 Ice Temp C + 2H 2 O + 2NaCl SO 2 CH 2 CH 2 OSO 3 H Vinyl sulphone SO 2 CH 2 CH 2 OSO 3 H Diazotized vinyl sulphone 2. Coupling N=N-Cl + SO 3 Na N C ONa N CH C SO 2 CH 2 CH 2 OSO 3 H COONa Diazotized vinyl sulphone SO 2 CH 2 CH 2 OSO 3 H SO 3 Na N C ONa N C N=N C COONa Re. Yellow FG Associated Dyestuff Pvt. Ltd., Unit-I 15

16 Mass Balance: Mass Balance Reactive Yellow FG INPUT KG OUTPUT KG VINYL SPULPHONE 360 HCl 180 SODIUM NITRITE 91 SPCP 360 SULPHAMIC ACID 2 WATER 1200 ICE 1500 Diazotization SODA BI CARB 55 CS LYE 127 SALT 400 WATER 1650 ICE 1250 SPCP 360 Coupling RO/UF w/w reuse 3100 Spray Drying Drying loss 3435 Standardization & Packing Reactive Yellow FG 1000 TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 16

17 5. Reactive Blue 222 Manufacturing Process: Cyanuration and Condensation: Take MPDSA and Cynauric Chloride. Use soda bi carb for the condensation purpose. Take ice in the condensed mass for keeping the temperature at 0 to 5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Keep temperature 0 to 5ºC throughout the diazotization reaction. Charge H Acid to the diazotized mass and stir it keeping the temperature between 0 to 5ºC by adding of ice. After cyanuration and MPDSA complete add Meta Base VS Ester for condensation. Second Diazotization: Sulpho Tobias Acid charged to a MSRL reaction vessel along with water and ice to maintain temperature 0 to 5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature 0 to 5ºC throughout the diazotization reaction. Second Coupling: Charge 1 st coupler mass to the diazotized STA and stir it keeping the temperature 0 to 5 C by adding of ice. Spray Drying: Final product clarified dye solution is spray dried in spray dryer. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauber salt and anti-dusted by antidusting oil. Packing: The final product is then packed in HDPE bags/m.s. Drums / Plastic Carboyes/Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 17

18 Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 18

19 Mass Balance: Mass Balance of Reactive Blue 222 INPUT KG OUTPUT KG CYANURIC CHLORIDE 350 MPDSA 350 SODA ASH 232 TAMOL 11 Water 1450 ICE 800 Cyanuration and Condensation of MPDSA HCl 640 SULPHAMIC ACID 1 H-ACID 275 SODA ASH 44 SODA BI CARB 70 Water 1650 ICE 700 First Diazotization of H-Acid STA 286 HCl 170 SODIUM NITRITE 66 SULPHAMIC ACID 2 SODA BI CARB 76 SODA ASH 93 OCTANOL 5 Water 1550 ICE 750 Second Diazotization of STA Second Coupling Charge Coupler Mass in to Diazotized STA DICAMOL 40 Solid waste 75 Clarification RO/UF w/w reuse 5285 SPRAY DRYING Drying loss 3251 Standardization & Packing Reactive Blue Total Associated Dyestuff Pvt. Ltd., Unit-I 19

20 6. Reactive Blue 194 Manufacturing Process: Charge VS in reaction vessel with water and clear it by SBC get ph 4.5. Cynuration of VS: In VS clear solution transfer in to cynuric chloride emulsion at temp 0 stir ½ hr then ph adjust by SBC 2.5 to 3.2 and maintain up to cynuration ok stir for an hour more. Temp below 10 0 C. Condense: Charge H acid powder direct into VS cynuration and PH adjust by SBC 4.5 up to condense ok check spl and cool it to 5 temp. Diazotization: Charge MPDSA and clear it by NaOH lye ph 7.0 and cool it 10 0 C temp and dumped Cyanuric Chloride powder this solution transfer into ICE. Charge Sodium Nitrite and HCl at temp 0 check SI & CR +ve and temp 0 0 C stir for ½ hr make SI ve by sulfuric acid. Coupling: MPDSA Cyanurated diazo transfer into H condense mass below temp 0 than ph adjust by SBC 6.5 and maintain for 8 hr Check tone and strength. Spray Dryer: Transfer solutions in to holding tank for spray. Standardization: Charge Spray powder in Ball Mill and de dusting by antidusting oil. Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 20

21 Mass Balance: Mass Balance of Reactive Blue 194 Input Kg Output Kg Water 2450 VS 190 ICE 1000 HCl 330 Sodium Nitrite 94 H Acid 217 Reaction Vessel Cynuric Chloride 125 Caustic Lye 75 ICE 1800 Soda Ash 160 MPDSA 126 Cynuration Coupling Vinyl Sulphone 190 Condensation RO/MF w/w reuse 2650 Spray dryer drying loss 3107 Packing Reactive Blue Total Associated Dyestuff Pvt. Ltd., Unit-I 21

22 7. Direct Black 22 Manufacturing Process: Diazotization: F C Acid charged to a reaction vessel along with water. Then Hydrochloric Acid will be added followed by stirring. Charge ice then charge Sodium Nitrite. Maintain it for some time. Remove excess Nitrite by adding sulphamic acid. Keep temperature between 0 to 5 0 C throughout the diazotization reaction. Gamma acid clear solution: Charge Gamma Acid with water. Raise the ph of the mass by addition soda ash and caustic flakes up to the Stir it for 30 minutes. Add ice to drop temp around 0 0 C. First coupling: Transfer Gamma Acid clear solution in to F C Diazo slowly with temp 5 to 10 0 C. Stirr for 2 hr. Diazo of coupler mass: Charge ice with HCl in coupler mass. Then dump sodium nitrite. Stir the solution for 0.5 hr. Add ice to set temp 0 C. Remove excess nitrite by adding sulphamic acid. MPD clear solution: Charge water and heat it up to 50 0 C. Then charge MPD and stir for 30 minutes. Second coupling: Transfer first coupled mass in to MPD clear solution. After completion of addition adjust ph 8.5 by charging Soda ash solution. Stir the solution for 8 hrs. Do the filtration of coupling solution after raising the temp up to 40 0 C. Then Charge with water to make slurry. Spray Drying: The liquid transferred to the spray drying holding tank and spray dry. Associated Dyestuff Pvt. Ltd., Unit-I 22

23 Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 23

24 Associated Dyestuff Pvt. Ltd., Unit-I 24

25 Mass Balance: Mass Balance of Direct Black 22 INPUT KG OUTPUT KG F. C. Acid 195 Water 800 HCl 550 Ice 800 DIAZOTIZATION Sodium Nitrite 220 sulphamic acid 2 Gamma Acid 345 Water 1000 Soda Ash 325 Caustic Flakes 60 Copler Solution 1st COUPLING Ice 800 HCl 650 MPD 165 Steam 250 Soda Ash 250 Ice 500 MPD solution 2nd COUPLING RO SPRAY DRYING w/w reuse 2762 Drying loss 3150 Direct Black TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 25

26 8. Acid Black 210 Manufacturing Process: First make PNA Diazo coupled with H Acid in acidic medium at 50 o C stir for 4 hours then DASA Tetrazo coupled with first coupling in alkaline medium at 100 o C stir for 2 hours & then last above coupling with make Phenyl Diamine in alkaline ph at 100 o C then clarify & RO and spray dry it. Chemical Reaction: Diazotisation 1 ST Coupling DASA Tetrazotisation 2 nd Coupling 3 rd Coupling Associated Dyestuff Pvt. Ltd., Unit-I 26

27 Mass Balance: Mass Balance of ACID BLACK 210 INPUT KG OUTPUT KG PNA 128 HCL 82 Sodium Nitrite 64 DIAZOTIZATION Ice 1000 Water 1500 Water 1200 H.acid 285 1st COUPLING CO2 22 Soda Ash 54 Water 1000 DASA 224 HCL 144 Sodium Nitrite 118 Ice 1500 Caustic Flakes 192 Water 500 MPD 68 2nd COUPLING 3rd COUPLING RO SPRAY DRYING w/w reuse 3300 drying loss 3737 ACID BLACK TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 27

28 9. Reactive Blue 160 Manufacturing process: Diazotization: MPDSA charged to a MSRL reaction vessel along with water and ice to maintain temperature between 0 to 5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding Sulfamic Acid just before coupling. Keep temperature between 0 to 5 C throughout the diazotization reaction. Cyanuration: Cynuric Chloride will be added in the diazotized mass in alkaline medium while keeping temperature between 0 to 5 C throughout process. Coupling: Above mass is coupled with H Acid. Condensation: The mass is condensed with Metanilic acid and Live Steam. Spray Drying: Final product clarified dye solution is spray dried. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauber salt and anti dusted by anti-dusting oil. Packing: The final product is then packed in HDPE bags/m.s. Drums/ Plastic Carboys / Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 28

29 Mass Balance Mass Balance of Reactive Blue 160 INPUT KG OUTPUT KG Water 800 MPDSA 135 Ice 1000 HCl 170 Sodium Nitrite 52 Reaction Vessel Water 775 Cynuric Chloride 125 Caustic Lye 75 Ice 800 Soda Ash 168 H-Acid 115 Live Steam 350 Metanilic Acid 145 Cynuration Coupling Condensation RO / UF Spray drying w/w reuse 1275 drying loss 2435 Standardization & Packing Reactive Blue Total Associated Dyestuff Pvt. Ltd., Unit-I 29

30 10. Reactive Blue 198 Manufacturing Process: Disulphonic Acid in Cold. Stir well to complete the cyanuration. Condensation: Cynurated mass is added in the slurry of Blue 198 base and slowly heated to 50 o C 55 o C maintaining ph 7.0 and stir well to get complete reaction. Clarification: Final product dye solution is clarified to remove any insoluble foreign particles in clarifier. Spray Drying: Final product clarified dye solution is spray dried in spray dryer. The standardized dye liquid will be transferred to the spray drying holding tank and spray dry. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauger s Salt and anti dusted by antidusting oil. Packing: The final product is then packed in HDPE bags / M.S. Drums / Plastic Carboys/Paper cartoon boxes. Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 30

31 Mass Balance: Mass Balance of Reactive Blue 198 INPUT KG OUTPUT KG CYANURIC CHLORIDE 250 SODA ASH 180 TAMOL 8 ANILINE 2:4 DSA 340 SODA BI CARB 130 WATER 1250 ICE 1200 Cyanuration of Aniline 2:4 DSA BLUE HEGN-BASE 425 HCl 1000 WATER 1500 Condensation of Blue 198 Base DICAMOL 40 Solid waste 70 Clarification RO/UF w/w reuse 2310 SPRAY DRYING Drying loss 2943 Standardization & Packing Reactive Blue Total Associated Dyestuff Pvt. Ltd., Unit-I 31

32 11. Reactive Blue 220 Manufacturing process: Diazotisation: Sulfo OAVS is diazotised with HCl and sodium Nitrite at 0 C temperature and Stired well to complete diazo. Coupling: Sulfo OAVS diazo is coupled with 4-Sulfo Hydrazone in alkaline condition in presence of Copper sulfate to form the final dye is called Reactive Blue BB. Clarification: The final dye is clarified to remove un-reacted reactants or foreign particles. Spray Drying: Final product clarified dye solution is spray dried in spray dryer. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauber s salt and anti dusted by anti-dusting oil. Packing: The final product is then packed in HDPE bags / M.S. Drums / Plastic Carboys / Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 32

33 Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 33

34 Associated Dyestuff Pvt. Ltd., Unit-I 34

35 Mass Balance: Mass balance of reactive blue 220 INPUT KG OUTPUT KG SULPHO OAVS 530 HCL 147 SODIUM NITRITE 47 CS LYE 26 SULPHAMIC ACID 2 SODA ASH 112 WATER 1550 ICE 1350 Diazotization of Supho OAVS 4-SULPHO HYDRAZO 437 HCL 145 SODIUM NITRITE 45 CS LYE 27 SULPHAMIC ACID 2 SODA ASH 112 WATER 1250 ICE 1100 Coupling of 4 - Sulpho Hydrazone COPPER SULPHATE 340 SODA BI CARB 170 WATER 1400 Coppering DICAMOL 60 Solid Waste 100 Clarification RO/UF w/w reuse 4372 SD Drying loss 3400 Spray Drying Standardization & Packing reactive blue TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 35

36 12. Reactive Blue 19 Manufacturing process: Diazotization: Charge Meta Base Easter in M.S.R.L reaction vessel along with water and ice to maintain temperature 0-5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite solution gradually till diazotization completed, which can be confirmed by starch iodide paper. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Keep temperature between 0 to 5 C throughout the diazotization reaction. Preparation of coupling component:-charge Bromamine acid in the MSRL vessel and make clear solution with caustic solution. Coupling:-Charge coupler solution to the diazo mass keeping the temperature 0 to 5 C by adding ice. Maintain till coupling is completed which can be confirmed by coupling tests. Filter the coupled mass. Drying:-Filter the dye solution. Charge the wet cake in a vessel with water and make the slurry. Take it to the dryer. Mass Balance: Mass Balance of Reactive Blue 19 INPUT KG OUTPUT KG Meta Based Easter 260 Sodium Nitrite 84 Water 1250 Ice 1200 HCl 372 Sulphamic Acid 2 Diazotization Bromamine Acid 353 CS Flakes 116 Ice 1500 Coupling RO/UF W/w Reuse 1037 Spray Drying Drying loss 3100 Standardization & Packing Reactive Blue Total: Associated Dyestuff Pvt. Ltd., Unit-I 36

37 13. Reactive Blue 221 Manufacturing Process: Diazotization: 6-Acetyl OAPSA charged to a MSRL reaction vessel along with water and ice to maintain temperature between 0 to 5 C. Then Hydrochloric Acid will be added followed by Sodium Nitrite powder gradually till diazotization completed. Any excess nitrite will be removed by adding 1 to 2 kg Sulfamic Acid just before coupling. Coupling: Coupling of above mass with 4-Sulpho hydrazone Acid the diazotized 6-Acetyl OAPSA stir it keeping the temperature between 0 to 5 C by adding of ice. Coppering: The above mass coppering with Copper Sulphate is done at 95 C temperature. Isolation: Blue BRF base to be isolated with HCL to remove extra impurity by isolation. Cyanuration: Blue BRF Base is condensed with of Cyanuric Chloride in neutral condition at 0 C temp. Condensation: The Cyanurated product is further condensed with N-Ethyl Meta Base Ester Eater at 50 C temperature in presence of slightly access of Sodium Carbonate to get the final dye. Clarification: Final product dye solution is clarified to remove any insoluble foreign particles in clarifier. The standardized dye liquid will be transferred to the spray drying holding tank and spray dry. Spray Drying: Final product clarified dye solution is spray dried in spray dryer. Standardization: The spray dried powder is then charged to the Ball Mill and standardize be adding Glauber s salt and anti dusted by anti-dusting oil. Packing: The final product is then packed in HDPE bags/m.s. Drums/ Plastic Carboys/Paper cartoon boxes. Associated Dyestuff Pvt. Ltd., Unit-I 37

38 Chemical Reaction: Associated Dyestuff Pvt. Ltd., Unit-I 38

39 Mass Balance: INPUT KG REACTIVE BLUE 221 OUTPUT KG 6-ACETYL OAPSA 233 CS LYE 37 HCL 582 SODIUM NITRITE 66 SULPHAMIC ACID 1 SODIUM ACETATE 108 SODA ASH 45 WATER 1000 ICE 1000 Diazotization 4-SULPHO HYDRAZONE 300 SODA ASH 98 ICE 800 HCL 565 WATER 1000 Coupling COPPER SULPHATE 237 CS FLAKES 310 HOT water 750 Coppering CYANURIC CHLORIDE 152 TAMOL 7 Base Cyanuration N-ETHYL MBE 255 SODA BI CARB 155 Condensation with N-Ethyl Meta Base VS DICAMOL 46 solid waste 95 Clarification RO/UF W/w Reuse 3525 Spray Drying Drying loss 3127 REACTIVE BLUE Total Associated Dyestuff Pvt. Ltd., Unit-I 39

40 14. Reactive Turquoise Blue 21 Manufacturing Process: Charge chloro sulphuric acid into the vessel. Add CPC, keep temperature 50 o C. Then add PCl 3, raise temperature and maintain for 2 hrs. In condensation vessel take VS and maintain ph 5-8. After that add wet cake Sulphonator and pyridine then after spray dry the product. Chemical Reaction: 1. Sulphonation SO 3 H C - N C - C - N C - Cu + 2ClSO3 H CSA Cu + 2HCl N C - N C - copper phthalocyamne SO 3 H Direct Blue 2. Condensation SO 3 H M.W. 736 SO 3 NH 2 C - N C - NH 2 C - N C - Cu + Cu SO 2 CH 2 CH 2 OSO 2 N C - SO 2 CH 2 CH 2 OSO 3 H N C - + H 2 O SO 3 H Direct Blue vinyl sulphone NHSO 2 M.W. 736 M.W. 281 Reactive Blue G SO 2 CH 2 CH 2 OSO 3 H Associated Dyestuff Pvt. Ltd., Unit-I 40

41 Mass Balance: Mass Balance Reactive Terq. Blue 21 INPUT KG OUTPUT KG Copper Pthelo Cynine Blue 330 Chloro Sulphonic Acid 1320 Sulphonation HCl & SO2 225 PCl3 160 ICE 2000 Dumping WATER 1550 Filtration Spent H2SO4(30 TO 32 %) 3173 Vinyl Sulphone 310 ICE 1500 Condansation Sodium Bi Sulphte 210 Neutralization Spray Drying Drying loss 2982 Reactive Terq. Blue TOTAL Associated Dyestuff Pvt. Ltd., Unit-I 41

42 Annexure-III Break up of Water Consumption and Wastewater Generation Sr. No. Source Water Consumption (KLD) Existing Proposed addition I Domestic II Gardening III Industrial a) Process b) Scrubber c) Boiler d) Washing Total Industrial Total (I+II+III) Recycle water Actual fresh water requirement Total after expansion Sr. Source Wastewater Generation (KLD) No. Existing Proposed addition Total after expansion I Domestic II Gardening III Industrial a) Process b) Scrubber c) Boiler d) Washing Total Industrial Total (I+II+III) Associated Dyestuff Pvt. Ltd., Unit-I 42

43 Water Balance Diagram Total fresh water consumption 27.2 KLD (13.15 KLD Fresh water KLD recycle) Domestic 1.5 Process 7.5 Scrubber 2.0 Washing 8.0 Utility 7.5 Greenbelt 0.7 Soak pit 1.2 Ice Steam Water retained with RM 2.4 Boiler Spent H 2SO 4 Sold to actual users Process RO/UF HCl Spray Dryer for product recovery 8.0 Spray Drying Loss Blow down ETP = RO 9.75 Permeate for reuse 6.05* 8.0 RO permeate Close Loop Recycle 3.7 to CETP- Vatva Associated Dyestuff Pvt. Ltd., Unit-I 43

44 Annexure-III(a) Details of ETP Associated Dyestuff Pvt. Ltd., Unit-I 44

45 Sr. No. Types of Waste Annexure-IV Details of Hazardous waste generation Source Category of Waste as per HWM Rules ETP Sludge ETP Mt/month 2 Discarded containers/ barrels/liners Raw material storage Nos./month Spent Oil Gear box Lit/month 4 Dilute HCl (18-20%) 5 Spent H 2 SO 4 (30-32%) from scrubber of turquoise blue 21 from process of turquoise blue 21 Quantity Existing Proposed Total after expansion 2.2 Mt/month 3.0 Mt/month 400 Nos./month 0.2 Mt/month Kl/month Kl/month 500 Nos./month 0.2 Mt/month 5.0 Lit/month 10.0 Lit/month 26.0 Kl/month 31.0 Kl/month Sr. No. Types of Waste Details of Hazardous Waste Management Category of Waste as per HWM Rules 2016 Quantity Composition 1 ETP Sludge Mt/month Collection, storage, transportation & disposal at TSDF site approved by GPCB. 2 Discarded containers/ barrels/liners Nos./month & 0.2 Mt/month 3 Spent Oil Lit/month 4 Dilute HCl (18-20%) 5 Spent H 2 SO 4 (30-32%) Collection, storage, transportation & sell to registered recycler/reprocesser. Collection, storage, transportation & use within premises as a lubricant/sell to registered recycler Kl/month Collection, storage, re-use in process within premises Kl/month Collection, storage, and sell to actual users under Rule-9. Associated Dyestuff Pvt. Ltd., Unit-I 45

46 Sr. No. Annexure-V Source of Air Emission Stack attached to Fuel Type Stack Height (m) Flue Gas Stacks- Existing APC measures Probable emission Current steam requirement is accomplish from boiler of sister concern unit M/s. Associated Dyestuff Pvt. Ltd. (Unit-2) Flue Gas Stacks- Proposed 1 Steam Boiler (0.5 TPH) PNG-500 SCM/day Process Emission - Existing 11 Not Required SPM <150 mg/nm 3 No process gas emission, spay drying of liquid dyes is out sourced Process gas emission - Proposed 1 Process reactor of Turquoise Dyes 2 Spray Dryer (500 Kg/hr.) Water scrubber followed by alkali scrubber PNG-1500 SCM/day 21 Cyclone separator followed by water scrubber SO 2 <100 ppm NO x <50 ppm HCl<20 mg/nm 3 SO 2 <40 mg/nm 3 SPM <150 mg/nm 3 SO 2 <100 ppm NO x <50 ppm Associated Dyestuff Pvt. Ltd., Unit-I 46

47 s Annexure - VI Land Possession document I I '+ PC;/ 3310~ ((7 L &.?No. *)p'kxrs 3 "7, Comparing & Conies Charges 4' - i,. > ;. u$.- Total Rs... kb.~..?. %,. '?...,, IN THE HIGH COURT OF GUJARAT AT AHMEDABAD ORIGINAL JURISDICTION COMPANY PETITION ~ OF Section Officers Decree Department Dt. 14 I[ [2000 I I CONNECTED WITH COMPANY APPLICATION ~0.750~ 2013 CQPY ~pplled on : ~t.3 C~PY Ready on :, c 3 Notified 0x1 In the matter of Scheme of Arrangement under Sections 391 and 39'4 read with Sec. 100 to 103 of the Companies ~ kt, 1956; i Iln the matter of And I Associated Dyestuff Private Limited. A Company registered under the Companies Act, i I

48 Y, "Demerged underthing" means Dyes Division of the Demerged Company, on a going concern basis, comprising, inter alia, the assets - - and liabilities (without limitation): relating thereto and which shall mean and include (i) all assets situate at Plot No. 74/3, Shed A-1/5, GIDC, Phase-1, Vatva in the state of Gujarat, admeasuring 2989 Sq. Mtrs. Out of total land admeasuring 3512 Sq. Mtrs, whether movable or immovable, tangible or intangible, including all buildings, offices,.. godowns, investments, interest, capital work-in-progress, furniture, furtures, office equipment, appliances, accessories, etc. pertaining to

49 I 1 B I LEAVE AND LICENCE AGREEMENT THIS DEED OF LEAVE AND LICENCE AGREEMENT is made on the day of 24th October, 2018 BETWEEN M/s. Associated Dvestuff Pvt. Ltd., Unit - I. (hereinafter called the "LESSEE") of the one part Associated Dvestuff Pvt. Ltd., Unit-2 Having Director Viral Hemendrabhai Shah (hereinafter called the 'LESSOR") of the other part. WHEREAS the Lessor are the owners of the adjacent Industrial plot 1 situated at Plot No- A-1/4, G.I.D.C., Phase-I, Vatva, Ahmedabad. Out of total plot area, Lessor agreed to give 751 Sa.Mtr. on lease to!, Lessee. I 6 AND WHEREAS the Lessee has expressed his desirous to take on lease from Associated Dvestuff Pvt. Ltd., Unit-2 the said premises 4 on the terms and conditions hereinafter appearing.

50 NOW THIS DEED WI'TNESSES AS UNDER: I. LEASE RENT Being a sister concern, land owner of Associated Dyestuff Pvt. Ltd., Unit-I will take token payment of Rs (Rupees Five Hundred Only) as lease rent in respect of the said premises. 2. SUB - LETTING. 'The lessee shall not, be entitled to sub-let the said premises to any other person except with the written consent of the lessor previously obtained PERIOD OF LEASE: The lease period will be minimum 10 years and it will be mutually extended. LICENSOR MIS. Associated Dyestuff Pvt. Ltd., Unit - 2 : LICENSEE MIS. Associated Dyestuff Pvt. Ltd., Unit - I :