proposed dyes & dyes intermediates, pigments, speciality chemicals & pesticide...

1

FORM-I

For

PROPOSED DYES & DYES INTERMEDIATES,

PIGMENTS, SPECIALITY CHEMICALS &

PESTICIDE INTERMEDIATES UNIT

of

M/s. ALPS CHEMICALS PVT. LTD.

PLOT NO. DP-102/103, G.I.D.C. SAYKHA,

TALUKA: VAGRA, DISTRICT: BHARUCH, GUJARAT

Prepared by:

Aqua-Air Environmental Engineers Pvt. Ltd. (Pollution Control Consultants & Engineers)

Reg. Office: 403, Centre Point, Nr. Kadiwala School, Ring Road,

Surat – 395 002, Gujarat, India Fax: +91 261 2707273 / 3987273

Tel: + 91 261 3048586 / 2460854 / 2461241

E-mail: [email protected] Visit us at: www.aqua-air.co.in

2

APPENDIX I

FORM 1

(I) Basic Information

Sr.

No.

Item Details

1. Name of the Project/s M/s. Alps Chemicals Pvt. Ltd.

2. S. No. in the Schedule 5(f) & 5(b)

3. Proposed

capacity/area/length/tonnage to be

handled/command area/lease

area/number of wells to be drilled

Dyes

Acid Dyes = 500 MT/Month

Direct Dyes = 1,000 MT/Month

Reactive Dyes = 250 MT/Month

Disperse Dyes = 500 MT/Month

Solvent Dyes = 50 MT/Month

Dye Intermediates = 250 MT/Month

Pigments = 500 MT/Month

Specialty Chemicals = 200 MT/Month

Pesticide Intermediates = 100 MT/Month

Total Production = 3,350 MT/Month

4. New/Expansion/Modernization New

5. Existing capacity/area etc. Not Applicable

6. Category of project i.e. ‘A’ or ‘B’ ‘A’

7. Does it attract the general condition? If

yes, please specify.

Not Applicable

8. Does it attract the specific condition? If

yes, please specify.

Not Applicable

9. Location Plot No. DP-102/103, GIDC Saykha, Taluka: Vagra,

District: Bharuch, Gujarat.

Plot/Survey/Khasra No. Plot. No. DP-102/103

Village Saykha

Tehsil Vagra

District Bharuch

State Gujarat

10. Nearest railway station/airport along

with distance in kms.

Nearest Railway Station: Bharuch = 20 kms

Nearest Airport: Baroda = 75 kms

11. Nearest Town, city, District

Headquarters along with distance in

km

Nearest Town: Bharuch = 20 kms

Nearest District Head quarter: Bharuch = 20 kms

12. Village Panchayats, zilla parishad,

Municipal corporation, Local body

Village: Saykha, Taluka: Vagra, District: Bharuch,

Gujarat.

3

13. Name of the applicant M/s. Alps Chemicals Pvt. Ltd.

14. Registered address Plot No. 612, Phase 4, GIDC, Vatva, Ahmedabad-

382445

15. Address for correspondence:

Name Mr. Chinmay Bhuta

Designation (Owner/Partner/CEO) Director

Address Plot No. 612, Phase 4, GIDC, Vatva, Ahmedabad

Pin Code 382445

E-Mail [email protected]

Mobile No. +919998228999

Fax No. --

16. Details of Alternative Sites examined, if

any location of these sites should be

shown on a topo sheet.

No

17. Interlinked Projects No

18. Whether separate application of

interlinked project has been

submitted?

Not Applicable

19. If Yes, date of submission Not Applicable

20. If no., reason Not Applicable

21.

Whether the proposal involves

approval/clearance under: If yes,

details of the same and their status to

be given.

(a) The Forest (Conservation) Act,

1980?

(b) The Wildlife (Protection) Act,

1972?

Not Applicable, as the project is located in notified

industrial estate.

22. Whether there is any Government

order/policy relevant/relating to the

site?

No

23. Forest land involved (hectares) No

24. Whether there is any litigation pending

against the project and/or land in

which the project is propose to be set

up?

(a) Name of the Court

(b) Case No.

(c) Orders/directions of the Court, if

any and its relevance with the project.

No

4

(II) Activity

1. Construction, operation or decommissioning of the Project involving actions, which

will cause physical changes in the locality (topography, land use, changes in water

bodies, etc.)

Sr.

No.

Information/Checklist confirmation Yes

/No?

Details thereof (with approximate quantities

/ rates, wherever possible) with source of

information data

1.1 Permanent or temporary change in

land

use, land cover or topography

including

increase in intensity of land use (with

respect to local land use plan)

No Proposed Project is within Saykha GIDC

Estate.

1.2 Clearance of existing land, vegetation

and buildings?

Yes Minor site clearance activities shall be carried

out to clear shrubs and weed.

1.3 Creation of new land uses? No --

1.4 Pre-construction investigations e.g.

bore houses, soil testing?

No --

1.5 Construction works? Yes Plant layout is attached as Annexure-1.

1.6 Demolition works? No --

1.7

Temporary sites used for construction

workers or housing of construction

workers?

No --

1.8 Above ground buildings, structures or

Earthworks including linear structures,

cut and fill or excavations

Yes Plant layout is attached as Annexure-1.

1.9

Underground works including mining

or tunneling?

No --

1.10 Reclamation works? No --

1.11 Dredging? No --

1.12 Offshore structures? No --

1.13 Production and manufacturing Yes List of Products is attached as Annexure-2

and manufacturing process is attached as

Annexure-3.

1.14 Facilities for storage of goods or

materials?

Yes Dedicated storage area for storage of Raw

Materials and finished products, solvents, etc.

shall be provided.

1.15

Facilities for treatment or disposal of

solid waste or liquid effluents?

Yes Effluent Treatment Plant & MEE system will

be installed to treat effluent so as to achieve

the GPCB norms.

Details of Effluent Treatment Plant are

attached as Annexure-5.

5

Details of Hazardous waste management and

disposal is attached as Annexure-6.

1.16

Facilities for long term housing of

operational workers?

No --

1.17 New road, rail or sea traffic during

construction or operation?

No --

1.18 New road, rail, air waterborne or

other airports etc?

No --

1.19 Closure or diversion of existing

transport routes or infrastructure

leading to changes in traffic

movements?

No --

1.20 New or diverted transmission lines or

pipelines?

No --

1.21

Impoundment, damming, converting,

realignment or other changes to the

hydrology of watercourses or

aquifers?

No --

1.22 Stream crossings? No --

1.23

Abstraction or transfers or the water

form ground or surface waters?

Yes No ground water shall be used. The

requirement of raw water will meet through

Saykha GIDC Authority.

1.24

Changes in water bodies or the land

surface affecting drainage or run-off?

No --

1.25

Transport of personnel or materials for

construction, operation or

decommissioning?

Yes Through hired Services.

1.26 Long-term dismantling or

decommissioning or restoration

works?

No --

1.27 Ongoing activity during

decommissioning which could have

an impact on the environment?

No --

1.28

Influx of people to an area in either

temporarily or permanently?

No This is a newly developed Industrial Area and

due to project, 150 people shall be employed

for operation.

1.29 Introduction of alien species? No --

1.30 Loss of native species of genetic

diversity?

No --

1.31 Any other actions? No --

6

2. Use of Natural resources for construction or operation of the Project (such as land, water,

materials or energy, especially any resources which are non-renewable or in short supply):

Sr.

No

Information/checklist confirmation Yes/

No?

Details there of (with approximate

quantities/rates, wherever possible) with

source of information data

2.1 Land especially undeveloped or

agriculture land (ha)

No --

2.2 Water (expected source & competing

users) unit: KLD

Yes Water requirement will meet through

Saykha GIDC Authority. Water balance is

given as Annexure-4.

2.3 Minerals (MT) No --

2.4

Construction material -stone,

aggregates, sand / soil (expected

source MT)

Yes Company shall use Sand, Stone, Cement and

Structural Steel for Construction as required.

2.5 Forests and timber (source - MT) No --

2.6

Energy including electricity and fuels

source, competing users Unit: fuel

(MT), energy (MW)

Yes Power Requirement:

Power required from DGVCL is 1000 KVA.

DG set = 1000 KVA (Stand by)

Fuel Requirement:

Coal = 50 T/Day

Diesel/Gas = 8400 L/Day

2.7 Any other natural resources

(use appropriates standard units)

No --

3. Use, storage, transport, handling or production of substances or materials, which could be

harmful to human health or the environment or raise concerns about actual or perceived

risks to human health.

Sr.

No.

Information / Checklist confirmation Yes/

No?

Details thereof (with approximate

quantities / rates wherever possible) with


3.1 Use of substances or materials, which

are hazardous (as per MSIHC rules) to

human health or the environment

(flora, fauna, and water supplies)

Yes

Please refer Annexure-8.

3.2 Changes in occurrence of disease or

affect disease vectors (e.g. insect or

water borne diseases)

No --

3.3 Affect the welfare of people e.g. by

changing living conditions?

No --

Vulnerable groups of people who No --

7

3.4

could be affected by the project e.g.

hospital patients, children, the elderly

etc.,

3.5 Any other causes No --

4. Production of solid wastes during construction or operation or decommissioning

(MT/month)

Sr.

No.

Information/Checklist confirmation Yes/

No?


quantities / rates, wherever possible) with


4.1 Spoil, overburden or mine wastes No --

4.2

Municipal waste (domestic and or

commercial wastes) No --

4.3

Hazardous wastes (as per Hazardous

Waste Management Rules)

Yes Please refer Annexure-6.

4.4 Other industrial process wastes Yes Please refer Annexure-6.

4.5 Surplus product No --

4.6

Sewage sludge or other sludge from

effluent treatment

Yes Please refer Annexure-6.

4.7 Construction or demolition wastes No --

4.8 Redundant machinery or equipment No --

4.9 Contaminated soils or other materials No --

4.10 Agricultural wastes No --

4.11 Other solid wastes No --

5. Release of pollutants or any hazardous, toxic or noxious substances to air (Kg/hr)

Sr.

No.


No?


quantities/rates, wherever possible) with


5.1 Emissions from combustion of fossil

fuels From stationary or mobile

sources

Yes Details of flue & process gas emission are


5.2 Emissions from production processes Yes Details of emission from process are


5.3 Emissions from materials handling

including storage or transport

Yes All liquid raw materials shall be procured in

bulk tankers and shall be transferred

through a closed circuit pipe lines by

pumps.

Solid raw material shall be handled in

closed charging rooms with proper

8

ventilation and charged through close

pipeline into reactors.

5.4 Emissions from construction

activities including plant and

equipment

No --

5.5

Dust or odors from handling of

materials including construction

materials, sewage and waste

No --

5.6 Emissions from incineration of waste No --

5.7 Emissions from burning of waste in

open air (e.g. slash materials,

construction debris)

No --

5.8 Emissions from any other sources No --

6. Generation of Noise and Vibration, and Emissions of Light and Heat:

Sr.

No.


No?

Details there of (with approximate

Quantities /rates, wherever possible) With

source of source of information data

6.1

From operation of equipment e.g.

engines, ventilation plant, crushers

Yes Acoustic enclosures shall be provided for DG

set.

6.2 From industrial or similar processes Yes All machinery / equipment shall be well

maintained, shall have proper foundation

with anti vibrating pads wherever applicable

and noise levels within permissible limits.

Acoustic enclosures shall be provided for DG

set.

6.3 From construction or demolition No --

6.4 From blasting or piling No --

6.5 From construction or operational

traffic No

--

6.6 From lighting or cooling systems No --

6.7 From any other sources No --

9

7. Risks of contamination of land or water from releases of pollutants into the ground or

into sewers, surface waters, groundwater, coastal waters or the sea:

Sr.

No


No?




7.1

From handling, storage, use or

spillage of hazardous materials

Yes All the raw material shall be stored

separately in designated storage area and

safely. Dyke walls shall be provided around

raw materials storage tanks for containing

any liquid spillage.

Other materials shall be stored in bags /

drums on pallets with concrete flooring and

no spillage is likely to occur.

Please refer Annexure-8.

7.2

From discharge of sewage or other

effluents to water or the land

(expected mode and place of

discharge)

No Sewage shall be treated in Septic Tank &

Soak Pit.

7.3

By deposition of pollutants emitted

to air into the land or into water

No --

7.4 From any other sources No --

7.5 Is there a risk of long term build up of

pollution in the environment from

these sources?

No

--

8. Risks of accident during construction or operation of the Project, which could affect

human health or the environment:

Sr.

No

Information/Checklist confirmation

Yes/

No?




8.1 From explosions, spillages, fires, etc.

from storage, handling, use or

production of hazardous substances

Yes The risk assessment will be carried out and

all mitigate measures shall be taken to avoid

accidents.

8.2 From any other causes No --

8.3 Could the project be affected by

natural disasters causing

environmental damage (e.g. floods,

earthquakes, landslides, cloudburst

etc)?

No --

10

9. Factors which should be considered (such as consequential development) which could lead

to environmental effects or the potential for cumulative impacts with other existing or

planned activities in the locality

Sr.

No.


No?




9.1 Lead to development of supporting

facilities, ancillary development or

development stimulated by the

project which could have impact on

the environment e.g.:

* Supporting infrastructure (roads,

power supply, waste or waste water

treatment, etc.)

• housing development

• extractive industries

• supply industries

• other

Yes Site is located in Saykha GIDC, shall have

entire required infrastructure.

This industrial zone is having existing road

infrastructure, power supply are to be

utilized.

Local people will be employed and no

housing is required.

Please refer Annexure–9.

9.2

Lead to after-use of the site, which

could have an impact on the

environment

No --

9.3 Set a precedent for later

developments No --

9.4 Have cumulative effects due to

proximity to Other existing or planned

projects with similar effects

No --

11

(III) Environmental Sensitivity

Sr.

No.

Information/Checklist confirmation Name /

Identity

Aerial distance (within 25 km). Proposed

Project Location Boundary.

1 Areas protected under international

conventions national or local

legislation for their ecological,

landscape, cultural or other related

value

Yes Site is located in Saykha GIDC, Village:

Saykha, Taluka: Vagra, District: Bharuch,

Gujarat.

2 Areas which are important or sensitive

for Ecological reasons - Wetlands,

watercourses or other water bodies,

coastal zone, biospheres, mountains,

forests

No Site is located in Saykha GIDC, Village:


Gujarat.

Forest area of Rajpipla is 75 kms away.

3 Areas used by protected, important or

sensitive species of flora or fauna for

breeding, nesting, foraging, resting,

over wintering, migration

No Site is located in Saykha GIDC, Village:


Gujarat.

4 Inland, coastal, marine or

underground waters

Yes Arabian Sea = 35 kms

River Narmada = 12 kms

5 State, National boundaries No --

6 Routes or facilities used by the public

for to recreation or other tourist,

pilgrim areas.

No --

7 Defense installations No --

8 Densely populated or built-up area Yes Bharuch city = 5 lakh population

9 Areas occupied by sensitive man-

made land community facilities)

No --

10 Areas containing important, high

quality or scarce resources (ground

water resources, surface resources,

forestry, agriculture, fisheries,

tourism, tourism, minerals)

Yes

The project being in notified industrial area

does not affect agricultural land.

11 Areas already subjected to pollution

or environmental damage. (those

where existing legal environmental

standards are exceeded)

Yes Site is located in Saykha GIDC, Village:


Gujarat.

12 Are as susceptible to natural hazard

which could cause the project to

present environmental problems

(earthquake s, subsidence ,landslides,

flooding erosion, or extreme or

adverse climatic conditions)

No --

13

ANNEXURES

1 PLANT LAYOUT

2 LIST OF PRODUCTS WITH PRODUCTION CAPACITY

3 BRIEF MANUFACTRING PROCESS, CHEMICAL REACTION AND MASS BALANCE WITH

FLOW DIAGRAM

4 WATER CONSUMPTION AND WASTEWATER GENERATION

5 DESCRIPTION OF EFFLUENT TREATMENT PLANT AND MEE SYSTEM

6 DETAILS OF SOLID HAZARDOUS WASTE MANAGEMENT AND DISPOSAL

7 DETAILS OF FLUE AND PROCESS GAS EMISSION

8 DETAILS OF HAZARDOUS CHEMICAL STORAGE FACILITY

9 SOCIO ECONOMIC IMPACTS

10 PROPOSED DRAFT TERMS OF REFERENCE

14

ANNEXURE: 1

_____________________________________________________________________________

PLANT LAYOUT

15

ANNEXURE: 2

________________________________________________________________________

LIST OF PRODUCTS WITH PRODUCTION CAPACITY

Sr. No. Name of Product Proposed Capacity

Dyes

Acid Dyes

500 MT/Month

1 Acid Black 1

2 Acid Black 52

3 Acid Black 63

4 Acid Black 71

5 Acid Black 84

6 Acid Black 107

7 Acid Black 172

8 Acid Blue 158

9 Acid Brown 75

10 Acid Brown 161

11 Acid Brown 165

12 Acid Brown 355

13 Acid Brown 425

14 Acid Brown 432

15 Acid Brown 434

16 Acid Green 104

17 Acid Orange 74

18 Acid Orange 142

19 Acid Red 97

20 Acid Red 357

21 Acid Violet 90

22 Acid Yellow 42

23 Acid Yellow 59

24 Acid Yellow 194

Direct Dyes

1 Direct Black 40

2 Direct Black 168

3 Direct Blue 71

4 Direct Green 26

5 Direct Orange 15

6 Direct Orange 118

16

7 Direct Red 81 1000 MT/Month

8 Direct Red 239

9 Direct Red 254

10 Direct Violet 9

11 Direct Violet 35

12 Direct Yellow 11

13 Direct Yellow 44

Reactive Dyes

1 Reactive Black B

250 MT/Month

2 Reactive Red-195

3 Reactive Golden Yellow-145

4 Reactive Golden Yellow Her

5 Reactive Orange H2R

Reactive Blue

6 Blue 3R

7 Blue F4R

8 Blue HERD

9 Blue 221

10 Blue HEGN

11 Blue LFNG

12 Blue BF

13 Blue BFN

14 Blue 2B

Reactive Golden Yellow

15 Golden Yellow R

16 Golden Yellow RNL

Reactive Navy Blue

17 Navy Blue 2G

18 Navy Blue XLE

19 Navy Blue RGB

Disperse Dyes

1. Azo Dyes

a. Yellow Dyes

b. Orange Dyes

c. Red Dyes

d. Blue Dyes

e. Violet Dyes

17

f. Green Dyes

500 MT/Month

g. Black Dyes & Mixtures

2. Anthraquinones/Condensed Dyes

a. Yellow Dyes

b. Orange Dyes

c. Red Dyes

d. Blue Dyes

e. Violet Dyes

f. Green Dyes


3. Cyanation Dyes

a. Yellow Dyes

b. Orange Dyes

c. Red Dyes

d. Blue Dyes

e. Violet Dyes

f. Green Dyes


Solvent Dyes

1 Solvent Blue 35

50 MT/Month

2 Solvent Blue 104

3 Solvent Blue 122

4 Solvent Green 3

5 Solvent Orange 60

6 Solvent Orange 86

7 Solvent Red 52

8 Solvent Red 135

9 Solvent Red 168

10 Solvent Red 195

11 Solvent Red 207

12 Solvent Violet 13

13 Solvent Violet 14

14 Solvent Yellow 33



17 Solvent Orange 58

18 Solvent Red 127

18

19 Solvent Black 27

Dye Intermediates

1 H Acid

250 MT/Month

2 J Acid

3 6 Nitro 1-Diazo, 2-Naphthol, 4-Sulphonic

Acid

4 Vinyl Sulphone

5 Pyrazolones

a. 2:5 Dichloro 4 Sulpho Phenyl 3 Methyl 5

Pyrazolone

b. 2 Chloro 5 Sulphophenyl 3 Methyl 5

Pyrazolone

c. 1,3 Sulpho Phenyl 3 Methyl 5 Pyrazolone

d. 1,4 Sulpho Phenyl 3 Methyl 5 Pyrazolone

e. 1:3 Phenyl Methyl 5 Pyrazolone

Pigments

1 Activated CPC Blue

500 MT/Month

2 CPC Blue

3 Alpha Blue (15:0 and 15:1)

4 Pigment Beta Blue (15:3)

5 Pigment Beta Blue (15:4)

6 Copper Phthalocyanine Pigment Green-7

7 Pigment Violet 23

8 Pigment Red 122

9 Pigment Violet 19

10 Solsperse 5000

11 Carbazole

Speciality Chemicals

1 2,4-Dichloro Phenyl Acetic Acid

200 MT/Month

2 2,4-Dichloro Phenyl Acetyl Chloride

3 2,4,6-Trimethyl Phenyl Acetyl Chloride

4 2,3,4,5-Tetrachloro Benzoyl Chloride

5 3,4,5 Trimethoxy Benzyl Chloride

Pesticide Intermediates

1. 2-Amino Benzo Nitrile

2. 2-Amino-5-Bromo Benzo Nitrile

19

3. 2,4,6-Trimethyl Benzaldehyde 100 MT/Month

4. Indoline

5. 5-(1-Carboxy Ethyl)-2-(Phenylthio)Phenyl

Acetic Acid

TOTAL 3350 MT/Month

20

LIST OF RAW MATERIALS

Sr. No. Product Name MT/MT

Acid Dyes

Acid Black 1

1 H-Acid 0.337

2 Caustic lye 0.096

3 PNA 0.150

4 Hydrochloric acid, 30% 0.650

5 Aniline 0.097

6 Sodium Nitrite 0.158

7 Water 1.100

8 Ice 2.400

9 Soda ash 0.200

Acid Black 52

1 6-Nitro 0.446

2 Beta Napthol 0.214

3 NaOH 0.321

4 Basic Chromium Sulphate 0.268

5 Steam 2.160

6 Water 1.800

7 Ice 1.690

8 Salicylic Acid 0.055

Acid Black 63

1 5-NAP 0.500


3 Ice 2.000



6 Caustic lye, 48% 0.800

7 Chrome Salam 1.500

8 Water 2.000

Acid Black 71

1 Sodium Bi-sulphite 0.357

2 Formaldehyde 0.250

3 Gamma Acid 0.365

4 J-Acid 0.064

5 Soda ash 0.070

6 Sodium Picramate 0.384

7 Sodium Dichromate 0.140

8 Sulphuric acid, 98% 0.108

9 Sorbitol 0.060

10 Sodium Formate 0.066

21



13 Water 2.000

14 Ice 1.500

Acid Black 84

1 Sodium bi-sulphite 0.365

2 Formaldehyde 0.245

3 Gamma acid 0.473

4 4NAPSA 0.431

5 Hydrochloric acid 30% 0.122


7 Soda ash 0.422

8 Ice 4.200

9 Water 3.700

Acid Black 107



3 Hydrochloric Acid 0.360

4 Caustic Flakes 0.075


6 Ice 1.00

7 6-Nitro 0.360


9 Caustic Lye 22.50

10 Chromuim Formate 0.325

11 Sulphuric Acid 0.120

12 Oxalic Acid 0.045


14 Water 1.150

Acid Black 172

1 6-Nitro 0.446


3 NaOH 0.321


5 Water 1.20

6 Ice 1.50

Acid Blue 158

1 Naptha Sultan 0.489

2 Caustic potash 0.555

3 Ammonium Sulphate 0.066

4 1-2-4 Diazo acid 0.555

5 Sodium Bi-chromate 0.445


22

7 Sorbitol 0.213


9 Ice 1.80

10 Water 1.80

11 Soda ash 0.10

Acid Brown 75

1 H-Acid 0.240

2 Soda ash 0.050



5 Resorcinol 0.084


7 Picramic acid 0.168

8 PNA 0.125

9 Water 1.150

10 Ice 3.00

Acid Brown 161

1 Anthranilic acid 0.154


3 Formaldehyde, 32% 0.061


5 Resorcinol 0.120


7 Sulphanilic acid 0.189

8 Hydrochloric acid 0.412

9 CuSO4. 5H2O 0.284

10 Water 2.450

11 Ice 3.900

Acid Brown 165

1 H-Acid 0.076




5 Resorcinol 0.070


7 Paranitro Aniline 0.112

8 Water 2.350

9 Ice 3.200

10 Ferric chloride 0.261

Acid Brown 355

1 4-NAPSA 0.333

2 PMP 0.264


23



6 Sodium Acetate 0.128

7 Potassium chloride 1.438

8 6-Nitro-1-Diazo acid 0.375


10 BCS, 16% 0.437

11 Salicylic acid 0.026


13 Water 4.515

14 Ice 3.500

15 Steam condensate 2.500

Acid Brown 425


2 O.T.5 SA 0.250



5 Resorcinol 0.150

6 Soda ash 0.350



9 Chromium Fluoride 0.128

10 Liq. Ammonia 0.078

11 Ice 2.000

12 Water 1.800

Acid Brown 432


2 Resorcenol 0.150

3 Lorrent acid 0.285



6 Soda ash 0.350


8 Caustic soda Flakes 0.057



11 Ice 2.300

12 Water 2.300

Acid Brown 434

1 Sodium Picrame 0.296

2 Resorcinol 0.145

3 Mix cleave acid 0.336


24


6 Sulfamic acid 0.002

7 Caustic flakes 0.140

8 Caustic lye 0.189

9 Ferrous sulphate 0.260

10 Water 1.800

11 Ice 3.000

Acid Green 104


2 Dahl's Acid 0.419



5 Ice 3.350


7 Cobalt Sulphate, 20% 0.295

8 Water 3.250

Acid Orange 74

1 4-NAPSA 0.530



4 PMP 0.425



7 Ice 2.500


9 BCS, 16% 0.900

10 Water 2.200

Acid Orange 142

1 Water 1.980

2 Ice 2.750

3 4NAPSA 0.363



6 Sulphamic acid 0.002

7 PMP 0.290



10 Sodium dichromate 0.136

11 Sorbitol 0.065



Acid Red 97

1 BDSA 0.455

25





6 Water 2.625

7 Ice 1.500

Acid Red 357

1 6NAPSA 0.358


3 PMP 0.280



6 Green solution 0.450

7 Water 2.350

8 Ice 1.200


Acid Violet 90

1 1-2-4 Diazo acid 0.400

2 PMP 0.304



5 BCS, 16% 0.266


7 Water 3.200

Acid Yellow 42

1 BDSA 0.360

2 PMP 0.410





7 Water 2.300

8 Ice 4.750

Acid Yellow 59


2 PMP 0.194

3 BCS, 16% Cr. 0.208

4 Formic acid, 85% 0.450

5 Ice 1.500




9 Water 1.050

26

10 Dispersing agent 0.600

Acid Yellow 194

1 4NAPSA 0.476

2 AAA 0.381





7 Ice 2.600

8 Water 2.600

Direct Dyes

Direct Black 40

1 PAA 0.150

2 Gamma acid 0.465

3 Mix Cleave acid 0.223



6 Caustic lye 0.263

7 Soda ash 0.475



10 Water 2.050

11 Ice 4.000

Direct Black 168

1 FC Acid 0.307

2 H-Acid 0.307



5 Aniline Oil 0.093

6 Soda ash 0.561

7 MPD 0.114

8 Ice 3.700

9 Water 1.900

Direct Blue 71

1 C-Acid 0.336

2 Napthyl Amine 0.170

3 Mix Cleave Acid 0.220



6 J-Acid 0.260

7 Caustic soda lye, 48% 0.050


9 Water 2.600

27

10 Ice 3.900

Direct Green 26

1 BHK Acid 0.434

2 H-Acid 0.234




6 Soda ash 0.177

7 PAPA's acid 0.154

8 Cyanuric chloride 0.110

9 Reaction oil 0.015

10 Aniline Oil 0.086

11 Ice 2.900

12 Water 3.600

Direct Orange 15

1 PNTOSA 0.818



4 Dichlone 0.025

5 Spent Acid, 50% 1.800

6 Ice 1.000

7 Water 1.500

Direct Orange 118

1 p-Cresidine-o-Sulphonic acid 0.231



4 Sodium bi-carbonate 0.475

5 J-Acid Urea 0.315

6 Water 3.000

7 Ice 3.500

Direct Red 81

1 PAABSA 0.308




5 J-Acid 0.279

6 Benzoyl Chloride 0.257



9 Soda ash 0.062

10 Water 2.800

11 Ice 2.000

Direct Red 239

28

1 Browner's acid 0.250

2 caustic lye, 48% 0.100



5 J-Acid Urea 0.292

6 Soda bi-carb, 25% 0.250

7 Soda ash, 20% solu. 0.100

8 Water 2.500

9 Ice 3.500

Direct Red 254

1 PAABSA 0.406

2 Caustic lye 0.200



5 J-Acid 0.351

6 Soda ash 0.300

7 Water 2.700

8 Ice 4.700

Direct Violet 9


2 p-Cresidine 0.150

3 n-Phenyl J Acid 0.327





8 Soda ash 0.175

9 Ice 3.800

10 Water 1.900

Direct Violet 35

1 C-Acid 0.331

2 p-Cresidine 0.150

3 n-Phenyl-J Acid 0.327





8 Soda ash 0.175

9 Ice 2.500

10 Water 2.000

Direct Yellow 11

1 PNTOSA 0.290


29

3 Nitrobenzene 0.016

4 Tri-Butyl Amine 0.021

5 Di-Ethanol Amine 0.160

6 Sulphuric Acid-70% 0.500

7 Water 3.250

8 Steam 0.150

Direct Yellow 44

1 MAMA'S Acid 0.787

2 BIS (Trichloro Methyl) Carbonate 0.375

3 Sodium Bi-Carbonate 0.625

4 Water 6.500

Reactive Dyes

Reactive Black B

1 Vinyl Sulphone 0.400

2 HCl 0.100


4 H Acid 0.230

5 Sodium BI Carbonate 0.230

6 Salt 0.140

Reactive Red-195


2 NaHCO3 0.210

3 Cynauric Chloride 0.150

4 H Acid 0.270

5 Na2CO3 0.090

6 STA Diazo 0.290

7 NaCl 0.050

Reactive Golden Yellow-145

1 K Acid 0.390


3 HCl 0.080

4 MUA 0.160


6 VS 0.290

Reactive Golden Yellow HER

1 K Acid 0.390


3 HCl 0.080

4 MUA 0.160


6 DASDA 0.350

Reactive Orange H2R

1 NMJ Acid 0.290

30

2 Sodium Hydroxide 0.050

3 Acetic Anhydride 0.120

4 Sulpho Tobias Acid 0.350

5 HCl 0.080


7 NaHCO3 0.190

8 NaOH 0.050

9 Cyanuric Chloride 0.210

10 NH4OH 0.040

Reactive Blue

Blue 3R

1 H Acid 0.032

2 Antifoam 0.005

3 Sulfamic Acid 0.001

4 SPD Oil 0.002

5 DDC Oil 0.010

6 Soda Ash 0.045

7 Sodium Sulphate 0.484

8 Sodium Bi Carbonate 0.041


10 Copper Sulphate 0.249

11 Caustic Soda 0.067

12 HCl 0.037

13 DMAVS 0.234

14 Acetic Anhydride 0.146

Blue F4R


2 Oil HS 0.001

3 4 ADPSA 0.082

4 H Acid 0.100


6 Antifoam 0.004


8 SPD Oil 0.002

9 DDC Oil 0.001

10 Soda Ash 0.113




14 HCl 0.125

Blue HERD


2 Oil HS 0.003.

31

3 6 AAPSA 0.106

4 4 Sulpho Hydrogen 0.133

5 Antifoam 0.003


7 SPD Oil 0.003

8 DDC Oil 0.010

9 Soda Ash 0.095






15 HCl 0.199

16 PPDDSA 0.069

Blue 221


2 Oil HS 0.002

3 6 AAPSA 0.171

4 NEPBE 0.178


6 Antifoam 0.005


8 SPD Oil 0.003

9 DDC Oil 0.010

10 Soda Ash 0.125


12 Sodium Bi carbonate 0.212




16 HCl 0.363

Blue HEGN


2 Oil HS 0.003

3 Aniline 2,4 Di Sulpho Acid 0.206

4 Antifoam 0.005

5 Blue 198 Base 0.200

6 SPD Oil 0.003

7 DDC Oil 0.020

8 Soda Ash 0.173



Blue LFNG

32


2 Oil HS 0.003

3 Aniline 2,5 Di Sulpho Acid 0.239

4 Meta Base Ester 0.296

5 Antifoam 0.005

6 Blue 198 Base 0.250

7 SPD Oil 0.005

8 DDC Oil 0.010

9 Soda Ash 0.200




13 HCl 0.100

Blue BF


2 Oil HS 0.001

3 H Acid 0.120


5 STA 0.119

6 Antifoam 0.002


8 SPD Oil 0.003

9 DDC Oil 0.010

10 Soda Ash 0.151




14 HCl 0.285

Blue BFN


2 Oil HS 0.002

3 H Acid 0.136

4 MPDSA 0.100

5 Meta Base Ester 0.149

6 STA 0.155

7 Antifoam 0.005


9 SPD Oil 0.004

10 Soda Ash 0.130





33

15 HCl 0.062

Blue 2B


2 Antifoam 0.005


4 Sulpho OAVS 0.453

5 SPD Oil 0.010

6 Soda Ash 0.113




Reactive Golden Yellow

Golden Yellow R

1 MPDSA 0.312


3 Antifoam 0.005

4 SPD oil 0.005



7 HCl 0.103

8 Caustic Lye 0.066


Golden Yellow RNL

1 A. MPDSA 0.238


3 Antifoam 0.004

4 SPD oil 0.004

5 DDC Oil 0.020


7 HCl 0.237

8 Caustic Lye 0.162



Reactive Navy Blue

Navy Blue 2G

1 H Acid 0.196

2 2,5 DMAVS 0.222


4 Antifoam 0.006


6 SPD Oil 0.004

7 DDC Oil 0.020

8 Caustic Lye 0.027

34

9 Sodium Bicarbonate 0.136


11 HCl 0.157


Navy XLE

1 H Acid 0.116

2 Antifoam 0.010


4 MPDSA 0.175


6 Oil HS 0.002

7 Ortho Toluidine Sul. Acid 0.175

8 SPD Oil 0.004

9 Caustic Lye 0.070



12 HCl 0.297

Navy RGB

1 H Acid 0.204


3 Antifoam 0.005


5 SPD Oil 0.004

6 DDC Oil 0.020

7 OAVS 0.234

8 Caustic Lye 0.026



11 HCl 0.179


Disperse Dyes

Azo Dyes

1 Amines 0.250

2 Acid 0.400

3 Ice 2.000


5 Couplers 0.280

6 Alkali 2.150

7 Auxilieries 0.400

Anthraquinones / Condensed Dyes

1 Solvent 2.000

2 Amines 0.250

3 A.Q.R.M 1 0.400

35

4 R.M.2 0.100

5 R.M.3 0.150

6 Auxiliaries 0.400

Cyanation Dyes

1. Solvent 1.500

2. Mono/R.M. Product 0.250

3. Sodium Cyanide 0.200

4. Sodium Bisulphite 0.250

5. Alkali 0.150

6. Wet Cake 1.400

7. D.A Auxiliaries 0.200

Solvent Dyes

Solvent Blue 35

1 Methanol 1.454

2 Quinizarine 0.563

3 Leuco Quinizarine 0.140

4 n-Butyl amine 0.512


6 Water 6.363

Solvent Blue 104

1 ODCB 0.789

2 Quinizarine 0.421


4 Mesidine 0.605

5 Methanol 1.578

6 Water 7.894

Solvent Blue 122

1 Iso propyl alcohol 1.960

2 Quinizarine 0.392


4 P-amino acetanilide 0.637

5 HCl 0.098

6 Water 9.803

Solvent Green 3

1 Butanol 2.474

2 Quinizarine 0.463


4 Para Toluidine 0.567

5 Water 6.597

6 HCl 0.309

Solvent Orange 60

1 o-Xylene 2.666

2 Phthalic Anhydride 0.575

36

3 1:8 Diamino Naphthalene 0.606

4 Methanol 5.296

5 Water 4.545

Solvent Orange 86

1 O-Xylene 2.714

2 Quinizarine 1.071

3 Methanol 0.714

4 Water 6.428

Solvent Red 52

1 o-Xylene 2.234

2 6-Bromo Anthrapyridone 0.978


4 Potassium acetate 0.468

5 Methanol 5.446

6 Water 14.893

7 HCl 0.340

Solvent Red 135

1 o-Xylene 2.080

2 TCPA 0.760

3 1:8 DAN 0.400

4 Methanol 0.480

5 Water 4.800

Solvent Red 168

1 o-Xylene 0.857

2 1-Chloro AQ 0.833

3 Mono cyclohexylamine 0.404


5 Methanol 3.809

6 Water 11.904

Solvent Red 195

1 3 Methoxy Propyl Amine 0.447.76

2 Tri Ethyl Amine 0.125

3 Amogh FP-165 0.395

4 Methanol 0.419

5 HCl 0.559

6 Sulfuric Acid 1.865


8 Acetic acid 1.791

9 Propionic Acid 0.298

10 Diazo component 0.425

11 Ice + Water 45.709

Solvent Red 207

1 o-Xylene 0.976

37

2 1:5 DCAQ 0.725

3 Mono cyclohexylamine 0.627


5 Methanol 5.093

6 Water 11.627

7 Acetic Acid 0.116

Solvent Violet 13

1 Butanol 3.157

2 Quinizarine 0.752



5 Zinc 0.034

6 HCl 0.842

7 Water 15.789

Solvent Violet 14

1 ODCB 0.838

2 1:8 DCAQ 0.645


4 Pot. Acetate 0.709

5 HCl 0.483

6 Water 9.677

7 Methanol 2.580

Solvent Yellow 33

1 ODCB 0.888

2 Phthalic anhydride 0.555

3 Quinaldine 0.555

4 Methanol 2.222

5 Water 6.250

Solvent Yellow 157

1 o-Xylene 2.472

2 Tetra Chloro Phthalic Anhydride 0.727

3 Quinaldine 0.443

4 Methanol 1.818

5 Water 8.181

Solvent Yellow 163

1 n-Butanol 2.946

2 1:8 DCAQ 0.678

3 Potassium Carbonate 0.401

4 Thiophenol 0.535

5 o-Xylene 1.785

6 Water 9.821

Solvent Orange 58

38

1 APMS 0.420

2 HCl 0.466


4 Caustic soda 0.233

5 m-Cl PMP 0.500

6 Chrominating Agent 0.066

7 Water + Ice 50.000

Solvent Red 127

1 Diazo Acid 0.250

2 PMP 0.187

3 Caustic soda 0.150



6 Rhodamine 0.500

7 2-EHA 0.110

8 Water 62.500

Solvent Black 27

1 4 NAP 0.217

2 5 NAP 0.217


4 HCl 0.535

5 Water 0.525

6 B-Naphthol 0.402



9 2-Ethyl Hexyl Amine 0.127


Dyes Intermediates

H Acid

1 Napthelene 0.123

2 Spent Sulphuric Acid 16.800

3 Oleum 0.659

4 Nitric Acid 0.328

5 Caustic Lye 2.511

6 Glaubber Salt 1.159

7 Iron Powder 0.221

8 Soda Ash 0.193


10 Methanol 0.232

J Acid

1 Tobias Acid 0.124

2 Oleum 0.379


39

4 Caustic lye 0.056


6 Nitro, 1-Diazo, 2-Napthol, 4-Sulphonic Acid

1 β-Napthol 0.830

2 Caustic Lye 0.330

3 Sodium Nitrate 0.660


5 Sodium -bi-Sulphite 1.670

6 Oleum-23% 0.830

7 Nitric Acid (70%) 0.420

Vinyl Sulphone

1 Acetanilide 0.630

2 Thionyl Chloride 0.630

3 Caustic Soda Lye 1.060

4 S.B.S 1.380

5 Ethylyn Oxide 0.330


2:5 Dichloro 4 Sulpho Phenyl 3 Methyl 5 Pyrazolone

1 2.5 Dichloro Aniline 0.022

2 Oleum 0.072

3 NaNO2 0.009

4 Soda Ash 0.022

5 SBS 0.031


7 H2SO4 0.036

8 Ester 0.015

9 HCL 0.049

2 Chloro 5 Sulpho Phenyl 3 Methyl 5 Pyrazolone

1 6 Chloro Metanilic Acid 0.031

2 NaNO2 0.011

3 Soda Ash 0.036

4 SBS 0.048

5 Ester 0.017


7 HCL 0.186

1, 3 Sulpho Phenyl 3 Methyl 5 Pyrazolone

1 Metanilic Acid 0.023

2 NaNO2 0.009

3 Soda Ash 0.045

4 SBS 0.035

5 Ester 0.015

6 HCL 0.138

1, 4 Sulpho Phenyl 3 Methyl 5 Pyrazolone

40

1 S . Acid 0.023

2 NaNO2 0.009

3 Soda Ash 0.045

4 SBS 0.035

5 Ester 0.015

6 HCL 0.138

1:3 Phenyl Methyl 5 Pyrazolone

1 Aniline 0.019

2 NaNO2 0.014

3 Soda Ash 0.068

4 SBS 0.051

5 Ester 0.022

6 HCL 0.208

Pigments

Activated CPC Blue

1 CPC Blue Crude 1.000

CPC Blue

1 Phthalic Anhydride 1.075

2 Carbomide salt / NH3 Gas 1.505

3 Cuprous Chloride 0.193

4 Ammonium Molybdate 0.030

5 Dilute H2SO4 (25 to 30%) 2.500

Alpha Blue (15:0 and 15:1)


2 H2SO4 4.810

Pigment Beta Blue (15:3)


2 Dilute HCl 0.013


4 IBA /xylene 0.500

Pigment Beta Blue (15:4)


2 Modified Sulpho 0.067

3 Xylene 0.033

4 HCl 0.117

Copper Phthalocyanine Pigment Green-7

1 Aluminum Chloride 1.825

2 Cupric chloride 0.080


4 MCB 0.060


6 HCl 0.475

7 NaOH 0.155

41

Pigment Violet 23

1 Carbazole 1.100

2 Mono Chloro Benzene 2.000


4 Di Ethyl Sulphate 1.000

5 Dilute Nitric Acid 1.220

6 Ortho Di Chloro Benzene 1.000


8 Benzene Sulphonyl 0.524

9 ODCB 1.200

10 Methanol 1.750

Pigment Red 122

1 Dimethyl Succinylo Succinate 0.400

2 Para Toludine 0.440

3 HCl 0.030

4 Methanol 2.800


6 Phosphoric Acid 1.600

7 Dimethyl Formamide 5.000

Pigment Violet 19

1 Dimethyl Succinylo Succinate 0.400

2 Aniline 0.385

3 HCl 0.030

4 Methanol 2.800



Solsperse 5000

1 Copper Pthalocynine 1.000

2 Oleum 5.000

Carbazole

1 HCl 0.530

2 Aniline 0.385


Speciality Chemicals

2,4-Dichloro Phenyl Acetic Acid

1 2,4-Dichloro Benzyl Chloride 1.230

2 Tri ethyl Amine 0.090


4 Sodium Cyanide 0.315

5 Hydro Chloric Acid (30%) 0.850

6 Toluene 0.150

7 Sodium bi Carbonate 0.090

2,4-DichloroPhenyl Acetyl Chloride

42

1 2,4-Dichloro Phenyl Acetic Acid 1.100


3 Toluene 0.050


2,4,6-Trimethyl Phenyl Acetyl Chloride

1 2,4,6-Trimethyl Phenyl Acetic Acid 1.060

2 Toluene 1.500



2,3,4,5-Tertrachloro Benzoyl Chloride

1 Pthalic Anhydride 0.635

2 OR Tetra Chloro Pthalic Anhydride 1.224

3 Chloro Sulphonic Acid 0.635

4 Chlorine Gas 1.218

5 Ethylene Dichloride 0.635

6 Caustic Soda Flakes 0.178

7 HCL30% 0.165

8 Di Methyl Formamide 2.200


10 Toluene 0.500

3,4,5 Trimethoxy Benzyl Chloride

1 3,4,5-Trimethoxy Benzyl Alcohol 1.000

2 HCL 30% 1.250

Pesticide Intermediates

2-Amino Benzo Nitrile

1 Toluene 0.840

2 PhosphorousPenta chloride 0.026


4 2-Aminobenzamide 0.015

2-Amino-5-Bromo Benzo Nitrile


2 2-Aminobenzonitrile 0.690

3 N-Bromo succinimide 1.035

4 Toluene 1.600

5 Hexane 0.140

2,4,6-Trimethyl Benzaldehyde

1 Mesitylene 3.360

2 Choral 1.134

3 Titanium Tetrachloride 1.460

4 Soda Ash 0.672

5 Acetone 0.160

6 Tetra Ethyl Benzyl Ammonium Chloride 0.010

Indoline

43

1 2-Chloro Phenethyl Amine 1.700

2 Liquid Ammonia 25% 4.800

3 Copper Chloride 0.050

5-(1-Carboxyethyl)-2-(phenylthio) Phenyl Acetic Acid

1 2-Phenylthio-5-propionyl Phenyl Acetic

Acid

1.350

2 Liquid Bromine 0.875

3 Trimethyl Ortho formate 1.150

4 Zinc-Dust 0.060

5 Caustic Soda Flakes 0.175


7 Toluene 0.410

8 Methanol 0.750

9 Ethylene Dichloride 1.500

44

ANNEXURE: 3

BRIEF MANUFACTRING PROCESS, CHEMICAL REACTION AND MASS BALANCE WITH FLOW

DIAGRAM

Acid Dyes:

1. Acid Black 1

Manufacturing Process:

(A) Preparation of PNA Diazo:

1. Make a clear solution of PNA in hydrochloric acid.

2. Cool to 0 C with ice and diazotize it with sodium nitrite.

3. Destroy excess Nirite before first coupling.

4. Make clear solution of H-Acid with soda ash.

5. Above PNA diazo coupled with H-Acid solution at 0 to 5 C, then,

6. This coupled mass is stirred for 3hr.

(B) Preparation of Aniline Diazo:

1. Make Aniline Hydrochloride with hydrochloric acid.

2. Cool to 0 C with ice and diazotize it with sodium nitrite.

3. Destroy excess nitrite before second coupling.

4. This Aniline diazo charge in to first coupled mass.

5. Adjust pH 8.5 – 9.50 with soda ash.

6. Heat to 80 C temp of second coupled mass.

7. Spray dry the reaction mass.

45

02N NH2+ HCl + NaNO 2 N N Cl- 02N

P-Nitroaniline P-Nitrodiazonium Chloride

NH2 + HCl + NaNO 2 N NCl-

Aniline Benzenediazonium Chloride

OH NH2

HO3S SO 3H

C.Lye

NaO3S SO 3Na

OH NH2

OH NH2

NaO3S SO 3Na

N N NO2 + Anilinediazo

NO2N N

SO3H SO 3H

OH NH2

N N

Acid Black - 1

Chemical Reaction:

46

Mass Balance:

Sr. No. Input Qty (Kg) Output Qty (Kg)

1 H-Acid 337.50 Product 1000.00

2 Caustic lye 96.00 Gas / Evaporation 4189.00

3 PNA 150.00


5 Aniline 97.50


7 Water 1100.00

8 Ice 2400.00

9 Soda ash 200.00

TOTAL 5189.00 5189.00

47

2. Acid Black 52:


Preparation of coupling component:-

Charge 6 - Nitro in the MSRL vessel. Add water and ice in it.


Charge B- Napthol in the MSRL vessel with caustic lye.

Coupling:-

Charge 6-Nitro slurry to the B – Napthol slurry. Keeping the temperature between 0 to 5 C by

adding of ice.

Chromination:-

Add Basic Chromium Sulfate and Salicylic acid in coupled mass and heat to 100 C and maintain

the pH 3.0-3.5.

Check the completion of reaction on paper chromatography.

Spray Drying:

Send the total mass for the drying purpose.

48

Chemical Reaction:

49

Mass Balance:


1 6-Nitro 358.00 Product 1000.00

2 Beta Napthol 172.00 Effluent 4581.00

3 NaOH 258.00


5 Steam 1733.00

6 Water 1445.00

7 Ice 1356.00


TOTAL 5581.00 5581.00

50

OH

NH2O2N+ HCl + NaNO2

Diazotisation

5-100CO2N N

OH

N Cl-

5-Nitro 2-Amino Phenol (5NAP) Diazo of 5NAP

OH

Coupling N NO2N

OH OH

Chromination

NO2N N

O2N N N

O

O

OO

Cr+3

Acid Black - 63

3. Acid Black 63:


• Prepare 5-NAP diazo with help of HCL, Sodium nitrite and ice at temp 5-10° C.

• Destroy the excess nitrite by using Salfamic acid.

• Prepare coupler solution (Beta Napthol) in alkaline media at 60° C.

• Add coupler solution to diazo at 8-10° C.

• Stir for overnight.

• Heat to 70° C and add chrom liquid.

• Further heat to 100° C and maintain for 3hr.

• Check the completion of reaction on TLC.

• The above reaction mass is spray dried.

Chemical Reaction:

51

Mass Balance:


1 5-NAP 500.00 Product 1000.00

2 Hydrochloric acid, 30% 1140.00 Gas / Evaporation 7648.00

3 Ice 2000.00




7 Chrome Salam 1500.00

8 Water 2000.00

TOTAL 8648.00 8648.00

52

4. Acid Black 71:


Gamma Acid and J-Acid block solution:

• Prepare Gamma Acid and J-Acid solution in water with Soda ash then block with sodium

bi-sulphite and formaldehyde.

• Stir for 2-3 hr.

Picramic acid diazo:

• Prepare Picramic acid diazo with help of Hydrochloric acid(30%), ice and Sodium Nitrite

solution.

• Keep the temp 5-10 C.

• Destroy the excess nitrite by Sulphamic acid.

Coupling:

• Transfer Picramic Acid diazo to Gamma Acid solution.

• Keep the temp to 10C.

• When coupling is over, stir for overnight.

Chromination:

• Coupled mass is chrominated in presence of Sodium Dichromate and Glucose as a

Oxidizing agent at temp 95-100 C.

• Time depend up on the tone required of the final product.

Drying:

• When the chromination is OK.

• Spray dry the reaction mass.

53

Chemical Reaction:

OH

NH2

SO3H

+ HCHO + NaHSO3H

SO3H

NH.CH2.SO3H

OH

Gamma Acid & J-Acid Mixture Blocked Soln. of Gamma & J-Acid Mixture

OH

NH2

NO2

O2N

+ HCl + NaNO2 Diazotisation

Temp 5-70C

NO2

NO2

N

OH

N Cl-

+

Picramic Acid

Coupling N

OH

N

NO2

NO2 OH

NH.CH2.SO3H

SO3H

Chromination

SO3H

NH.CH2.SO3H

NO2

NO2

N

OH

N

N N

NO2

NO2

NH.CH2.SO3H

SO3H

O O

O OCr+3

Acid Black - 71

54

Mass Balance:


1 Sodium Bi-sulphite 357.00 Product 1000.00

2 Formaldehyde 250.00 Gas / Evaporation 5487.00

3 Gamma Acid 365.00

4 J-Acid 64.00

5 Soda ash 70.00


7 Sodium Dichromate 140.00


9 Sorbitol 60.00




13 Water 2000.00

14 Ice 1500.00

TOTAL 6487.00 6487.00

55

OH

NH2

SO3H

+ Formaldehyde + Sodium Bisulphite

SO3H

NH.CH2.SO3H

OH

Gamma Acid Blocked Gamma Acid (Sulpho methylamino)

HO3S OH

NH2

NO2

+ HCl + NaNO2 Diazotisation

5-100C

NO2

N N Cl-

SO3H OH

4-Nitro-2-Amino Phenol-6-Sulphonic Acid (4NAPSA) 4-NAPSA Diazo

+

SO3H OH

N N

NO2

OH

NH.CH2.SO3H

SO3H

Monoazo

Chromination

SO3H

NH.CH2.SO3H

SO3H

N N

NO2

HO3S

N N

NO2

NH.CH2.SO3H

SO3H

O

O

O O

Cr+3

Acid Black - 84

5. Acid Black 84:


1. Gamma acid: Prepare Gamma acid solution with help of soda ash and blocking take

place by sodium bi-sulphite and formaldehyde.

2. Blocked solution act as a coupler.

3. Prepare diazo of 4-NAPSA: in the presence of 30% Hydrochloric acid and Sodium nitrite.

4. Coupling: Transfer 4-NAPSA diazo to Gamma acid solution in alkali medium. Check

completion of coupling reaction.

5. Chromination of above coupled mass is carried out with chrome solution at temp 90-

100° C and check the completion of metallization.

6. Spray dry the above reaction mass.

Chemical Reaction:

56

Mass Balance:


1 Sodium bi-sulphite 365.00 Product 1000.00

2 Formaldehyde 245.00 Gas / Evaporation 9088.00

3 Gamma acid 473.00

4 4NAPSA 431.00

5 Hydrochloric acid 30% 122.00


7 Soda ash 422.00

8 Ice 4200.00

9 Water 3700.00

TOTAL 10088.00 10088.00

57

6. Acid Black 107


• Prepare Sodium Picramate diazo with HCl, Sodium Nitrite and ice at 0-5 C.

• Stir for 2hr.

• Destroy the excess nitrite by Sulfamic acid solution.

• Prepare Beta Napthol solution in alkaline media at 60 C.

• Transfer Beta Napthol solution to diazo slowly in 30 min keeping temp 5-10 C.

• Stir monoazo reaction mass for 8-10 hr.

• Transfer monoazo reaction mass to asymmetric complexing vessel Step-1.

• Prepare 1:1 chrom complex of 6-NDA+Beta Napthol (Step-2) as couple 6-NDA slurry and

Beta Napthol in alkaline media.

• Above monoazo reaction mass subjected to metallization with chromium formate in

acidic condition.

• Transfer self isolated chrome complex to asymmetric complexing vessel Step-2.

• Mix above step-1 and step-2 and heat to 100 C.

• Check the completion of the reaction by TLC.

• Spray dry the material.

58

NO2 OH

NH2

NO2

+ HCl+NaNO2+Ice

Dioazotization

NO2

N

OHNO2

N.Cl- +

OH

Picramic Acid(4:6 Dinitro-2-Aminophenol)

Beta Naphthol

Coupling

OH

N

NO2 OH

N

NO2

Monoazo

OH

NH2N

NO2

HO3S

OH

+

HO3S

NO2

OH

N N

OH

Chromination

Basic & Acidic 1:1

O

N N

O

Cr+3

1:1 Cr Complex of 6NDA

Beta Naphthol

+ Monoazo

NO2

N

NO2

N

O O

Cr

O O

N N SO3H

NO2Acid Black - 107

Chemical Reaction:

59

Mass Balance:


1 Sodium Picramate 227.00 Product 1000.00

2 Beta Napthol 160.00 Gas / Evaporation 3343.00

3 Hydrochloric Acid 360.00



6 Ice 1000.00

7 6-Nitro 360.00


9 Caustic Lye 22500

10 Chromuim Formate 325.00


12 Oxalic Acid 45.00


14 Water 1150.00

TOTAL 4343.00 4343.00

60

7. Acid Black 172:


Preparation of Diazo component:-

Charge 6 - Nitro in the MSRL vessel. Add water and ice in it.


Charge B- Napthol in the MSRL vessel with caustic lye.

Coupling:-

Charge Beta Napthol slurry to 6-Nitro slurry, Keeping the temperature between 5 to 10 C by

adding of ice.

Chromination:-

Add Basic Chromium Sulfate in monoazo mass and heat to 95 C for the completion of

metallization.

Spray Drying:

Send the above mass for the spray drying purpose.

61

Chemical Reaction:

62

Mass Balance:


1 6-Nitro 446.40 Product 1000.00


3 NaOH 321.00


5 Water 1200.00

6 Ice 1500.00

TOTAL 3878.10 3878.10

63

SO3H NH2

Diazotisation

H2SO4 + NaNO2& Hydrolysis

SO3H OH

+

OH

SO3HH2N

Peri Acid Suetan 1:2:4 Diazo Acid

CouplingN SO3H

OHSO3H OH

N

Monoazo1:1 Chromination inAcidic Medium

N

HO3S O

O

SO3HN

Cr+3

Acid Blue 158

8. Acid Blue 158:


• Naptha sultan is hydrolysed with the help of caustic potash at temp 95-100° C.

• Maintain temp 95-100° C for 6 hr.

• Cool to room tem.

• Charge 1:2:4 Diazo acid at 25-30° C, slowly in 1.5 hr.

• Stir for 6-8 hr and to complete the coupling.

• Adjust pH 8-9 with hydrochloric acid.

• Add chrome liquid which is previously prepared in another vessel.

• Heat to 100° C.

• Maintain temp to 10-12 hr.

• Check reaction mass for the completion of reaction on TLC.

• If TLC is OK, adjust pH 4.5-5.0 with soda ash.

• Sprays dry the above mass.

Chemical Reaction:

64

Mass Balance:


1 Naptha Sultan 489.00 Product 1000.00

2 Caustic potash 555.00 Gas / Evaporation 5562.00


4 1-2-4 Diazo acid 555.00

5 Sodium Bi-chromate 445.00


7 Sorbitol 213.00


9 Ice 1800.00

10 Water 1800.00

11 Soda ash 100.00

TOTAL 6562.00 6562.00

65

9. Acid Brown 75


(A) H-Acid diazo:

1. Make a clear solution of H-Acid with soda.

2. Add sodium Nitrite in the solution and make reverse diazo in Hydrochloric acid and ice.

3. Destroy excess Nitrite before first coupling.

4. Above H-Acid diazo coupled with Resorcenol at pH 12-13 with caustic lye.

5. This coupled mass is stirred for 3hr.

(B) Preparation of Sodium Picramate diazo:

6. Make Sodium Picramate Hydrochloride with hydrochloric acid.

7. Cool to 0C with ice and diazotized it with Sodium nitrite.

8. Destroy excess Nitrite before second coupling.

9. This Picramate diazo charge in to first coupled mass.

10. Adjust pH 8.9 with caustic lye.

(C) Preparation of PNA diazo:

11. Make a clear solution of PNA in Hydrochloric acid.

12. Diazotized it with sodium nitritebefore third coupling, destroy excess Nitrite.

13. After completion of third coupling, spray dry the reaction mass.

Mass Balance:


1 H-Acid 240.00 Product 1000.00

2 Soda ash 50.00 Gas / Evaporation 5773.00



5 Resorcinol 84.00



8 PNA 125.00

9 Water 1150.00

10 Ice 3000.00

TOTAL 6773.00 6773.00

66

10. Acid Brown 161


Anthranilic acid:

• First Anthranilic acid has been made solution in 98% Sulphuric acid, in continuous

stirring.

• Block with Formaldehyde and maintain for 3-4 hr.

• Then make tetrazo of Anthranilic acid with help of Sodium Nitrite in presence of ice to

maintain temp of tetrazo.

• Further tetrazo coupled with Resorcinol solution, which is cleared in water and also with

caustic lye in alkaline medium.

• When coupling is OK.

• Add couple mass diazo of 2.4 Sulfanilic acid which is made by help of Hydrochloric acid,

Sodium nitrite and ice.

• After then metallization with copper sulphate.

• The above reaction mass is then spray dried.

67

NH2

COOH

Condensation

HCHO/H2SO4

C OOH

H2N CH2

OHC O

NH2Tetrazotisation

2

OH

OH

Coupling

Resorcinol

OH

OH

N N

O

COH

CH2

OHOC

N N

OH

OH

2

NH2

SO3H

HCl + NaNO2

Diazotisation

SO3H

N N Cl

OH

OH

N N

C OOH

CH2

OHC

O

NN

OH

OH

N

N

SO3H

Metall izationCuSO4.5H2O

SO3H

N

N

N

N

SO3HSO3H

N

N

OH

O

N N

O

COH

CH2

OOC

N N

OH

OH

Cu

Acid Brown - 161

Chemical Reaction:

68

Mass Balance:


1 Anthranilic acid 154.50 Product 1000.00

2 Sulphuric acid, 98% 140.08 Gas / Evaporation 7102.96



5 Resorcinol 120.00




9 CuSO4. 5H2O 284.00

10 Water 2450.00

11 Ice 3900.00

TOTAL 8102.96 8102.96

69

11. Acid Brown 165:


H-Acid diazo:

• Prepare H-Acid diazo with help of caustic lye, Hydrochloric acid, ice and Sodium Nitrite

solutions, keeping the temp 5-10 C.

Picramic acid diazo:

• Picramic acid diazo with help of Hydrochloric acid and Sodium Nitritesolution, ice and

maintain the temp to 5-7 C.

PNA diazo:

• PNA diazo prepare in Hydrochloric acid, ice and Sodium Nitrite solution keeping temp 5-

10 C.

Coupler solution:

• Prepare Resorcinol solution in water and stir to get clear solution.

• Add ice to get temp 0 C, then transfer H-Acid diazo.

• Stir for 2hr.

• Then add Picramic acid diazo and PNA diazo gradually.

• First couple mass maintaining pH alkaline by using caustic lye and temp 10 C.

• When coupling is over, heat to 80-90 C.

Metalization:

• Metalize the coupled mass with Ferric chloride, when test and tone is OK.

Drying:

• Spray dry the above mass.

70

OH NH2

SO3H SO3H

Diazotisation

HCl + NaNO2 Ice

SO3H SO3H

OH N N Cl

+

OH

OH

H-Acid

1st Coupling

SO3H

OH

HO3S

N N

OH

OH

N

N

OH

NO2NO2

2nd Coupling

OH

NO2

NO2

H2N

Picramic Acid

NH2

NO2

HCl + NaNO2 Ice

Diazotisation

+

Cl NN

NO2

3rd Coupling

NO2NO2

OH

N

N

OH

OH

NN

OH

SO3H

SO3H

N N NO2

Metall izationFeCl3

80-85OC

NO2 NN

SO3H

SO3H

O

N N

O

OH

N

N

OH

NO2NO2

Fe

Acid Brown 165

Chemical Reaction:

71

Mass Balance:


1 H-Acid 76.00 Product 1000.00

2 Caustic lye, 48% 200.00 Gas / Evaporation 6539.20



5 Resorcinol 70.00


7 Paranitro Aniline 112.00

8 Water 2350.00

9 Ice 3200.00

10 Ferric chloride 261.00

TOTAL 7539.20 7539.20

72

12. Acid Brown 355:


• Prepare 4-NAPSA diazo with the help of hydrochloric acid and sodium nitrite in presence

of ice at 5-10 C.

• Prepare PMP coupler solution with caustic lye and cool to 10 C with ice.

• Add coupler to diazo mass at temp 5-10 C.

• Stir for overnight to complete the coupling.

• Charge 1:1 chrom complex of 6-Nitro+Beta and heat to 95-100 C.

• Maintain temp till it is OK.

• Adjust qty of chrome complex according to monoazo of 4NAPSA to PMP.


Chemical Reaction:

OH

NH2

NO2

SO3HDiazotisation

HCl + NaNO2

SO3H OH

N=N-Cl

NO2

+

CH3

O

NO2 N=N

OH

SO3H

NN

NN

OH

CH3

Orange Monoazo

Coupling

Diazo 4 NAPSA 1-Phenyl 3-Methyl5-Pyragolone

4-Nitro 2-aquizoPhenyl 6-Sulphonic Acid

NO2

SO3H

OH

N=N +

OH

Coupling

NO2

SO3H

OH

N=N

OH

N=N

O

NO2

SO3H

Chlorination

O

Cr

6 Nitro 1:2:4Diazo Acid

B NaphtholMonoazo

Cr

O

SO3H

NO2

O

N=N

+

NO2

SO3H OH

N=N

NN

O

CH3

N=N

O

NO2

SO3H

O

Cr

OO

N

N

CN=N

SO3H

NO2. 3 Na +

Acid Brow n 355

73

Mass Balance:


1 4-NAPSA 276.00 Product 1000.00

2 PMP 219.00 Effluent 3726.00

3 Hydrochloric acid, 30% 520.00 Water Losses 1924.00




7 6-Nitro-1-Diazo acid 311.00


9 BCS, 16% 362.00



12 Water 2915.00

13 Ice 1244.00

TOTAL 6650.00 6650.00

74

13. Acid Brown 425:


• Make a Anthranilic acid diazo with Hydrochloric acid and sodium nitrite in the presence

of ice.

• Destroy the excess nitrite by Sulfamic acid.

• Dissolve Resorcinol in water, Soda and ice.

• Transfer diazo to Reesorcinol, alkaline solution.

• This first coupled mass, further couple with OT 5SA diazo.

• Prepared OT 5SA diazo with hydrochloric acid, sodium nitirte and ice.

• Destroy the excess nitrite by sulfamic acid.

• Transfer in to first coupled mass.

• Stir over night.

• Coupled mass then chrominated with Chromium Fluoride at 95-100 C.


Chemical Reaction:

NH2

C=OH

O

+ HCl + NaNO2N=N-Cl

C-OH

O

+

OH

OH

Anthranilic Acid

NH2

SO3H

Cl-N=N

CH3

SO3H

OH

OH

N=N

O

C-OH

Anthranilic Acid Diazo Resorcinal Monoazo

C-OH

N=N

OH

OH

O

N

N

CH3NaNO2

HCl

CH3

SO3H

O.T. 5 S.A O.T. 5 S.A Diazo

SO3H

CH3

N=N

OH N=N

C

O

Cr

O

O

O

3+

O

C

O

N=N OH

N

SO3H

CH3

Acid Brown 425

Chlorination

75

Mass Balance:



2 O.T.5 SA 250.00 Gas / Evaporation 5051.00



5 Resorcinol 150.00

6 Soda ash 350.00





11 Ice 2000.00

12 Water 1800.00

TOTAL 6051.00 6051.00

76

14. Acid Brown 432


• Make Anthranilic acid diazo with HCl, Sodioum nitrite and ice at temp 5-10 C.

• Remove excess nitrite with sulfamic acid.

• Dissolve Resorcenol in water, ice and Soda ash.

• Transfer diazo to Resorcinol solution in alkaline media.

• This first coupled mass is further coupled with Lorrent Acid diazo.

• Prepare Lorrent Acid diazo with HCl, Sodium nitrite and ice at 5-7 C.

• Remove excess nitrite with sulfamic acid and then coupled with first coupled mass.


• Coupled mass is chrominated with Chromium Fluoride at 95-100 C.

• Spray dry the above chrominated mass.

Chemical Reaction:

NH2

COOH

+ HCl + NaNO2

N=N-Cl

C=O

OH

+

OH

OH

Anthranilic Acid Resorcinol

C-OH

O

N=N

OH

OH

NH2

SO3H

NaNO2

HCl

Cl-N=N

SO3H

OH

OH

N=N

O

C-OH

N

N

SO3H

N=N

C

O O

OH

O

Cr

OO

OH

N

N

N=N

C

O

Acid Brown 432

Chlorination

77

Mass Balance:



2 Resorcenol 150.00 Gas / Evaporation 6151.00

3 Lorrent acid 285.00



6 Soda ash 350.00


8 Caustic soda Flakes 57.00



11 Ice 2300.00

12 Water 2300.00

TOTAL 7151.00 7151.00

78

15. Acid Brown 434


• Make Anthranilic acid diazo with HCl, Sodioum nitrite and ice at temp 5-10 C.

• Remove excess nitrite with sulfamic acid.

• Dissolve Resorcenol in water, ice and Soda ash.

• Transfer diazo to Resorcinol solution in alkaline media.

• This first coupled mass is further coupled with Lorrent Acid diazo.

• Prepare Lorrent Acid diazo with HCl, Sodium nitrite and ice at 5-7 C.

• Remove excess nitrite with sulfamic acid and then coupled with first coupled mass.


• Coupled mass is chrominated with Chromium Fluoride at 95-100 C.

• Isolate the product with salt.

• Filter the isolated mass in filter press.

• Collect the wet cake and dry.

Chemical Reaction:

OHNO2

NO2

NH2 + HCl + NaNO2 + Ice

Diazotisation

NO2 OH

N=N-Cl

NO2

+

OH

OH

Picraunic Acid(4:6 Dinitro 2-anino Phenol)

Diazo of Picraunic Acid Resorcinol

NO2 OH

N=N

NO2

OH

OH

Diazotisation

HCl + NaNO2

NH2

SO3H

1st Coupling

2nd Coupling

Monoazo 1:1 Cleve's Acid

NO2

N=N

NO2 OH OH

OH

N

N

SO3H

Metallization

O

OH

NN

O

Fe 3 +

NO2

NO2

N

N

SO3H

Acid Brow n 432

79

Mass Balance:


1 Sodium Picrame 296.00 Product 1000.00

2 Resorcinol 145.00 Gas / Evaporation 6303.00

3 Mix cleave acid 336.00



6 Sulfamic acid 2.00


8 Caustic lye 189.00

9 Ferrous sulphate 260.00

10 Water 1800.00

11 Ice 3000.00

TOTAL 7303.00 7303.00

80

16. Acid Green 104


• Prepare diazo of Sodium Picramate with the help of Hydrochloric acid, Sodium Nitrite

and ice.

• Before coupling destroy the excess nitrite by sulfamic acid.

• Sodium Picramate diazo coupled in alkaline medium with (Oxy Larrent acid) Dahl’s acid.

• When coupling is over confirmed the test.

• Metallized the coupled mass with cobalt sulphate.

• Spray dry the above reaction mass.

Chemical Reaction:

NO2 OH

NH2

NO2

Diazotisation

5-7 CHCl + NaNO2

NO2 OH

N=N-Cl

NO2

+

NH2

SO3H

NO2 OH

N=N

NO2

NH2

SO3H

Picranic Acid Diazo of Picranic Acid 2-Amino-5-Naphthalene (4:6 Dinitro Sulphonic Acid2-Amino Phenol)

Coupling

NO2

NO2O

N=N

SO3H

NH

CO

NH O

SO3H

N=N

NO2

NO2

Acid Green 104

81

Mass Balance:


1 Sodium Picramate 405.00 Product 1000.00

2 Dahl's Acid 419.00 Gas / Evaporation 7723.00



5 Ice 3350.00



8 Water 3250.00

TOTAL 8723.00 8723.00

82

17. Acid Orange 74


• Prepare 4-NAPSA diazo with HCL, Sodium nitrite and ice.

• Destroy the excess nitrite by sulfamic acid.

• Prepare PMP solution in alkaline media and add sodium acetate.

• Add coupler solution to diazo slowly in 1hr.


• Heat to 70 C and add Salicylic acid followed by BCS powder.

• Prepare chrome complex at 100 C in acidic condition.

• Cool to room temp and adjust pH to 7.5 to 8.0.


Chemical Reaction:

NO2

NH2

OHSO3H

+ HCl + NaNO2

NO2

N=N-Cl

OHSO3H

+ N

NO

CH3

+ NaOH

CH3

NN

OH

+ 4 NAPSA Diazo

4-Nitro 2-Amino Phenol6-Sulphonic Acid

1-Phenyl 3-Methyl 5-Pyrazolone

NO2

SO3H

N=N

O

NN

O

Cr

H2O H2O H2O

CH3

Acid Orange 74

83

Mass Balance:


1 4-NAPSA 530.00 Product 1000.00



4 PMP 425.00



7 Ice 2500.00


9 BCS, 16% 900.00

10 Water 2200.00

TOTAL 8143.00 8143.00

84

18. Acid Orange 142


• Prepare 4-NAPSA diazo with HCL, Sodium nitrite and ice at 5-10° C.

• Destroy the excess nitrite by using sulfamic acid.

• Prepare coupler solution (PMP) in alkaline media.

• Make buffer with sodium acetate.

• Cool to 10° C with ice.

• Add coupler solution to diazo slowly in 1hr.

• Stir for overnight.

• Heat to 70° C and add chrom liquid.

• Further heat to 100° C.

• Maintain temp for 2hr.

• Check the completion of reaction on TLC.


Chemical Reaction:

SO3H OH

NH2

NO2

+ HCl + NaNO2

NO2

OHSO3H

N=N-Cl NN

CH3

O

+ NaOH

CH3N

NOH

4-Nitro 2-Amino Phenol6-Sulphonic Acid(4 NAPSA)

1-Phenyl 3-Methyl 5-Pyrazolone

NO2

N=N

SO3H OH

NN

CH3

O

+ Salicylic Acid & Green Solution

N=N

NO2

SO3H O O

NN

CH3

Cr

O OSO3H

NN

NO2

NN

CH3

Acid Orange 142

85

Mass Balance:


1 Water 1980.00 Product 1000.00

2 Ice 2750.00 Gas / Evaporation 5196.59

3 4NAPSA 363.60




7 PMP 290.90



10 Sodium dichromate 136.35

11 Sorbitol 65.00



TOTAL 6196.59 6196.59

86

19. Acid Red 97


1. Tetrazo of BDSA prepared in presence of Hydrochloric acid, Sodium nitrite and Ice.

2. Coupling component: Dissolve Beta Napthol in water and caustic flakes to get clear

solution.

3. Coupling: Transfer tetrazo to Beta Napthol solution in alkaline medium, stir overnight.

4. Next day spray dry the above reaction mass.

Chemical Reaction:

NH2

SO3H

NH2

SO3H

HCl + NaNO2

Cl.N=N

SO3H

SO3H

N=N-Cl +

OH

Coupling

N=N

OH

SO3H

SO3H

N=N

OH

Acid Red 97

Mass Balance:


1 BDSA 455.00 Product 1000.00





6 Water 2625.00

7 Ice 1500.00

TOTAL 6490.00 6490.00

87

20. Acid Red 357


• Prepare 6NAPSA diazo with Sodium nitrite and ice.

• Prepare PMP solution in alkaline media and buffered with sodium acetate.

• Add coupler solution to diazo slowly in 1 hr.

• Stir for 8-10 hr to complete the coupling.

• Add Green solution and further heat to 100 C.

• Maintain temp for 2-3 hr, check completion of metallization on TLC.

• SPD the material.

Chemical Reaction:

NO2 OH

NH2

SO3H

NaNO2

Diazotisation

NO2 OH

N=N-Cl

SO3H

+ N

NO

CH3Coupling

SO3H

N=N

OHNO2

NN

OH

CH3Chlorination

NO2

N=N

SO3H

O

NN

CH3

O

Cr

OO

NN

N=NCH3

SO3H

NO2

Ph

Acid Red 357

88

Mass Balance:


1 6NAPSA 358.00 Product 1000.00

2 Sodium Nitrite 109.25 Gas / Evaporation 4183.76

3 PMP 280.59



6 Green solution 450.00

7 Water 2350.00

8 Ice 1200.00


TOTAL 5183.76 5183.76

89

21. Acid Violet 90


• Prepare solution of PMP in water with help of caustic lye to get clear solution.

• Charge Ammonium Sulphate followed by addition of 1-2-4 Diazo acid 300 kg.

• After that Chrominated with BCS at 90-100 C.


Chemical Reaction:

OH

N=NaSO3H

Coupling NN

CH3

O+

OH

N=NSO3H

NN

CH3

OH

Ph

Chlorination

1:2:4 Diazo Acid 1-Phenyl 3-Methyl Pyrazolone Monoazo

N=N

NN

CH3SO3H

O O

Cr

O O

NN

CH3

Ph

SO3HN=N

Acid Violet 90

90

Mass Balance:


1 1-2-4 Diazo acid 400.00 Product 1000.00

2 PMP 304.00 Gas / Evaporation 3647.00



5 BCS, 16% 266.00


7 Water 3200.00

TOTAL 4647.00 4647.00

91

22. Acid Yellow 42


1. Prepare Tetrazo of BDSA in presence of Hydrochloic acid, Sodium Nitrite and Ice.

2. Dissolve PMP in water in presence of caustic flakes to to get clear solution and add

Sodium Acetate.

3. Transfer tetrazo to coupler.

4. Stir over-night.

5. Check completion of coupling reaction.


Chemical Reaction:

NH2

SO3H

NH2

SO3H

HCl + NaNO2

Cl-N=N

SO3H

SO3H

N=N-Cl

O

CH3

NN N

N

CH3 N=N

SO3H

N=N

SO3H

NN

CH3

OO

Acid Yellow 42

92

Mass Balance:


1 BDSA 360.00 Product 1000.00






7 Water 2300.00

8 Ice 4750.00

TOTAL 9710.00 9710.00

93

23. Acid Yellow 59


• Prepare Anthranilic acid diazo with help of Hydrochloric acid, sodium nitrite and ice.

• Destroy the excess nitrite by sulphamic acid.

• Prepare PMP solution in alkaline medium and add sodium acetate.

• Add diazo solution to coupler solution in course of an hour.

• The dye further metallized with BCS.

• Check the completion of metallization.

• Neutralize reaction mixture with caustic lye.

• Cool to 50º C and dispersing agent AB-300.


Chemical Reaction:

NH2

C=O

OH

HCl + NaNO2 N=N-Cl

C=O

OH

+ NN

CH3

O

N=N

NN

CH3

OHC

O OH

Anthranilic Acid Diazo of Anthranilic Acid 1-Phenyl 3-Methyl Pyrazolone

Monoazo

Chlorination

N=N

NN

CO

OO

Cr

ON

N

CH3 N=N

O

C=O

Acid Yellow 59

94

Mass Balance:




3 BCS, 16% Cr. 208.00

4 Formic acid, 85% 450.00

5 Ice 1500.00




9 Water 1050.00

10 Dispersing agent 600.00

TOTAL 5030.00 5030.00

95

24. Acid Yellow 194

Process Description:

4-NAPSA diazo:

• Prepare 4-NAPSA diazo with help of Hydrochloric acid and sodium nitrite in presence of

ice to maintain temp.

AAA Coupler solution:

• Make clear solution of AAA with help of caustic lye.

• 4-NAPSA diazo coupled with AAA in alkaline medium and then metallization with cobalt

sulphate at 80-90 C for 3-4 hr.

• When test is OK.


Chemical Reaction:

OHSO3H

NH2

NO2

HCl + NaNO2OHSO3H

N=N-Cl

NO2

+ Aceto AcetanilideOH SO3H

NO2

N=NCH

C

O

NH Ph

C

O

CH3

+ Cobalt Sulphate CoSO4.7H2O

NO2

SO3HO

N=NCH

C

O

-Ph HN

C

CH3 O

Co

OSO3H

NO2

N=N HC C

C

O

- CH3

O

NHPh

Acid Yellow 194

96

Mass Balance:


1 4NAPSA 476.00 Product 1000.00

2 AAA 381.00 Gas / Evaporation 6366.00





7 Ice 2600.00

8 Water 2600.00

TOTAL 7366.00 7366.00

97

Direct Dyes:

1. Direct Black 40


PAA Diazo:

• Prepare PAA diazo with help of Hydrochloric acid (30%) and Sodium Nitrite in presence

of ice.

• Couple this diazo to clear solution of Gamma Acid in alkaline medium.

• When coupling is over, and test is OK.

• Heat the first coupled mass to 90-100° C, in presence of caustic flakes for 4-5 hr for

hydrolysis, when OK.

• Cool to room temp.

• Further hydrolysis the mass acidify and make diazo with help of Hydrochloric acid, 30%,

ice and Sodium Nitrite.

• When diazo is OK, stir for 3-4 hr.

• Destroy the excess nitrite by Sulfamic acid.

• Then couple with Mix cleave acid in mild alkaline medium and then with final coupling

with Gamma acid in alkaline medium.

• Presipitated product is then spray dried.

98

Chemical Reaction:

NH2CH3.C.HN

O

+ HCl + NaNO2

O

CH3.C.HN N=N.Cl Coupling

NH2

SO3H

OH

P-Amino Acetanilide P-Acetanilide Diazonium Chloride Gamma Acid

CH3.C.HN

O

N=N

SO3H

OH

NH2

SO3H

NH3

OH

N

NH2

N=

Hydrolysis

Caustic Lye

SO3H

NH2

&

OH

NH2

SO3H

Mix Clever Acid Complex I

Gamma Acid Complex II

N

N

NH2

N=N

OH

SO3H

SO3H

Direct Black 40

N=N

OH

NH2

SO3H

Tetrazotisation

HCl + NaNO2

Monoazo

99

Mass Balance:


1 PAA 150.00 Product 1000.00

2 Gamma acid 465.00 Gas / Evaporation 9705.00

3 Mix Cleave acid 223.00



6 Caustic lye 263.00

7 Soda ash 475.00



10 Water 2050.00

11 Ice 4000.00

TOTAL 10705.00 10705.00

100

2. Direct Black 168


• Prepare FC Acid tetrazo with help of Hydrochloric acid, sodium nitrite and ice.

• FC Acid tetrazo coupled with H-Acid solution in acidic medium.

• Stirred over night.

• Further coupled with Aniline diazo in alkaline medium and subsequently final coupling

with MPD in mild alkaline medium.

• When coupling is confirmed OK.

• Then Spray dry the reaction mass.

Chemical Reaction:

SO3H

NHNH2 NH2

N=N-Cl N=N-Cl

HCl + NaNO2

Tetrazotisation

NH2 OH

Soda

pH 6.5-7.0

NH2 OH

SO3NaSO3NaSO3H SO3H

H - Acid

+ Tetrazo of F.C. Acid

OH NH2

SO3H SO3H

N=N NH N=N-Cl + NH2 + HCl + NaNO2 N=N Cl

Aniline

N=N

OH NH2

SO3H SO3H

N=N

SO3H

NH N=N-Cl +

NH2

NH2/OH

NH2

NHN=N

SO3H SO3H

OH NH2

N=N N=N

OH/NH2

Direct Black 168

101

Mass Balance:


1 FC Acid 307.00 Product 1000.00

2 H-Acid 307.00 Gas / Evaporation 7171.00



5 Aniline Oil 93.00

6 Soda ash 561.00

7 MPD 114.00

8 Ice 3700.00

9 Water 1900.00

TOTAL 8171.00 8171.00

102

3. Direct Blue 71


C-Acid diazo solution:

• Prepare diazo of C-Acid with help of Hydrochloric acid (30%) and Sodium Nitrite solution

in presence of ice.

αNapthylamine solution:

• Prepare αNapthylamine clear solution by heating with Hydrochloric acid (30%) and

water.

• Clear pinkish solution.

First coupling:

• Transfer αNapthylamine solution to C-Acid diazo keeping temp to 10° C under

continuous stirring.

Monoazo diazo:

• Prepare diazo of first coupled mass with help of Sodium nitrite and ice.

• When diazo is ready.

• Add to Mix cleave acid clear solution.

• When coupling is over, make disazo of aforesaid coupling mass with help of

Hydrochloric acid, ice and Sodium Nitrite.

J-Acid solution:

• Prepare J-Acid solution in water, ice and caustic lye.

• Transfer disazo to J-Acid solution in alkali condition.

• Check the completion of reaction.

Drying:


103

Chemical Reaction:

SO3H

NH2 SO3H

+ HCl + NaNO2

SO3H

SO3HN=N-Cl

NH2

SO3H

SO3HN

N

NH2

HCl + NaNO2

C-Acid C-Acid Diazonium Chloride Naphthylamine

Monoazo

SO3H

SO3HN

N

N=N-Cl

+ SO3H

NH2

N

N

SO3H

SO3H

N

N

SO3HNH2 Direct Blue 71

Mass Balance:


1 C-Acid 336.00 Product 1000.00

2 Napthyl Amine 170.00 Gas / Evaporation 7171.00

3 Mix Cleave Acid 220.00



6 J-Acid 260.00

7 Caustic soda lye, 48% 50.00


9 Water 2600.00

10 Ice 3900.00

TOTAL 8936.00 8936.00

104

4. Direct Green 26


• BHK acid is diazotized with help of Hydrochloric acid, sodium nitrite in presence of

ice.

• The above mass is coupled with H-Acid in alkaline medium.

• Then the dye is isolated, dissolved in water.

• The above is then condensed with cyanuric chloride.

• The remaining two halogen atoms of the cyanuric chloride moles are substituted by

condensation with p-Amino Phenyl azo salicylic acid and Anilin Oil respectively.

• The resultant reaction mass is then spray dried.

Chemical Reaction:

N=NOSO2

SO3H SO3H

CH3

OCH3

NH2

PhO2S O N=N

SO3H SO3H

OCH3

CH3

BHK Acid Monoazo Diazo of BHK Acid

+

OH NH2

SO3H SO3H

H - Acid

CH3

PhO2S O N=N

OCH3

N=N

OH NH2

SO3H SO3H

+

C

N N

C C-Cl

N

Cl

Diazo BHK H Acid Cyanuric Chloride

CH3

OCH3

SO3H SO3H

PhO2S O N=N N=N

SO3H SO3H

OH NH

1 st

Condensation

2 nd

Condensation

PAPAS

NH2 N=N OH

C=O

OHPAPAS

Condensation

3 rd

Aniline

NH2

Aniline

Hydrolysis

NaOH

105

OH N=N

SO3H SO3H

CH3

O CH3

N=N

OH NH

SO3H SO3H

CN C

N C

N

NH Aniline

NH N=N OH

C=O

OH

Direct Green 26

Mass Balance:


1 BHK Acid 434.00 Product 1000.00

2 H-Acid 234.00 Gas / Evaporation 7719.00




6 Soda ash 177.00

7 PAPA's acid 154.00

8 Cyanuric chloride 110.00

9 Reaction oil 15.00

10 Aniline Oil 86.00

11 Ice 2900.00

12 Water 3600.00

TOTAL 8719.00 8719.00

106

5. Direct Orange 15


• Prepare FC Acid tetrazo with help of Hydrochloric acid, sodium nitrite and ice.

• FC Acid tetrazo coupled with H-Acid solution in acidic medium.

• Stirred over night.

• Further coupled with Aniline diazo in alkaline medium and subsequently final coupling

with MPD in mild alkaline medium.

• When coupling is confirmed OK.

• Then Spray dry the reaction mass.

Chemical Reaction:

CH3

SO3H

NO2

Condensation

In presenceof caustic soda

CH=CHNO2

SO3H

NO2

SO3H

n

Condensed product of 2-Phenyl 5-Nitro benzeneSulphonic Acid

Reaction withHCHO reduction

N=N CH=CH

SO3H

N=N

SO3H

CH=CH

SO3H SO3H

N=N

n

Direct Orange 15

107

Mass Balance:


1 PNTOSA 818.00 Product 1000.00

2 Caustic Flakes 750.00 Gas / Evaporation 5743.00


4 Dichlone 25.00

5 Spent Acid, 50% 1800.00

6 Ice 1000.00

7 Water 1500.00

Total 6743.00 6743.00

108

6. Direct Orange 118


1. Diazotization of p-Cresidine-o-Sulphonic acid: p-Cresidine-o-Sulphonic acid is diazotized

in presence of Hydrochloric acid and Sodium Nitrite.

2. Just before coupling make CR and SI –ve with sodium bi-carbonate.

3. Coupler solution: Take water and add J-Acid Urea and make uniform solution.

4. Add Sodium bi-carbonate.

5. Receive above diazo mass in course of 45 min.

6. Stir overnight.

7. Heat to 80° C.

8. Stir for 2hr.


109

Chemical Reaction:

Me NH2

OMeSO3H

+ HCl + NaNO2

Me N=N-Cl

OMeSO3H

P-Cresidine O-Sulphonic Acid P-Cresidine O-Sulphonic Diazonium Chloride

OH

SO3H

NH-C-NH

O OH

SO3H

+ NaHCO3

J Acid Urea

OH

SO3Na

NH-C-NH

O

OH

SO3Na

+ 2 Cl-N=NMe

SO3HOMe

J Acid Urea Disodium Salt

Me

N=N

OMe SO3H SO3H

OH

NH-C-NH

O

OH

SO3

N=N

OMe SO3H

Me

Direct Orange 118

110

Mass Balance:


1 p-Cresidine-o-Sulphonic acid 231.00 Product 1000.00




5 J-Acid Urea 315.00

6 Water 3000.00

7 Ice 3500.00

TOTAL 7958.00 7958.00

111

7. Direct Red 81


1. Prepare clear solution of J-Acid.

2. Benzolyte with Benzoylchloride at 18-20 °C.

3. Check completion of Benzoylation.

4. Prepare reverse Diazo of p-Aminoazobenzene-4-Sulphonic acid with help of caustic lye,

hydrochloric acid, ice and sodium nitrite.

5. Add Diazo mass to coupler solution.

6. Stir for 2 hr till coupling is completed.


Chemical Reaction:

SO3H N=N NH2 + HCl + NaNO2 N=NSO3H N=N Cl

4 4' p-Amino Azo Benzene Sulphonic Acid

OH

SO3H NH2

+ C-Cl

O

J Acid Benzoyl Chloride

OH

SO3H

NH-C

O + SO3H N=N N=N-Cl

Benzoylated J Acid

N=NSO3H N=N

OH

SO3H NH-C

O

Direct Red 81

112

Mass Balance:


1 PAABSA 308.00 Product 1000.00

2 Caustic lye, 48% 210.00 Gas / Evaporation 5923.00



5 J-Acid 279.00

6 Benzoyl Chloride 257.00



9 Soda ash 62.00

10 Water 2800.00

11 Ice 2000.00

TOTAL 6923.00 6923.00

113

8. Direct Red 239


Bronner’s Acid:

• Make clear solution of bronner’s Acid with caustic lye.

• Add Sodium Nitrite in the solution and make reverse diazo in Hydrochloric acid and ice

to maintain diazo at temp 5-7° C.

Coupler solution:

• Prepare J-Acid Urea solution in water, stir to form good slurry.

• Transfer diazo to coupler solution in alkali medium.

• When coupler is over, stir over night.

Drying:


Chemical Reaction:

NH2

SO3H

2 + NaNO2 + HCl

N=N-Cl

SO3H

2

Bronner's Acid

SO3H

N=N

OH

SO3H

NH-C-NH

O

OH

N=N

SO3H SO3H

Direct Red 239

114

Mass Balance:


1 Browner's acid 250.00 Product 1000.00

2 caustic lye, 48% 100.00 Gas / Evaporation 6637.50



5 J-Acid Urea 292.50

6 Soda bi-carb, 25% 250.00

7 Soda ash, 20% solu. 100.00

8 Water 2500.00

9 Ice 3500.00

TOTAL 7637.50 7637.50

115

9. Direct Red 254


PAABSA solution:

• Prepare solution of PAABSA by caustic lye.

• Stir and add Sodium Nitrite in the solution and make reverse diazo in Hydrochloric acid

and ice.

• Just before coupling destroy excess nitrite by sulfamic acid.

Coupler solution:

• Prepare J-Acid solution with help of caustic soda lye.

• Transfer the diazo to coupler solution in alkali medium.

• When coupling is over, heat the coupling mass.

Drying:


Chemical Reaction:

SO3H N=N NH2 + HCl + NaNO2

P-Aminoazo Benzene 4-Sulphonic Acid

SO3H N=N N=N-Cl

P-Aminoazo Benzene 4-Sulphonic Acid

+

SO3H

NH2

OH

J Acid

SO3H N=N N=N

OH

NH2

SO3H

Direct Red 254

116

Mass Balance:


1 PAABSA 406.25 Product 1000.00

2 Caustic lye 200.00 Gas / Evaporation 8633.85



5 J-Acid 351.60

6 Soda ash 300.00

7 Water 2700.00

8 Ice 4700.00

TOTAL 9633.85 9633.85

117

10. Direct Violet 9


Sulfanilic acid diazo:

• Prepare diazo of sulfanilic acid in presence of Hydrochloric acid, Sodium Nitrite and ice.

p-Cresidine solution:

• Prepare solution of p-Cresidine in water.

• Couple with Sulfanilic acid diazo.

• Stir continuously.

• When coupling is over make monoazo diazo by adding Hydrochloric acid and Sodium

Nitrite solution in presence of ice.

• Stir monoazo diazo for 4-5 hr to consume sodium nitrite.

• After that destroy excess nitrite by adding sulfamic acid.

• Final coupling will take place with n-Phenyl J-Acid in alkaline medium.

• After completion of coupling, heat to 70° C.


Chemical Reaction:

SO3H NH2 + NaNO2 + HCl SO3H N=N-Cl + CH3

Me

NH2

OCH3(OMe)

P-Cresidine

Sulphanilic Acid

SO3H N=N

Me

NH2

OMe

Monoazo

HCl + NaNO2

N=NSO3H

Me

N=N Cl

OMe

Monoazo Diazo

+

Ph NH2 SO3H

OH N-Phenyl J Acid

SO3H N=N

Me

N=N

OMe SO3H

NH-Ph

OH

Direct Violet 9

118

Mass Balance:


1 Sulphanilic acid 180.00 Product 1000.00

2 p-Cresidine 150.00 Gas / Evaporation 6975.00

3 n-Phenyl J Acid 327.00





8 Soda ash 175.00

9 Ice 3800.00

10 Water 1900.00

TOTAL 7975.00 7975.00

119

11. Direct Violet 35


C-Acid diazo:

• Prepare diazo of C-Acid in presence of Hydrochloric acid (30%) Sodium Nitrite and ice.

P-Cresidine:

• Make solution of p-Cresidine in water.

• Then couple with C-Acid diazo.

• Stir continuously.

• When coupling is over, make monoazo diazo by adding Hydrochloric acid and Sodium

nitrite solution in presence of ice.

• Stir monoazo diazo for 4-5 hr.

• Then destroy excess sodium nitrite adding sulfamilic acid.

• Final coupling will take place with n-Phenyl J-Acid solution in alkaline condition.

• After completion of final coupling, heat to 70° C.

• Spray Dry the above reaction mass.

Mass Balance:


1 C-Acid 331.00 Product 1000.00

2 p-Cresidine 150.00 Gas / Evaporation 5978.00

3 n-Phenyl-J Acid 327.00





8 Soda ash 175.00

9 Ice 2500.00

10 Water 2000.00

TOTAL 6978.00 6978.00

120

n

CH3

SO3H

NO2

+ NaOH O2N CH CH NO2

SO3NaSO3Na

P-Nitro TolueneO-Sulphonic AcidP.N.T.O.S.A

Direct Yellow - 11

Alkaline Condensation of 4-Nitro Toluene-2-Sulphonic Acid

12. Direct Yellow 11


STEP-1: CONDENSATION

1. Take water in vessel and add caustic lye, then add PNTOSA slowly and after complete

charging check pH.

2. Adjust pH 8.00 and temp to 55° C and maintain for 1 hr.

3. Then charge caustic for condensation.

4. After complete charging bring the temp to 66° C and maintain for 3 hr.

5. Then add 50% Sulphuric acid for reduction, at pH 2.00, maintain for 2 hr.

STEP-2:

1. Take Nitrobenzene and Amine in vessel, then add above condensed mass slowly and

after complete charging, complete the reduction by adding extra amine and check for

separation.

2. Then stop the stirrer and give 3.00 hr of settling time.

STEP-3:

1. Take DEA + water in vessel and add above mass (Dye + NB + Amine) slowly in vessel and

stop when water level is reached.

2. Then stop addition and transfer the water in to Multi Effect Evaporator.

3. Complete the reduction by adding extra DEA and adjust pH at 8.50.

4. Stop the stirrer for 7.00 hr.

5. Recover dye from bottom and send for packing.

6. The balanced Nitrobenzene + Amine use in next batch.

Chemical Reaction:

121

Mass Balance:


1 PNTOSA 290.00 Product 1000.00

2 Caustic Flakes 213.00 Liquid Effluent (Recycled) 3600.00


4 Tri-Butyl Amine 21.00

5 Di-Ethanol Amine 160.00

6 Sulphuric Acid-70% 500.00

7 Water 3250.00

8 Steam 150.00

TOTAL 4600 4600

122

13. Direct Yellow 44


• Prepare MAMA’s acid solution in water.

• To this solution charge Bis (Trichloro Methyl) Carbonate.

• Charge Sodium Bi-carbonate.

• Heat to 70° C slowly in 4-5 hr.

• Stir at 70° C for 6hr.

• Heat to 80-85° C and maintain for 1hr.

• The above reaction mass is spray dried.

Chemical Reaction:

N=N

SO3H

NH2

OMe

Methylamino Azobenzenem-Sulphonic Acid

+ Cl3-C-O C O-C-Cl3

O

(MAAMSA)

Bis (Trichloro Methyl Carbonate)

Condensation in presence of

Sodium Bicarbonate

at 60-80 C

SO3H

N=N NH C

O

OMe

NH N=N

OMe SO3H

Direct Yellow 44

Mass Balance:


1 MAMA'S Acid 787.00 Product 1000.00

2 BIS (Trichloro Methyl)

Carbonate 375.00 Gas / Evaporation

7287.00

3 Sodium Bi-Carbonate 625.00

4 Water 6500.00

TOTAL 8287.00 8287.00

123

Reactive Dyes:

1. Reactive Black B


Diazotization of Vinyl Sulphone by Hydro Chloric Acid, Sodium Nitrite, Ice and Water. This

mixture is known as diazotization of VS. Coupling of Diazo - 1 with H Acid. This is known as

Coupler 1. Send the liquefied material of coupler 1 for spray drying activity. Finally the powder

material is placed into bags.

Chemical Reaction:

124

Mass Balance:

1400 Kgs Finished product Reactive Black B

Water : 250 Kgs

Vinyl Sulphone : 562 Kgs

Ice : 500 Kgs

HCl : 146 Kgs

Sodium Nitrite : 138 Kgs

Ice : 1000 Kgs

Total : 2596 Kgs

VESSEL: 1 (Diazo of Vinyl

Sulphone)

VS Diazo : 657 Kgs

Salt Generation : 177 Kgs

Water Generation : 72 Kgs

Water + Ice : 1750 Kgs

Total : 2596 Kgs

VESSEL: 2 (Coupling with

H Acid) 3433 Kgs

Reactive Black B : 991 Kgs

Salt : 434 Kgs


CO2 Liberate : 132 Kgs

Total : 3433 Kgs

H acid : 319 Kgs

Sodium Bi Carbonate : 318 Kgs

Salt : 200 Kgs

Total : 837 Kgs

Spray Drying

Spray drying Loss 1901 Kgs

Including Ice & water qty.

with 25 Kgs product loss.

125

2. Reactive Red - 195


Take initial water and chrge Vinyl Sulphone in it. Then adjust pH by sodium Bi Carbonate. Take

water in another vessel. Then add Cynuric Chloride in it. Couple both the solution. This is known

as coupler-1. Then copupled this mass with H acid solution. This is known as coupler-2. Then

prepare Diazo of Sulpho Tobias Acid. Then couple the coupler-2 with STA Diazo. Send the

liquefied material of coupler-1 for spray drying activity. Finally the powder material is packed

into bags.

Chemical Reaction:

• Cynuration

126

• Coupling Cynurated Vs with H Acid

• Preaparation of STA Diazo

127

• Coupling of Coupler 1 with STA Diazo

128

Mass Balance:

Water: 600 Liter

Vinyle Sulphone: 84 Kgs

Sodium Bi Carbonate: 84 Kgs

Total: 965 Kgs

Water: 900 Liter

Cynuric Chloride: 184.5 Kgs

Total: 1084.5 Kgs

VS Slurry: 903 Kgs

Water Generation: 18 Liter

CO2 Genearation: 44 Kgs

(Go to Air)

Total: 965 Kgs

Cynuric Chloride Solution

Total: 1084.5 Kgs

Vessel-1

921 Kgs

Vessel-2

1084.5 Kgs

Coupling-1

2005.5 Kgs

H Acid: 319 Kgs

Water: 700 Liter

Total: 1019 Kgs

Coupler: 451 Kgs

Water Genration: 18 Liter

HCl Generation: 36.5 Kgs

Water: 1500 Liter

Total: 2005.5 Kgs

Coupling-2

3130.5 Kgs Na2CO3: 106 Kgs CO2 Generation: 44 Kgs (Air)

Coupler: 777.5 Kgs


HCl Generation: 73Kgs

Water: 2200 Liter

Coupling-3

4599.5 Kgs CO2 Generation: 88 Kgs (Air)

NaHCO3: 168 Kgs

Water: 900Liter

STA Diazo: 350.5 Kgs

NaCL: 58.5 Kgs

Water: 36 Liter

Coupler: 1135.5Kgs



Water & Ice: 3100 Liter

NaCL: 58.5 Kgs

Total: 4511.5 Kgs

129

Spray Drying

Reactive Red 195 (Including Salt): 1194 Kgs

Spray Drying Loss




Total: 3317.5 Kgs

130

3. Reactive Golden Yellow - 145


Take water in a Vessel. Then add K acid, Sodium Nitrite, HCL in it. The Diazo of K Acid is coupled

with MUA. This is known as coupler-1. This coupler is Cynurated by Cynuric Chloride. This

cynurated mass is coupled with VS. After condensation the liquefied material is sending for

spray drying. Finally the powder material is packed into bags.

Chemical Reaction:

• Diazo of K–Acid

131

• Coupling with Meta Urido Aniline

• Cynuration

132

• Condensation with Vinyl Sulphone

133

Mass Balance:

Water : 1000 Liter

K Acid : 383 Kgs

SodiumNitrite : 69 Kgs

HCl : 73 Kgs

Ice : 1000 Kgs

Total : 2525 Kgs

K Acid Diazo : 430.5 Kgs Water

Generation : 36 Liter Salt

Generation : 58.5 Kgs Water &

Ice : 2000 Liter

Total : 2525 Kgs

VESSEL : 1

2525 Kgs

Coupling – 1

2676 Kgs

MUA : 151 Kgs

Coupler: 545 Kgs


Salt : 58.5 Kgs

Water : 2036 Liter

Total : 2676 Kgs

Coupling - 2 : 2860.5

Kgs

Cynuric Chloride : 184.5

Kgs

Coupler: 693 Kgs

HCl: 73 Kgs

Water: 2036 Liter

Salt: 58.5 Kgs

Condensation with Vinyl

Sulphone

VS: 218 Kgs

Reactive Yellow145: 937.5 Kgs

Water: 2036 Liter


NaCl: 58.5 Kgs

Total: 3141.5 Kgs

Spray drying

Spray Drying Loss


Water: 2036 Liter

Product Loss: 25 Kgs

Total: 2170 Kgs

Reactive Yellow 145(Including Salt):971Kgs

134

4. Reactive Golden Yellow HER


Take water in vessel. Then add K acid, Sodium Nitrite, HCL in it. The Diazo of K acid is coupled

with MUA. This is known as coupler-1. This coupler is Cynurated by Cynuric Chloride. This

Cynurated mass is coupled with VS. After filtration the effluent will go to ETP. The wet cake is

condensed with DASDA. The liquefied material is sending for spray drying. Finally the powder

material is packed into bags.

Chemical Reaction:

• Diazo of K–Acid

• Coupling with Meta Urido Aniline

135

• Cynuration

• Condensation with DASDA

136

Mass Balance:

Water: 1000 Liter

K Acid: 383 Kgs

Sodium Nitrite: 69 Kgs

HCl: 73 Kgs

Ice: 1000 Kgs

Total: 2525 Kgs

VESSEL : 1 2525 Kgs

K Acid Diazo: 430 Kgs

Water Generation: 36 Liter

Salt Generation: 58.5 Kgs


Total: 2525 Kgs

Coupler: 545 Kgs


Salt: 58.5 Kgs

Water: 2036 Liter

Total: 2676 Kgs

Coupling-1 2672Kgs MUA : 151

Filtration 2116 liter waste water

will go to ETP

Cynuric Chloride:

184.5Kgs

Coupling – 2

744.5Kgs

Coupler: 708 Kgs

HCl: 36.5 Kgs

DASDA: 344 Kgs Condensation with DASDA

Spray drying

Reactive Yellow HER: 1000.5 Kgs

HCl Generation: 73 Kgs

Total: 1073.5Kgs

Reactive Yellow HER (Including Salt):

9715 Kgs

Spray Drying Loss

HCl Generation: 73 Kgs

Product Loss: 29 Kgs

Total: 102 Kgs

137

5. Reactive Orange H2R


Acetylation of N Methyl J Acid: Charge real quantity of NMJ acid into Water. And take pH 7 By

use of 20 % solution of NaOH. Then add Ice and take temperature 15 degree C. and then charge

Acetic Anhydride then stir for 6 Hrs. then check unreacted NMJ acid. If it is OK then take pH by

use of 20 % solution os NaOH Flakes.

Diazotization of Sulpho Tobias Acid: Charge real quantity of S.T.A in water. Then charge HCL. In

the solution. Then slowly charge sodium Nitrite solution till SI positive stable and Cr Positive.

Coupling: Add Acetyl NMJ solution to S.T.A. Diazo. After completion of adding take pH 6.5 by

Sodium Bi Carbonate. After adjusting pH it till Diazo negative in coupling test.

Hydrolysis: heat the coupled mass to 40-45 degree C and then charge NaOH flakes and then

heat 80 degree c and maintain the mass for 3-4 Hrs. till hydrolysis completion. After completion

of hydrolysis adjust pH 7 by use of HCL.

Base Dissolving: Take upper filter w/c into water and stir the material till clear on spot.

Cynuration of Upper Clear Base Solution: Take Cynuric Chloride into water with Ice. Then add

upper clear base solution slowly and stir the material. Then take pH 6.5 by use of soda solution.

After completion of Cynuration reaction the mass will be transferred for condensation process.

Condensation: Add Ammonia solution into the Cynuration mass and stir the material to

complete condensation. Then after the mass is send for spray drying activity for obtain finished

product.

Chemical Reaction:

• Activation of NMJ

138

• Di Azotization of STA

• Coupling Acetyl-N-Methyl J Acid with STA Diazo

139

• Hydrolysis

140

Mass Balance:

Water : 1500 Liter

NMJ Acid : 253 Kgs

Sodium Hydroxide : 40 Kgs

Acetic Anhydride : 102 Kgs

Total : 1895 Kgs

Acetyl NMJ Acid : 317 Kgs

Water Generation : 18 Liter

CH3COOH Generation : 60 Kgs

Water : 1500 Liter

Total : 1895 Kgs

STA Diazo : 350.5 Kgs

Salt generation : 58.5 Kgs


Water generation : 36 Liter

Total : 2245 Kgs

CO2Generation 88 Kgs (Go to Air) Coupling : 4308 Kgs

Coupler : 675 Kgs

Salt generation 58.5 Kgs Water

Generation : 90 Liter


HCl Generation : 36.5 Kgs

Water & Ice : 3300 Liter

Total : 4220 Kgs

NaHCO3 : 168 Kgs

VESSEL : 2 (Preparation of SAT Diazo)

2245 Kgs VESSEL : 1 (Asetylation of NMJ Acid)

1895 Kgs

NaOH : 40 Kgs Hydrolysis : 4260 Kgs

Base of Orange M.R : 633 Kgs

Salt generation :58.5 Kgs

Water Generation : 90Liter


CH3COONaGeneration : 82 Kgs



Water : 800 Liter

Sulpho Tobias Acid : 303 Kgs

HCl : 73 Kgs

Sodium Nitrite : 69 Kgs

Ice : 1000 Kgs

Total: 2245 Kgs

141

Filtration Effluent goes to ETP: 3469 Liter

Cyutric Chloride : 184.5 Kgs

Water : 4000 Liter

Ice : 1000 Kgs

Total : 5184.5 Kgs

Wet Cake including Salt

and Moisture : 791 Kgs

Cynuration : 5975.5 Kgs

NH4OH Solution : 35 Kgs Reactive Orange M2R : 859 Kgs

Water &Ice : 5080 Liter

HCl : 36.5 Kgs

Total : 5975.5 Kgs

Isolation : 6010.5 Kgs

Reactive Orange H2R (Including Salt):

869.0 Kgs

Spray drying Loss:

Water & Ice : 5080

Liter HCl : 36.5 Kgs

Product Loos : 25 Kgs

Total : 5141.5 Kgs

Base of Orange M.R : 633 Kgs

Salt generation :58.5 Kgs

Water Generation : 90 Liter


CH3COONaGeneration : 82 Kgs



142

� REACTIVE BLUE

1. BLUE 3R

PROCESS DISCRIPTION

H acid is cynurated & coupled with dizotized vinyl sulphone. Product condensed

with metanilic acid & spray deried.

CHEMICAL REACTION

(A- SO

2

CH

2

CH

2

OSO

3

H )

A

OCH

3

CH

3

NH

2

+ +

2HClNaNO

2

+

OH

NH

2

SO

3

H SO

3

H

+

CH

3

CH

3

CO

O

CO

+

NaHCO

3,

CuSO

4

CH

3

OCH

3

A

NN

SO

3

HSO

3

H

NH

2

OCH

3

OH

Cu

+ 2NaCl + 3H

2

O + CO

2

CH

3

COONa+

143

NH

SO

3

H

NH

2

+

+

NaNO

2

2HCl

++

+

SO

3

HSO

3

H

NH

2

OH

ClCl

Cl

N

NN

AH

2

N+

NaHCO

3,

Na

2

CO

3

SO

3

H

NH

N N

OH

SO

3

H SO

3

H

NH

N N

N

Cl

NH

A

(A- SO

2

CH

2

CH

2

OSO

3

H )

2NaCl + 3H

2

O + CO

2

+

Reactive BLUE F4R

2. BLUE F4R

PROCESS DISCRIPTION

4 ADAPSA Diazo H acid is coupled with H-Acid, cynurated condensed with vinyl

sulphone ester & spray deried.

CHEMICAL REACTION

3.

144

3. BLUE HERD

PROCESS DISCRIPTION

4 Sulpho Anthranilic acid hydrozone is coupled with 6-AAPSA diazo product

obtained is completed with copper Sulphate. The mass filtered wet caked

hydrolysis and base is condensed with Cynurated metanilic Acid & with cynurated

PPDDSA. Product obtained & spray dried.

CHEMICAL REACTION

145

++

2HCl

NaNO

2

+

+

+

SO

3

H

OH

NH

NaOHCuSO

4

O

N

OH

C

SO

3

H

H

2

N

HO

NHCOCH

3

ClCl

Cl

N

NN

+

(A- SO

2

CH

2

CH

2

OSO

3

H )

A

NH

C

2

H

5

+

NaHCO

3 ,

Na

2

CO

3

N N

N

Cl

SO

3

H

NH

O

N

N

O

N

N

Cu

O

SO

3

H

O

N

C

2

H

5

A

+ CO

2

2NaCl + 3H

2

O+

Na

2

SO

4

+

4. BLUE 221

PROCESS DISCRIPTION

4 Sulpho Anthranilic acid hydrozone is coupled with 6-AAPSA diazo product

obtained is complexed with copper Sulphate. The mass filtered wet caked

hydrolysis and base is condensed with N Ethyl Meta Base Ester.

CHEMICAL REACTION

146

SO

3

H

SO

3

H

H

3

OS

NH

2

O

N

N

O

SO

3

H

H

2

NCH

2

CH

2

NH

Cl

Cl

NHCH

2

CH

2

NH

2

2

+

Cl

N N

N

Cl

Cya Chloride

+

Cl

2

NaHCO

3

, Na

2

CO

3

H

3

OS

SO

3

H

NH

Cl

N

NN

HNCH

2

CH

2

NH

Cl

Cl

SO

3

H

O

N

N

O

SO

3

H

NHCH

2

CH

2

NH

Cl

N

NN

NH SO

3

H

SO

3

H

+ 2NaCl + Na

2

SO

4

+ CO

2

Reactive Blue HEGN

5. BLUE HEGN

PROCESS DISCRIPTION

Aniline 2, 4 Disulphonic Acid Is Cynurated & Condensed with Blue 198 Base &

Spray dried.

CHEMICAL REACTION

147

NH

2

SO

3

H

SO

3

H

NH

2

A

NHCH

2

CH

2

NH

2

Cl

Cl

H

2

NCH

2

CH

2

NH

SO

3

H

O

N

N

O

SO

3

H

2

2

+

+

2

Cl

+

Cya Chloride

Cl

N

NN

Cl

(A- SO

2

CH

2

CH

2

OSO

3

H )

MBVSE

NaHCO

3

, Na

2

CO

3

SO

3

H

SO

3

HNH

N N

N

NHCH

2

CH

2

NH

SO

3

H

O

N

N

O

SO

3

H

Cl

Cl

HNCH

2

CH

2

NH

N N

N

NH

SO

3

H

H

3

OS

NH

A

A

NH

+ CO

2

2NaCl

+

Reactive Blue FGN

6. BLUE LFNG

PROCESS DISCRIPTION

Aniline 2,4 Disulphonic Acid Is Cynurated & Condensed With Blue 198 Base &

Spray dried.

CHEMICAL REACTION

148

H

2

N

NH

2

SO

3

H

A

2NaNO

2

4HCl

OH

NH

2

SO

3

H

NH

2

NH

2

SO

3

H

++

+

++

+

Cl

N

NN

Cl Cl

SO

3

H

SO

3

H

MPDSA

CYA CHLORIDE

H-Acid

NaHCO

3

, Na

2

CO

3,

NaOH

SO

3

H

SO

3

H

NN

SO

3

HSO

3

H

OHNH

2

N N NH

N N

N

Cl

SO

3

H

NH

A 2NaCl + 3H

2

O + CO

2

+

Reactive Blue FB

(A- SO

2

CH

2

CH

2

OSO

3

H )

STA

7. BLUE BF

PROCESS DISCRIPTION

MPDSA Is Cynurated & Condensed With Vinyl Sulphone. Product diazotized &

coupled with H acid, Product again coupled with Sulfo Tobias Acid & spray dried.

CHEMICAL REACTION

149

+

SO

3

H

NH

2

H

2

N

ClCl

N N

N

Cl

+

+

SO

3

H

NH

2

SO

3

H

NH

2

A

+

+ 4HCl

2NaNO

2

H-Acid

SO

3

H

SO

3

H

+

NH

2

OH

MPDSA

CYA CHLORIDE

(A- SO

2

CH

2

CH

2

OSO

3

H )

STA

NaHCO

3

, Na

2

CO

3,

NaOH

NN

NH

2

OH

SO

3

H SO

3

H

N N

SO

3

H

SO

3

H

SO

3

H

NH

NH

Cl

N

NN

A

+

+ CO

2

2NaCl + 3H

2

O

Reactive Blue BFN

8. BLUE BFN

PROCESS DISCRIPTION

MPDSA is Cynurated & Condensed with Vinyl Sulphone. Product diazotized &


CHEMICAL REACTION

150

9. BLUE 2B

PROCESS DISCRIPTION

MPDSA is Cynurated & Condensed With Vinyl Sulphone. Product diazotized &


CHEMICAL REACTION

151

Mass Balance:

Sr.

NO.

Raw

Materials

Total Input Quantity (Kg)

BLUE

3R

BLUE

F4R

BLUE

HERD

BLUE

HEGN

BLUE

LFNG

BLUE

221

BLUE

BF

BLUE

BFN

BLUE

2B

1 Cynauric

Chloride

- 64 144.5 156 176 109 78 100 -

2 Oil HS - 1 3 3 3 1 1 2 -

3 Aniline 2,4 Di

Sulpho Acid

- - - 206 - - - - -

4 Aniline 2,5 Di

Sulpho Acid

- - - - 239 - - - -

5 4 ADPSA - 82 - - - - - - -

6 6 AAPSA - - 106 - - - - - -

7 NEPBE - - - - - - - - -

8 4 Sulpho

Hydrogen

- - 133 - - - - - 364

9 H Acid 32 100 - - - 168 120 136 -

10 MPDSA - - - - - - - 100 -

11 Vinyl Sulphone - 107 - - - 164 117 - -

12 Meta Base

Ester

- - - - 296 - - 149 -

13 STA - - - - - 167 119 155 -

14 Antifoam 5 4 3 5 5 2 2 5 5

15 Blue 198 Base - - - 200 250 - - - -

16 Sulfamic Acid 1 1 1 - - 1 1 1 1

17 Sulpho OAVS - - - - - - - - 453

18 SPD Oil 2 2 3 3 5 3 3 4 10

19 DDC Oil 10 10 10 20 10 10 10 - -

20 Soda Ash 45 113 95 173 200 211 151 130 113

21 Sodium

Sulphate

484 600 280 427 37 100 290 240 -

22 Sodium

Bicarbonate

41 - 120 76 270 - - 88 287

23 Sodium Nitrite 49 21 30 - - 77 55 70 79

24 Copper

Sulphate

249 - 112.5 - - - - - 331

25 Caustic Soda 67 25 257 - 32 21 15 45 -

26 HCl 37 125 199 - 100 261 285 62 -

27 DMAVS 234 - - - - - - - -

28 Acetic

Anhydride

146 - - - - - - - -

29 PPDDSA - - 69 - - - - - -

Total 1586 1255 1566 1269 1623 1295 1247 1287 1643

152

Sr.

NO.

TOTAL MASS

REMOVED

Total Output Quantity (Kg)

BLUE

3R

BLUE

F4R

BLUE

HERD

BLUE

HEGN

BLUE

LFNG

BLUE

221

BLUE

BF

BLUE

BFN

BLUE

2B

1 Total Water

Evaporated

73 41 174 45 106 83 60 98 121

2 CO2 Evolved during

Reaction

40 47 102 112 224 87 62 100 197

3 Salt Formation

during reaction,

Removed from NF

273 162 250 107 268 120 120 84 320

4 Organics removed

from NF

200 5 40 5 25 5 5 5 5

5 Total Finished

Product

1000 1000 1000 1000 1000 1000 1000 1000 1000

Total 1586 1255 1566 1269 1623 1295 1247 1287 1643

153

� REACTIVE GOLDEN YELLOW

1. Golden Yellow R

Process Description

Vinyl Sulphone diazotized coupled with MPDSA and spray dried.

Chemical Reaction

PBVSE

+NH

2

A NaNO

2

2HCl

+

+ NH

2

SO

3

H

NaHCO

3

,NaOH

N N

A

NH

2

NH

2

SO

3

H

NH

2

+ 2NaCl + 3H

2

O + CO

2

Reactive Golden Yellow R

MPDSA

2. Golden Yellow RNL

Process Description

Vinyl Sulphone ester is diazotized & coupled with Acetyl MPDSA and spray dried.

Chemical Reaction

Acetyl MPDSA

SO

3

H

NH

2

+

+

2HClNaNO

2

A NH

2

+

PBVSE

NHCOCH

3

NaHCO

3

+ CO

2

2NaCl + 3H

2

O+

NH

2

SO

3

H

A

NN

NHCOCH

3

Reactive Golden Yellow RNL

154

Mass Balance:

Input:

Sr. No. Raw Materials Total Input Quantity (Kg)

Golden Yellow RNL Golden Yellow R

1 A. MPDSA 238 -

2 MPDSA - 312

3 Vinyl Sulphone 298 467

4 Antifoam 4 5

5 SPD oil 4 5

6 DDC Oil 20 -

7 Sulfamic Acid 1 1

8 Sodium Bi

Carbonate

237 140

9 HCl 162 103

10 Caustic Lye - 66

11 Sodium Sulphate 176 -

12 Sodium NItrite 72 70

Total 1212 1169

Output:

Sr. No. Total Mass

Removed From

Reaction & Process

Total Output Quantity (Kg)

Golden Yellow RNL Golden Yellow R

1 Total Water

Evaporated

88 96

2 CO2 Evolved during

Reaction

124 73

3 Total Finished

Product

1000 1000

Total 1212 1169

155

PBVSE

NH

2

A

NH

2

NH

2

OCH

3

A

+ + +

4HCl2NaNO

2

(A- SO

2

CH

2

CH

2

OSO

3

H )

DMAVSE

OH

NH

2

SO

3

H SO

3

H

+

H-Acid

NaHCO

3

, NaOH

NNA

SO

3

HSO

3

H

NH

2

OH

N N

SO

3

H

OCH

3

A + CO

2

2NaCl + 3H

2

O+

NAVY Blue 2G

� REACTIVE NAVY BLUE

1. Navy Blue 2G

Process Description

Vinyl Sulphone ester & DMAVS are diazotized & coupled with H Acid and spray

dried.

Chemical Reaction

156

2

NH

2

SO

3

H

NH

2

Cya Chloride

2

Cl Cl

Cl

N

NN

+ H

2

N

CH

3

SO

3

H

+ 2

2NaNO

2

4HCl

++

H-Acid

+

SO

3

HSO

3

H

NH

2

OH

MPDSA

OTSSA

Na

2

CO

3

, NaOH

H

3

OS

CH

3

NH

N N

N

Cl

NH

OH

NH

2

SO

3

H SO

3

H

SO

3

H

N N NN

SO

3

H

NH

N N

N

Cl

NH

CH

3

SO

3

H

+ 3H

2

O + CO

2

Navy Blue XLE

2. NAVY BLUE XLE

Process Description

Vinyl Sulphone ester & DMAVS are diazotized & coupled with H Acid and spray

dried.

Chemical Reaction

157

3. NAVY BLUE RGB

Process Description

Vinyl Sulphone ester & OAVS ester are diazotized & coupled with H Acid and

spray dried.

Chemical Reaction

DMAVSE

(A- SO

2

CH

2

CH

2

OSO

3

H )

+

A

OCH

3

NH

2

NH

2

PBVSE

A + +

4HCl2NaNO

2

OH

NH

2

SO

3

H SO

3

H

+

H-Acid

NaHCO

3

NAVY Blue RGB

A

OCH

3

NN

OH

NH

2

SO

3

H SO

3

H

N N

A

+ 2NaCl + 3H

2

O

158

Mass Balance:

Input:

Sr.

No.

RAW MATERIALS TOTAL INPUT QUANTITY (kg)

NAVY BLUE 2G NAVY RGB NAVY XLE

1 H Acid 196 204 116

2 2,5 DMAVS 222 - -

3 Vinyl Sulphone 176 193 -

4 Antifoam 6 5 10

5 Sulfamic Acid 1 1 2

6 MPDSA - - 175

7 Cynauric Chloride - - 175

8 Oil HS - - 2

9 Ortho Toluidine Sul. Acid - - 175

10 SPD Oil 4 4 4

11 DDC Oil 20 20 -

12 OAVS - 234 -

13 Caustic Lye 27 26 70

14 Sodium Bicarbonate 136 166 291

15 Sodium Nitrite 88 98 65

16 HCl 157 179 297

17 Sodium Sulphate 230 199 -

1263 1329 1388

Output:

Sr.

No.

RAW MATERIALS TOTAL OUTPUT QUANTITY (kg)

NAVY BLUE 2G NAVY RGB NAVY XLE

1 Total Water Evaporated 87 71 130

2 CO Evolved during Reaction 71 87 156

3 Salt formation during the

reaction removed from NF

95 161 92

4 Organics removed from NF 10 10 10

5 Total Finished Product 1000 1000 1000

1263 1329 1388

159

Disperse Dyes:

1. AZO Dyes


1. Preparation of Hydrochloride &Diazonium Salt compounds For Monoazo Dyes:

DM water/ Process water is charged in Reaction vessel. Then required quantity of Amines as

mentioned in Raw Material list Annexure (A) is charged. Then required quantities add Acid

[HCL / H2SO4 / Nitric] is added & it is stirred for 4-5 hrs to form good suspension of

Hydrochloride. Now Crushed ICE is added to reduce temperature 0 to 5 Deg.C. Then Sodium

Nitrite is slowly added keeping Congo red paper positive & S.I. paper slightly positive

&stirred for 1-2 hrs at 0 to 5 Deg.C. Now diazo is ready for coupling.

2. Preparation of Coupler compound:

In Coupling reaction vessel, required quantity of Process / DM water is taken & required

quantity of coupler as mentioned in Raw Material list Annexure is added. Then little

quantity of eighter alkali or acid is added to make soluble & buffer to maintain coupling

condition. Then crushed ICE is added to reduce temperature 15 to 20 Deg.C

3. Coupling:

Now in above coupling reaction vessel previously prepared diazo mass is slowly received in

2-3 hrs. Keeping temperature 5 to 10 Deg.C & is stirred to complete coupling reaction.

Reaction mass is filtered, washed with Water. Filtrate & Washing is send to ETP for further

treatments

4. Grinding in Sand / Beed Mills / Homozinizer

Press cake is mixed with Dispersing agents/ auxiliaries & grinded in Sand Mills / Beed Mills /

Homozinizer. Now the mass is eighter directly converted in Liquid & standardization to

Dispatch as A Liquid Dyes OR if powder require, it is directly straightway Spray Dried to

dispatch as a Powder form.

160

Mass Balance:

FLOW CHART WITH MATERIAL BALANCES [Mono Azo]:

INPUT IN KGS OUTPUT IN KGS

Water 1000 kg

Amines 250 kg

Acid 400 kg

ICE 1000 kg

Sodium Nitrite 95kg

Water 500 kg

Coupler 275 kg

Alkali / Acid 150 kg

ICE 1000 kg

Water for Washing 4670 kg ML to ETP

2000 kg 2000 kg wet cake

Auxiliaries 400Kg

Press Cake 2000 kg

1400 kg Water evaporation

in Spray Drying

1000 kg Finish Product

Total 9070 kg 9070 kg

Diazotization

Diazo Reaction

Vessel

I Coupling

Reaction Vessel

Filtration &

Washing

Spray drying Unit

Sand Mills Unit

161

2. Anthraquinones / Condensed Dyes


In suitable reaction vessel, require quantity water Or suitable solvent like Dimethyl Form amide

/ Toluene / Xylene is taken .Then mono azo mass or condensing Product is condensed with

require condensed products as mentioned in raw material list Annexure (A) at require

parameters. After completion of condensation, Solvents are Distilled out for Re-Use &

remaining reaction mass is filtered, washed with Water. Filtrate & Washing is send to ETP for

further treatments.


Homozinizer. Now the mass is eighter directly converted in Liquid & standardization to Dispatch

as A Liquid Dyes OR if powder require, it is directly straightway Spray Dried to dispatch as a

Powder form.

Mass Balance:

FLOW CHART WITH MATERIAL BALANCES [Mono Azo]:

INPUT IN KGS OUTPUT IN KGS

Water 800 kg

Amines 150 kg

Acid 200 kg

ICE 1000 kg

Sodium Nitrite 50kg

Cold Water Wash 1000 kg 2000 kg ML to ETP

1200 kg Press cake

Water 500 kg

Press Cake 1200 kg

Couplers 100kgs

ICE 500 kg

700 kg water recycled to first stage

Auxiliaries’

For STD 200Kg 1800 kg Finish Product

Total 5700 kg 5700 kg

Diazotization

Diazo Reaction

Vessel

Reverse Osmosis

Unit

Standardization

Filter press

I Coupling

Reaction Vessel

162

3. Cyanation Dyes


In a suitable reaction vessel require quantity water OR suitable Solvents like Dimethyl Form

amide / Methanol taken. Then mono azo OR AQ Product mass is charged & further condensed

with Sodium Cyanide. After Completion Of complete consumption of Sodium Cyanide, Solvent

is distilled out for Re-Use & reaction mass is filtered. ML is collected in separate Vessel for

Killing / Detoxification of traces cyanide with Sodium Bisulphite. Again it is filtered. Ml is send to

ETP for further treatment.


Homozinisers. Now the mass is eighter directly converted in Liquid & standardization to ispatch

as A Liquid Dyes OR if powder require, it is directly straightway Spray Dried to dispatch as a

Powder form.

163

Mass Balance:

INPUT IN KGS

OUTPUT IN KGS

Solvent 1500 kg

Mono/R.M.Product 250 kg

Sodium Cyanide 200 kg

Water 750 kg

1425 kg solvent recycle

Water 500 kg

Sodium Bisulphite 250 kg

Alkali 150 Kg

1400 kg Wet cake

Water 1000kg Reslury

Wet Cake 1400kg

Water for Washing

2500 kg 775 kg ML ETP

3300 kg ML to ETP

1600 kg wet cake for Sand

D.A Auxiliaries 200Kg mill

Press Cake 1600 kg

800 kg Water evaporation

in Spray Drying

1000 kg Finish Product

Total 10300 kg 10300 kg

Reaction Vessel

Detoxification

Vessel

Sand Mills Unit

Spray drying Unit

Solvent recovery

system

Re-Slurry

Filter Press

Filter press Filter press

164

O

O

OH

OH

2C4H9 NH2

Quinizarine(M.Wt. 240)

n-Butylamine (M.Wt. 73)

HN

HN

C4H9

C4H9

O

O

H2O

Solvent Blue 35 (M.Wt. 350)

Solvent Dyes:

1. Solvent Blue 35


A mixture of Quinizarine and Leuco Quinizarine is reacted with n-Butyl amine using methanol as

a solvent. The product is then filtered and washed with water. The wet cake is dried and

pulverized to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Blue 35

Sr. No. Input Kg Output Kg

1 Methanol 1454.55 Solvent Blue 35 1000

2 Quinizarine 563.63 Methanol Recovered 1420.05

3 Leuco Quinizarine 140 Butyl Amine Recovered 498.10

4 n-Butyl amine 512.72 Effluent 5641.40

5 Nitrobenzene 85.45 Loss on drying 545.45

6 Water 6363.64 Residue 15.00

Total 9120 Total 9120

165

O

O

OH

OH

2

H3C

NH2

CH3

CH3


Mesidine(M.Wt. 135)

O

O

HN

HN

CH3

CH3

CH3CH3

CH3

CH3

H2O


2. Solvent Blue 104


A mixture of Quinizarine and Leuco Quinizarine is reacted with Mesidine using ODCB as a

solvent. The reaction mass is then oxidized using air. The product is isolated using methanol. It

is then filtered and washed with water. The wet cake is dried and pulverized to get the finished

product.

Chemical Reaction:

Mass Balance:

Solvent Blue 104


1 ODCB 789.47 Solvent Blue 104 1000

2 Quinizarine 421.05 ODCB Recovered 774.78

3 Leuco Quinizarine 105.26 Methanol Recovered 1541.05

4 Mesidine 605.26 Effluent 7410.46

5 Methanol 1578.95 Loss on drying 657.89


Total 11394.70 Total 11394.70

166

OHO

OHO NH2

NHCOCH3


p-Amino Acitanilide (M.Wt. 150)

O OH

O NH NHCOCH3

H2O


3. Solvent Blue 122


A mixture of Quinizarine & Leuco Quinizarine is reacted with p-amino acetanilide using Iso

propyl alcohol as a solvent. The reaction mass is then oxidized using air. The product is then

isolated using water. It is then filtered and washed with water. The wet cake is dried,

pulverized and sieved to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Blue 122


1 Iso propyl alcohol 1960.78 Solvent Blue 122 1000

2 Quinizarine 392.15 IPA Recovered 1915.74

3 Leuco Quinizarine 98.04 Effluent 8201.72

4 P-amino acetanilide 637.25 Los on drying 1862.74

5 HCl 98.04 Residue 10.00

6 Water 9803.92

Total 12990.20 Total 12990.20

167


O OH

O OH

NH2

CH3

p-Toluidine(M.Wt. 107)

NHO

NHO CH3

CH3

H2O

Solvent Green 3 (M.Wt. 418)

4. Solvent Green 3


A mixture of Quinizarine & Leuco Quinizarine is reacted with Para Toluidine using Butanol as a

solvent. The product is isolated by distilling off the Butanol; it is then filtered and washed with

HCl. The wet cake is dried, pulverized and sieved to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Green 3


1 Butanol 2474.23 Solvent Green 3 1000

2 Quinizarine 463.91 Butanol Recovered 2440.51


4 Para Toluidine 567.01 Loss on drying 298.96


6 HCl 309.27

Total 10542.25 Total 10542.25

168

C

O

C

O

ONH2NH2

Phthalic Anhydride (M.Wt. 148)

1:8 Diamini Napthalene (M.Wt. 158)

C

N

C

N

O

H2O

Solvent Orange 60 (M.Wt. 270)

5. Solvent Orange 60


Phthalic anhydride is reacted with 1: 8 Diamino Naphthalene using o-Xylene as a solvent. The

product is isolated using methanol. It is then filtered and washed with water. The wet cake is

dried and pulverized to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Orange 60


1 o-Xylene 2666.67 Solvent Orange 60 1000

2 Phthalic Anhydride 575.75 o-Xylene Recovered 2610.33

3 1:8 Diamino Naphthalene 606.06 Methanol Recovered 5216.70

4 Methanol 5296.97 Effluent 4448.72

5 Water 4545.45 Loss on drying 400

6 Residue 15.15

Total 13690.90 Total 13690.90

169

O OH


o-Xylene


OHO

O OH

OHO



Crude Quinizarine is refluxed using o-Xylene as a solvent. The resulting product is then filtered

and washed with methanol followed by hot water wash. The wet cake is dried and pulverized to

get the finished product.

Chemical Reaction:

Mass Balance:

Solvent orange 86


1 O-Xylene 2714.29 Solvent orange 86 1000

2 Quinizarine 1071.43 O-xylene recovered 2680.02

3 Methanol 714.28 Methanol recovered 696.14

4 Water 6428.57 Effluent 6245.26

5 Loss on drying 150

6 Residue 157.15

Total 10928.57 Total 10928.57

170

N

NC

HC

O

CH3

BrO

CH3

NH2

6-Bromo Anthrapyridone (M.Wt. 340)


KOH

O

HN

CH3

CH3

KBr H2O

O

Solvent Red 52 (M.Wt. 366)

7. Solvent Red 52


6-Bromo Anthrapyridone is condensed with Para Toluidine using o-Xylene as a solvent. The

product is isolated by adding methanol. It is then filtered & washed with water. The wet cake is

dried & pulverized to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Red 52


1 o-Xylene 2234.04 Solvent Red 52 1000

2 6-Bromo Anthrapyridone 978.74 o-Xylene Recovered 2196.38

3 Para Toluidine 382.97 Methanol Recovered 5375.95

4 Potassium acetate 468.08 Residue 25.53

5 Methanol 5446.81 Aqueous effluent 15189.46

6 Water 14893.60 Loss on drying 957.44

7 HCl 340.42

Total 24744.76 Total 24744.76

171

O

Cl O NH2

O

Cl

Cl

Cl

+

NH2

Tetra Chloro Phthalic Anhydride (M.Wt. 286)

1:8 Diamino Naphthalene(M.Wt. 158)

Cl

Cl

ClOCl

C

N

C

N+ H2O


8. Solvent Red 135


Tetra Chloro Phthalic Anhydride is reacted with 1:8 Di Amino Naphthalene using o-Xylene as a

solvent. The product is filtered and washed with water. The wet cake is dried and pulverized to

get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Red 135


1 o-Xylene 2080 Solvent Red 135 1000

2 TCPA 760 o-Xylene Recovered 2010

3 1:8 DAN 400 Methanol Recovered 466

4 Methanol 480 Effluent 4524

5 Water 4800 Loss on drying 504

6 Residue 16


172

O

O

Cl NH2

+

1-Chloro Anthraquinone (M.Wt. 242.5)

Mono Cyclo Hexyl Amine (M.Wt. 99)

Sodium Acetate

HN

O

O

+ +NaCl H2O

Solvent red 168 (M.Wt. 305)

9. Solvent Red 168


1-Chloro Anthraquinone is condensed with mono cyclohexylamine using o-Xylene as a solvent.

The product is isolated using methanol and then filtered. It is then washed with water. The

wet cake is dried and pulverized to give the finished product.

Chemical Reaction:

Mass Balance:

Solvent Red 168



2 1-Chloro AQ 833.33 o-Xylene Recovered 834.28

3 Mono cyclohexylamine 404.76 Methanol Recovered 3755.25

4 Sodium Acetate 259.52 Residue 14.28



Total 18069.07 Total 18069.07

173

S+

H3C CN

H3COOC NH2

CN

CH3

HN NH

(CH2)3

OCH3OCH3

(CH2)3

Diazo Compound (M.Wt. 196)

Coupler Component (M.Wt. 292)

1. H2SO4 + NaNO2

2. Coupling

NH3COOC

CNH3C

S

(CH2)3

OCH3 OCH3

(CH2)3

NHHN

CH3

N CN


10. Solvent Red 195


The diazo component is diazotized using Sulfuric acid and Sodium nitrite. It is then coupled with

Coupler 195 in the acidic medium. It is filtered and washed till neutral. The wet cake is dried.

The product is then pulverized to get the finished product.

Chemical Reaction:

174

Mass Balance:

Solvent Red 195


1 3 Methoxy Propyl Amine 447.76 Solvent Red 195 1000

2 Tri Ethyl Amine 125 Aqueous Effluent 48194.04

3 Amogh FP-165 395.52 Loss on drying 3000

4 Methanol 419.77

5 HCl 559.70

6 Sulfuric Acid 1865.67


8 Acetic acid 1791.04

9 Propionic Acid 298.50

10 Diazo component 425.37

11 Ice + Water 45709

Total 52194.04 Total 52194.04

175

+

OCl

NH2O Cl

1:5 Dichloro Anthraquinone (M.Wt. 277)

Mono Cyclo Hexyl Amine (M.Wt. 99)

Sodium Acetate

HNO

NH O

+ NaCl + H2O


11. Solvent Red 207


1:5 Dichloro Anthraquinone is condensed with mono cyclohexylamine using o-Xylene as a

Solvent. The product is isolated using methanol and then filtered. It is then washed with water.

The wet cake is dried and pulverized to give the finished product.

Chemical Reaction:

Mass Balance:

Solvent Red 207



2 1:5 DCAQ 725.58 o-Xylene Recovered 957.90

3 Mono cyclohexylamine 627.90 Methanol Recovered 4986.04

4 Sodium Acetate 493.02 Residue 13.95



7 Acetic Acid 116.27

Total 19660.43 Total 19660.43

176

12. Solvent Violet 13


A mixture of Quinizarine and Leuco Quinizarine is reacted with Para Toluidine using Butanol as a

solvent in the presence of HCl & Zinc. The product is filtered and washed with dilute HCl &

water. The wet cake is dried and pulverized and sieved to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Violet 13


1 Butanol 3157.89 Solvent Violet 13 1000

2 Quinizarine 752.63 Butanol Recovered 2905.26


4 Para Toluidine 394.73 Loss on drying 300

5 Zinc 34.21 Residue 15.00

6 HCl 842.10

7 Water 15789.50

Total 20986.84 Total 20986.84

S olv ent V io le t 13 (M.W t. 329)

H2 O+

O

O HN

p-Toluid ine(M.W t. 107)

Quinizarine(M.W t. 240)

OHO NH2

O

+

OH CH3

CH3

177

CH3

CH3

+

O

NH2O



HNO

O

+ H2O

Solvent Violet 14 (M.Wt. 418)

Cl Cl

2

Potassium Acetate

NHH3C

+ KCl

13. Solvent Violet 14


1:8 Dichloro Anthraquinone is reacted with Para Toluidine using ODCB as a solvent. The product

is isolated using methanol. It is then filtered and washed with water. The wet cake is dried and

pulverized to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Violet 14


1 ODCB 838.71 Solvent Violet 14 1000

2 1:8 DCAQ 645.16 ODCB Recovered 818.64

3 Para Toluidine 564.52 Methanol Recovered 2534.58

4 Pot. Acetate 709.67 Effluent 10872.58

5 HCl 483.87 Loss on drying 258.08


7 Methanol 2580.65


178

O +N CH3

O

O

Phthalic Anhydride (M.Wt. 148)

Quinaldine(M.Wt. 143)

C

CH

C

N+ H2O

Solvent Yellow 33 (M.Wt. 273)

14. Solvent Yellow 33


Phthalic anhydride is reacted with Quinaldine using ODCB as a solvent. The product is isolated

using methanol. It is then filtered and washed with water. The wet cake is dried and pulverized

to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Yellow 33


1 ODCB 888.88 Solvent Yellow 33 1000

2 Phthalic anhydride 555.55 ODCB Recovered 865.54

3 Quinaldine 555.55 Methanol Recovered 2180


5 Water 6250 Loss on Drying 333.34

6 Residue 13.88

Total 10472.20 Total 10472.20

179

O

Cl O

O

Cl

Cl

Cl

+

Tetra Chloro Phthalic Anhydride (M.Wt. 286)

Quinaldine(M.Wt. 143)

Cl

Cl

Cl

O

OCl

CHN

Solvent Yellow 157

CH3N



Tetra Chloro Phthalic anhydride is reacted with Quinaldine using O-Xylene as a solvent. The

product is isolated using methanol. It is then filtered and washed with water. The wet cake is


Chemical Reaction:

Mass Balance:

Solvent Yellow 157


1 o-Xylene 2472.73 Solvent Yellow 157 1000

2 Tetra Chloro Phthalic

Anhydride

727.27

o-Xylene Recovered 2419.09

3 Quinaldine 443.63 Methanol Recovered 1776.36



6 Residue 21.82

Total 13643.63 Total 13643.63

180

Cl O

2

SHCl

O

+


Thiophenol(M.Wt. 110)

O

SOS

Solvent Yellow 163 (M.Wt. 424)



1:8 Dichloro Anthraquinone is reacted with Thiophenol using n-Butanol as a solvent. The crude

is filtered and purified using 0-Xylene. The product is filtered and washed with water. The wet

cake is dried and pulverized to get the finished product.

Chemical Reaction:

Mass Balance:

Solvent Yellow 163


1 n-Butanol 2946.43 Solvent Yellow 163 1000

2 1:8 DCAQ 678.57 n-Butanol Recovered 2911.43

3 Potassium Carbonate 401.78 o-Xylene Recovered 1735.42

4 Thiophenol 535.71 Effluent 10265.64

5 o-Xylene 1785.71 Loss on drying 250.00


Total 16169.63 Total 16169.63

181

OH

NH2

SO2CH3

2-Amino Phenol 4-N-Methyl Sulfone (M.Wt. 187)

1. Diazotization

2. Coupling m-Chloro DMP

3. Chromination

CN

N C

CH

CH3

OH

(M.Wt. 208.5)

CH3

CN

N C

CH

Cl

Cl

N N

SO2CH3

O

Cr

O


O

CN

N C

C

O

N N

SO2CH3

Cl

CH3



2 Amino Phenyl Methyl Sulfone is diazotized and coupled with m-Chloro PMP. It is then

metalized, filtered and washed with water. The wet cake is dried and pulverized to get the

finished product.

Chemical Reaction:

182

Mass Balance:

Solvent Orange 58


1 APMS 420 Solvent Orange 58 1000

2 HCl 466.66 Effluent 49346.7

3 Sodium Nitrite 160 Loss on drying 1500

4 Caustic soda 233

5 m-Cl PMP 500


7 Water + Ice 50000

Total 51846.7 Total 51846.7

183

N

O

SO3H

N CN

N C

CH

OH

Phenyl Methyl Pyrazolone (PMP) (M.Wt. 174)

Diazo Acid(M.Wt. 250)

1. Chromination

2. Co Precipitation with Rhodamine

3. Condensation with Primene (M.Wt. 200)

Solvent Red 127

CH3

N N

O

C N

NC

C

O

O

Cr

O

SO3HNN

CN

N C

C

CH3

Primene

+

Rhodamine

18. Solvent Red 127


Diazo acid is coupled with Phenyl Methyl Pyrazolone. It is metallized and then condensed with

Rhodamine and 2-Ethyl Hexyl Amine. It is then filtered and washed with water. The wet cake is


Chemical Reaction:

184

Mass Balance:

Solvent Red 127


1 Diazo Acid 250 Solvent Red 127 1000

2 PMP 187.5 Effluent 61265

3 Caustic soda 150 Loss on drying 1500

4 Chrominating Agent 35


6 Rhodamine 500

7 2-EHA 110

8 Water 62500


185

OH

NH2

NO2

O2N

OH

NH2

4-Nitro, 2-Aminophenol (M.Wt. 154)

5-NItro 2-Aminophenol (M.Wt. 154)

1. Diazotization

2. Coupling with B-Napthol (M.Wt. 144)

OH

3. Chromination

4. 2-Ethyl Hexylamine (M.Wt. 129)

N

O

Cr

NO2N

O

NN

O

O

NO2

CH3

CH C2H5

(CH2)4

NH2

Solvent Black 27

19. Solvent Black 27


Mixture of 4 NAP & 5 NAP is diazotized and coupled with B-Naphthol. It is then chrominated. It

is then condensed with 2-Ethyl Hexyl Amine. The product is filtered and washed with water.

The wet cake is dried and pulverized to get the finished product.

Chemical Reaction:

186

Mass Balance:

Solvent Black 27


1 4 NAP 217.5 SOLVENT BLACK27 1000

2 5 NAP 217.5 EFFLUENT STEAM 52185

3 SODIUM NITRITE 185 LOSS ON DRYING 1500

4 HCl 535

5 WATER 52500

6 B-NAPHTHOL 402.5

7 CAUSTIC SODA 100

8 CHROMINATING AGENT 65

9 2-ETHYL HEXYL AMINE 127.5

10 SALICYLIC ACID 335


187

Dyes Intermediates:

1. H Acid


The process steps involve Sulphonation, Nitration, Neutralization, Filtration, Reduction,

concentration, Autoclaving and Isolation.

(a) Sulphonation: Naphthalene is charged in the cast iron sulphonator and sulphuric acid with

oleum is charged at low temperature to have reaction with monohydrated acid. The reaction

mass is then heated to 170 degree centigrade and 65% oleum is charged. The temperature is

maintained for about 3 hours. On completion of the reaction it is taken for nitration.

(b) Nitration: Nitration is carried out in CI vessels. The sulphonated mass is reacted with Nitric

acid at controlled temperature. The mass is then taken to neutralizer.

(c) Neutralization: This reaction is carried out in a MSRL brick lined vessel. The excess acid is

reacted with limestone to get gypsum.

(d) Filtration: The gypsum is then precipitated out and separated in horizontal vacuum filter

and is thoroughly washed with water.

(e) Reduction: The nitro mass thus obtained is reduced to amino compound by iron powder

and HCL in hot condition.

After completion of the reaction the mass is filtered to remove iron oxide sludge.

(f) Concentration: The amino solution is concentrated in the multiple effect evaporators to a

desired level for hydrolysis.

(g) Autoclaving: The concentrated mass is hydrolyzed under pressure of 6-7 kg/cm2 with

caustic soda at a temperature of 170 degree centigrade.

(h) Isolation: The hydrolyzed product obtained from the autoclave is reacted with Sulphuric

acid or HCL for an acidic p H of about 2.Hacid is thereby precipitated and filtered through

vacuum filters and washed to obtain wet cake of H acid. The wet cake is finally dried to get the

product.

188

Chemical Reaction:

190

2. J Acid


Tobias Acid is sulphonated by 23% Oleum, hydrolyzed by water and the wet cake is autoclaved

with caustic flakes. After autoclaving the mass is isolated with the help of 98% H2SO4. It is then

filtered, centrifuged and dried to obtain J acid.

Chemical Reaction:

191

Mass Balance:

192

Mass Balance:

Input Qty (Kg) Output Qty (Kg)

Tobias 1389 Product 1000

Oleum 23% 4243 Spent Acid 8750

Caustic Flake 958 Effluent 13055

Caustic Lye 625

H2SO4 98% 1563

Water 14028


193

3. 6-Nitro, 1-Diazo, 2-Napthol, 4-Sulphonic Acid


First of all takes water 500 lit. Then we add caustic lye 400 kgs. Heats upto 60c. Then we charge

b- Naphthol 1000 kgs. Add into reduce temp. upto 0c is block approx.- 25 Blanks. Then we

charge sodium nitrite 500 kgs. Then we charge sulphuric acid 500 kgs. Then charge sodium-bi-

sulphide 2000 kgs. Then salt 500 kgs. Then again sulphuric acid 1000 kgs.

Then discharge in Nutch. After filter take we take in vessel. Add sodium nitrite 300 kgs. Filter in

filter press isolate with sulphuric acid 500 kgs. Filter in nutch centrifuge that is 1-diazo.

Take oleum 23% 1000 kgs charge above 1-diazo. Then cool to 0 to 10c by chilling plant. Charged

nitric acid 500 kgs. dumped in 20 block ice. Filter in nutch centrifuge wet cane in 6-Nitro, 1-

Diazo, 2-Napthol, 4-Sulphonic Acid.

194

Mass Balance:


β-Napthol 833.33 Product 1000

Caustic Lye 333.33 Effluent 4166.70

Sodium Nitrate 666.67 Process Sludge 833.30

Sulphuric Acid 833.33

Sodium-bi-Sulphite 1666.67

Oleum-23% 833.33

Nitric Acid-70% 416.67

Salt 416.67


195

4. Vinyl Sulphone


Acetanilide is charged into chlorosulphonic acid below 30 degree centigrade. After the addition

the temperature is raised to 50-55 degree centigrade and maintained for 4 hrs. It is cooled and

drowned over ice and filtered. The acetyl sulphochloride is charged into a slurry of sodium

bisulphate and made neutral with caustic and the pH is maintained at 7. Eyhylene oxide is

passed into the solution maintaining pH 7 by adding H2SO4. When the reaction is complete, it is

filtered and dried .It is further clarified by heating with calculated quantity of H2SO4 and then

pulverized. The final product is packed as Para base Vinyl Sulphone.

Chemical Reaction:

196

Mass Balance:

197

NH2

HSO3

Cl

Cl

2:5 DCASA

NaNO2

HCl

N=NCl

HSO3

Cl

Cl

SBS

Soda Ash

Cl

Cl

NH-NHSO3NH

HSO3

HCl

NHNH2

HSO3

Cl

Cl

MAA

NH-N=C-CH3COCH3

Cl

Cl

HSO3

HCl

N

N=C-CH3

C

CH2

O

Cl

Cl

HSO3

2:5 DCSPMP

5. Pyrazolones

a. 2:5 Dichloro 4 Sulpho Phenyl 3 Methyl 5 Pyrazolone


• Take water and oleum in the vessel and then add slowly 2.5 Dichloro Aniline.

• Then diazotize it with sodium nitrite at 0˚C.

• Pour diazo for neutral reduction into solution of SBS and soda ash.

• Heat at 80˚C and carry out hydrolysis by HCl.

• Then do formation of hydrazine with M.A.A Ester.

• Then isolation with HCl.

• Then cool it down and filter out the material.

Chemical Reaction:

198

Mass Balance:

2:5 DICHLORO 4 SULPHO PHENYL 3 METHYL 5 PYRAZOLONE

Sr. No. Inlet Kgs Outlet Kgs

1 2.5 Dichloro Aniline 700 2:5 Dichloro 4 Sulpho Phenyl 3

Methyl 5 Pyrazolone 1400

2 Oleum 2250 Waste Water to ETP 16560

3 NaNO2 310 SO2 585

4 Soda Ash 700

5 SBS 975

6 Caustic Soda Lye 1000

7 H2SO4 1150

8 Ester 475

9 HCL 1550

10 Water + Ice 9435


199

NH2

Cl

HSO3

6 CMA

NaNO2

HCl

Cl

HSO3

N=NCl

Soda Ash

SBS

Cl

NH-NHSO3NH

HSO3

HCl

NHNH2

Cl

HSO3

MAA

NH-N=C-CH3COCH3

Cl

HSO3

HCl

N

N=C-CH3

C-CH2

O

CL

HSO3

OCSPMP

b. 2 Chloro 5 Sulphophenyl 3 Methyl 5 Pyrazolone


• Take water and oleum in the vessel and then add slowly 6 Chloro Metanilic Acid.





• Then isolation with HCL.


Chemical Reaction:

200

Mass Balance:

2 CHLORO 5 SULPHO PHENYL 3 METHYL 5 PYRAZOLONE

Sr.

No. Inlet Kgs Outlet Kgs

1 6 Chloro Metanilic Acid 750 2 Chloro 5 Sulpho Phenyl 3 Methyl

5 Pyrazolone (900 Kgs 100%) 1060

2 NaNO2 265 Waste Water 9135

3 Soda Ash 850 SO2 690

4 SBS 1150

5 Ester 420

6 Caustic Soda Lye 450

7 HCL 4400

8 Water + Ice 2600

10885 10885

201

NH2

HSO3

NaNO2

HCl

HSO3

N=NCl

Soda Ash

SBS

NH-NHSO3NH

HSO3

HCl

NHNH2

HSO3

MAA

NH-N=C-CH3COCH3

HSO3

HCl

N

N=C-CH3

C-CH2

O

HSO3

1:3 SPMP

c. 1,3 Sulpho Phenyl 3 Methyl 5 Pyrazolone


• Take water and oleum in the vessel and then add slowly Metanilic Acid.







Chemical Reaction:

202

Mass Balance:

1,3 SULPHO PHENYL 3 METHYL 5 PYRAZOLONE

Sr.


1 Metanilic Acid 750 1,3 Sulpho Phenyl 3 Methyl 5

Pyrazolone (1000 Kgs 100%) 1400


3 Soda Ash 1450 SO2 675

4 SBS 1125

5 Ester 485

6 HCL 4400

7 Water + Ice 2600

11115 11115

203

NH2

HSO3

NaNO2

HCl

HSO3

N=NCl

Soda Ash

SBS

NH-NHSO3NH

HSO3

HCl

NHNH2

HSO3

MAA

NH-N=C-CH3COCH3

HSO3

HCl

N

N=C-CH3

C-CH2

O

HSO3

1:4 SPMP

d. 1,4 Sulpho Phenyl 3 Methyl 5 Pyrazolone


• Take water and oleum in the vessel and then add slowly S. Acid.








Chemical Reaction:

204

Mass Balance:

1,4 SULPHO PHENYL 3 METHYL 5 PYRAZOLONE

Sr.


1 S. Acid 750 1, 4 Sulpho Phenyl 3 Methyl 5

Pyrazolone (1000 Kgs 100%) 1400


3 Soda Ash 1450 SO2 675

4 SBS 1125

5 Ester 485

6 HCL 4400

7 Water + Ice 2600

11115 11115

205

NH2

NaNO2

HCl

N=NCl

Soda Ash

SBS

NH-NHSO3NH

HCl

NHNH2

MAA

NH-N=C-CH3COCH3

HCl

N

N=C-CH3

C-CH2

O

PMP

e. 1:3 Phenyl Methyl 5 Pyrazolone


• Take water and oleum in the vessel and then add slowly Aniline.







Chemical Reaction:

206

Mass Balance:

1:3 PHENYL METHYL 5 PYRAZOLONE

Sr.


1 Aniline 500 1:3 Phenyl Methyl 5 Pyrazolone

(875 Kgs 100%) 1150

2 NaNO2 378 Waste Water to ETP 11376

3 Soda Ash 1798 SO2 800

4 SBS 1333

5 Ester 601

6 HCL 5456

7 Water + Ice 3260

13326 13326

207

Pigments:

1. Active CPC Blue


CPC Blue Crude is to be charged in the ball mill. Where sheering, hammering and grinding

process occurs and as a result finest particles of Activated CPC Blue is obtained, which is called

Activated CPC Blue. In this process no chemical process or reaction is involved but it is a

physical process by which desired particles shape and size are attained. In this way, after the

physical process, such obtained Activated CPC Blue is to be discharged from the grinding mill

and packed in HDPE Bags/Drums.

Chemical reaction:

Mass Balance:


CPC Blue Crude 1000.0 Activated CPC Blue 1000

Total 1000.0 1000.0

208

2. CPC Blue


Phthalic Anhydride, Urea and solvent (TCB/NB/ONT) are mixed in the vessel equipped with

heating arrangement (by Thermopack Boiler for circulation of high temperature oil) and stirrer.

Cuprous Chloride and ammonium Molybdate are then added.

The mixture is heated up slowly for 20 hours at 180 C temperatures. Ammonia gas and carbon

dioxide gas is liberated with the formation of Phtahlamide at 135 C temp. Formation of Copper

phthalocyanine takes place at a temp. 185 C with release of Ammonia gas & carbon dioxide gas.

The Ammonia gas & carbon dioxide gas is scrubbed through series of scrubbers under water

circulation. The reaction mass is stirred till formation of Copper Pthalocyanine is completed.

The reaction mass is then transferred to rotary vacuum drier and solvent is recovered

completely under vacuum from rotary drier. The dried powder of Copper phthalocyanine is

then purified in MSRL brick lined vessel by treating it with acidic effluent (diluted sulphuric Acid)

generated during manufacture of pigment Apha Blue. The resulting mixture is filtered in filter

press and wet cake is washed with either the effluent generated during Beta Blue manufacture

and finally with fresh water till the soluble Salt are removed. Filtrate is transferred to ETP for

treatment, while the wet press cake of CPC Blue is dried in tray dryer/spin flash dryer,

pulverized and packed into HDPE bags.

Chemical reaction:

209

Mass Balance:

210

3. Alpha Blue (15:0 and 15:1)


Acid Pasting:

Receive 70% sulphuric acid in glass line vessel,cool sulphuric acid. add copper phthalocyanine.

Maintain temperature as per requirement.stirring is done for 4 hours, drown in water.

Filtration:

Filter above material in pp filter press,wash with water till neutral pH.

Pigmentation:

Charge acid free press cake in treatment vessel with required quantity of water, take pH 8-8.5

with caustic & add Tri-Lauryl ammonium sulphate ( Emulsifire) Now increase temperature to

90°c.maintain temperature for 4 hrs.

Filtration:

Filter material in pp filter press, wash with water properly till desired conductivity.

Drying:

Dry above cake in spin flash dryer or Tray dryer as per requirement.

Pulverising:

If material is tray dry then pulverise on micro pulveriser & collect in poly propylene bag.

Blending:

Take dry finished alpha blue powder as per quality requirement for mixing and blend powder

for atleast 2 hours in blender for proper mixing.

Chemical Reaction:

211

Mass Balance:

212

4. Pigment Beta Blue (15:3)


CPC Blue crude is used for manufacturing of Beta blue. It is taken into ball mil for grinding.

Here the particle size of the material gets reduced. The grinded material is taken into the

reactor with caustic Flakes. Caustic flakes are used to get alkaline pH.

The alkaline pH results in better dispersion of particles for pigmentation. The mass is refluxed

for pigmentation. Here the color of the material gets enhanced due to fine tuning with xylene /

IBA.

After completion of reflux, the mass is distilled for recovery of xylene / IBA. After recovery of

xylene / IBA, the mass is neutralized with hydrochloric acid to increase the particle size of beta

blue.

The whole mass is washed and filtered in filter press and washed with water properly till

desired conductivity.

Wet cake from filter press is dried in dryer / SFD. Dried cake is the pulverized and packed for

dispatch.

Chemical Reaction:

213

Mass Balance:

214

5. Pigment Beta Blue (15:4)


CPC blue crude is used for manufacturing of Beta blue. It is taken into ball mil for grinding. Here

the praticle size of the material gets reduced. The grinded material is taken into the reactor

with caustic Flakes, add-1, add-2, sulpho CPC & wood rosin with xylene solvent. The alkaline pH

results in better dispersion of particles for pigmentation. The mass is refluxed for pigmentation.

Here the colour of the material gets enhanced due to fine tuning with xylene.

This is only a physical process and does not involve any chemical reaction. After completion of

reflux, the mass is distilled for recovery of xylene. After recovery of xylene, the mass is

neutralized with hydrochloric acid to increase the particle size of beta belue. The whole mass is

filtered and washed in filter press. Wet cake from filter press is dried in dryer/SFD. Dried cake is

the pulverized and packed for dispatch.

Chemical Reaction:

215

Mass Balance:

216

6. Copper Phthalocyanine Pigment Green-7


Chlorination:

In a glass line vessel Aluminum chloride, vacuum salt, cupric chloride are collected then copper

phthalocyanine blue is added & continue chlorination is done by maintaining temperature as

per requirement. Remove sample & check end point; stop chlorination & drown in process

water. From this process by product HCL gas is generated which is scrubbed.

Filtration:

Above materialism filtered in pp filter press, and washed with water till filtrate is aluminum

free.

Pigmentation (Distillation):

Aluminum free press cake is charged in treatment vessel with required quantity of water, take

pH 12-12.5 with caustic & add oleic acid (Emulsifier) Now increase temperature to continue

reflux for 12hrs. Complete distillation & filter batch.

Filtration:

The material is filtered in pp filter press and washed with water properly till desired

conductivity.

Drying:

Above cake is dried in spin flash dryer or Tray dryer as per requirement.

Pulverizing:

If material is tray dry then pulverize on micro pulverized & collect in poly propylene bag.

Blending:

Take dry finished powder as per quality requirement for mixing and blend powder for least 2

hours in blender for proper mixing.

Chemical Reaction:

217

Mass Balance:

219

7. Pigment Violet 23


Ethylation:

Ethylation of Carbazole (Di- Benzo Pyrole) is carried out in Mono Chloro Benzene on solvent and

Di Ethyl Sulfate in ethylating agent in presence of Alkali. This step will give slurry of Ethyl

Carbazole. Reaction Temp. is 30º C to 130ºC.

Nitration:

Nitration of above slurry is carried out in Mon Cjloro Benzene media on solvent and dilute Nitro

Acid as nitrating agent. This step will give wet cake of Nitro cabazole, Reaction Temp os 25 º C -

75 º C.

Reduction:

Reduction of above wet cake is carried out in Ortho Di Chloro Benzene media and Solvent and

Hydrogen gas and Raney Nikel as reducing agent. After neutralization and filtration of above

reduced mass slurry will get reduction mass mother Liquor. This step will give Amlno Ethyl

Carbazole as mother liquor. Reaction Temp. is 25 º C - 95 º C.

Condensation and Cyclisation:

Above mother liquor is condensed with Chloronil and Sodium Acetate is used as Acid Binding

Agent. At high temp. and in presence of Benzene Sulfonil Chloride above condensed mass will

cyclised. After hot filtration, Methanol and hot water washing will get crude Pigment Violet 23

will get Crude Pigment Violet 23 Reaction Temp is 5 º C to 85 º C.

Pigmentation:

Above dry crude is grinded in kneader with salt in presence of Diethylation glycol will give cake

of kneading mass.

Acid Treatment:

Make slurry of above cake in hot water and hydrochloric acid. After filtration and hot water

washing will give wet cake of Pigment Violet 23.

Drying:

After drying of above wet cake in Spin Flash or Tray Dryer will give powder form of Pigment

Violet 23.

220

Chemical Reaction:

221

Mass Balance:

224

8. Pigment Red 122


Condensation:

DMSS condensed with peratoludine & HCl in present of methanol this step will give wet cake

reaction temperature 30 degree centigrade to 80 degree centigrade.

Oxidattion:

Above wetcake oxidize with R. salt, caustic flakes in present of methanol & filter it this step will

give slurry & this slurry isolate with HCl & filter it & washed it & dry it. Reaction temperature 30

degree centigrade to 90 degree centigrade.

Cyclisation:

Above dry materials cyclised with (P2O5 + H3PO4) PPA (poly phoshphoric acid) & drowing in

MSRL BL & Filter it & washed it & unload wet cake reaction temperature 30 degree centigrade

to 150 degree centigrade.

Pigmentation:

Above wet cake pigmentation with IBA + water & recovered IBA & Filter it & dry it. It is pigment

red-122 reaction temperature 30 degree centigrade to 120 degree centigrade.

225

Chemical Reaction:

226

Mass Balance:

229

9. Pigment Violet 19


Condensation:

DMSS condensed with Aniline & HCL in present of Methanol this step will give Wet cake

Reaction temperature 30ºC to 80ºC.

Oxidation:

Above Wet cake oxidize with R. salt, Caustic Flakes in present of Methanol & filter it this step

will give Slurry & this slurry Isolate with HCL & Filter it & washed it & Dry it. Reaction

temperature 30ºC to 90ºC.

Cyclisation:

Above Dry materials cyclised with (P2O5 + H3Po4) PPA (Poly Phosphoric Acid) & Drawing in

MSRL BL & Filter it & washed it & unload wet cake Reaction Temperature 30ºC to 150ºC.

Pigmentation:

Above Wet cake Pigmentation with IBA + water & recovered IBA & filter it & washed it & Dry it.

It is Pigment Voilet-19 Reaction Temperature 30ºC to 120ºC.

230

Chemical Reaction:

231

Mass Balance:

234

10. Solsperse 5000


Sulphonation:

Charge olieum in CI reactor. Cooled it to 25°C and then slowly charged Copper Pthalocynine

keeping temperature below 35°C. Then heat it to 65-70°C slowly. Then Keep this temperatures

for Six Hours. Check Sulphonation test. Then cool it to 40°C. Then dumped this mass in to

MSRLTL reactor in presence of Ice and keeping temperature below 5°C stir for two hours and

then filtered of in Filter press. Then give washing to W/C till congo +Ve ( 4.0 pH). Unload the

wet Cake.

Condensation:

Make slurry of above wet cake in water and then heat it to 50°C. Stir it well till it becomes

properly mix. Then charge Quaternary Amine slowly keeping temperature 50°C and pH 8.5.

Then Stir it for Four hours. And then filtered it in filter Press. Washed it with DM water till it is

salt free. Then unload it from Filter Press and dry it in Spin Flash Dryer.

Chemical Reaction:

236

Mass Balance:

237

11. Carbazole


Aniline to Phenyl Hydrazine:

Take Aniline in MSRLTL reactor in Presence of Ice and water. Make it diazotized with Kgs

Hydrochloric Acid and Sodium Nitrite. Check and confirm Diazotization by Confirmative test

with SI Paper. Then make Sodium Sulphite Solution in presence of Caustic Lye and charge it in

above Diazo Mass. Then Heat it to 60°C till the reaction complete. Then acidify it with

Hydrochloric Acid. And then filter it as W/C.

Phenyl Hydrazine to Tetra Hydro Carbazole

Take Cyclohexenon in SS reactor and heat it to reflux. Add of Acetic acid and again reflux it.

Then slowly charged Phenyl Hydrazine and then again reflux it for two hours. Then cool it to

room temperature and filter it in Filter Press and washed it with water. Then dumped the filter

Press and dried it in tray dryer.

Tetra Hydro Carbazole To Carbazole

Take Tetra Hydro carbazole in SS reactor and the charge Raney Nickel as catalyst. Then heat it

and maintain the temperature for 6 Hours and then dumped reaction mass in water. Then Filter

of Carbazole. And purify it with Acetone.

Chemical Reaction:

238

Mass Balance:

240

Speciality Chemicals:

1. 2,4 – Dichloro Phenyl Acetic Acid


2,4-Dichlorobenzyl chloride is reacted with Sodium cyanide to make 2,4-Dichlorobenzyl

cyanide.

2,4-Dichlorobenzyl cyanide is then hydrolyzed with caustic soda to make 2,4-

Dichlorophenylacetic acid.

Chemical Reaction:

241

Mass Balance:

242

2. 2,4 – Dichloro Phenyl Acetyl Chloride


2,4-Dichlorophenyl acetic acid is chlorinated with Thionyl chloride, using toluene as solvent to

convert it to 2,4-Dichlorophenyl acetyl chloride. The product is isolated after recovery of

toluene by doing high vacuum distillation and pure product is collected separately.

Chemical Reaction:

Mass Balance:

243

3. 2,4,6-Trimethyl Phenyl Acetyl Chloride


2,4,6-Trimethylphenyl acetic acid is chlorinated with thionyl chloride to convert it to 2,4,6-

Trimethylphenyl acetyl chloride using Toluene as solvent.

Chemical Reaction:

Mass Balance:

244

4. 2,3,4,5 - Tertrachloro Benzoyl Chloride


2,3,4,5-Tetrachloro phthalic anhydride is hydrolyzed with caustic flakes to 3,4,5,6- Tetrachloro

phthalic acid which is decarboxylate to make 2,3,4,5-Tetrachloro benzoic acid .This benzoic acid

is then reacted with thionyl chloride to make 2,3,4,5-Tetrachloro benzoyl chloride (TCBOC).

Chemical Reaction:

245

Mass Balance:

246

5. 3,4,5 Trimethoxy Benzyl Chloride


3,4,5 Trimethoxy benzyl alcohol is reacted with HCl to produce pure 3,4,5 Trimethoxy benzyl

chloride.

Chemical Reaction:

Mass Balance:

247

Pesticide Intermediates:

1. 2-Amino Benzo Nitrile


2-Amino-benzamide is dehydrated with phosphorus pentachloride. After reaction completion,

reaction mixture was quenched in water and pH was adjusted up to 6.5-8.5 Separate the

organic layer, Product was distilled off under reduce pressure after distillation of solvent.

Chemical Reaction:

Mass Balance:

248

2. 2-Amino-5-Bromo Benzo Nitrile


2-Amino-benzonitrile is brominated with N-bromosuccinimide in presence of solvent DMF.

After reaction completion, DMF is recovered, added water and filter the crude product. Crude

product was crystallized with toluene to get the pure material.

Chemical Reaction:

249

Mass Balance:

250

3. 2,4,6 - Trimethyl Benzaldehyde (Mesitaladehyde)


Chloral and mesitylene are reacted in presence of Titanium chloride.Product obtained is

isolated after quenching ,mass is hydrolyzed with soda ash to make product mesiatldehyde.

Distilled mesitsldehyde is mixed with acetone to get 84 % concentration.

Chemical Reaction:

251

Mass Balance:

252

4. Indoline


2-Chlororphenethyl amine is reacted with aq. ammonia in autoclave with presence of Copper

chloride to produce indoline. After washing this crude mass is distilled under reduced pressure

to get pure Indoline.

Chemical Reaction:

Mass Balance:

253

5. 5-(1-Carboxy Ethyl)-2-(Phenylthio) phenyl Acetic Acid (DIACID)


2-Phenylthio-5-propionyl phenyl acetic acid (PPP) interacts with bromine, Trimethyl

Orthoformate (TMOF) in presence of Zn to produce Diester, then Diester hydrolise with help

sodium hydroxide flakes then acidified with acid to produce Diacid.

Chemical Reaction:

254

Mass Balance:

255

ANNEXURE: 4

WATER CONSUMPTION AND WASTE WATER GENERATION

Sr.

No.

Category Proposed Scenario (KL/Day)

Water Consumption Waste Water Generation

1. Industrial

Process 987 974

Boiler 100 03

Cooling 68 01

Washing 04 03

Total (Industrial) 1159 981

2. Gardening 10 00

3. Domestic 15 12

Total 1184 994

256

Water Balance Diagram:

974 KL/Day 03 KL/Day 01 KL/Day 03 KL/Day

925 KL/Day

49 KL/Day

MEE Salt

* SS & MEE = Solvent Stripper & Multiple Effect Evaporator

Raw Water

1184 KL/Day

Domestic:

15 KL/Day

Washing:

04 KL/Day

Effluent Treatment Plant

932 KL/Day

Gardening:

10 KL/Day

SS & MEE*:

331 KL/Day

Industrial:

1159 KL/Day

Cooling:

68 KL/Day

Boiler:

100 KL/Day

Process:

987 KL/Day

To Septic Tank/

Soak Pit Tank:

12 KL/Day

RO Treated -

650 KL/Day

RO Reject -

282 KL/Day

MEE

Condensate -

280 KL/Day

ATFD

257

ANNEXURE: 5

DESCRIPTION OF EFFLUENT TREATMENT PLANT AND MEE SYSTEM

PROCESS DESCRIPTION: ETP (EFFLUENT TREATMENT PLANT)

PROCESS DESCRIPTION:

Low COD Stream

1) The low COD stream (932 KLD) shall be passed through Screen Chamber (SC) where manual

screen (S) shall be provided to remove floating material. Then effluent shall be collected in

Collection cum Equalization Tank-1 (CET-1). Pipe grid is provided at bottom of the CET-1 to

keep all suspended solids in suspension and to provide proper mixing. 2 nos. of Air Blowers

(B-01) shall supply air through diffusers to pipe grid.

2) Then after, equalized wastewater shall be pumped to Neutralization Tank-1 (NT-1) where

the continuous addition and stirring of Lime solution is done (to maintain neutral pH of

wastewater) from Lime Dosing Tanks (LDTs) as per requirement. Then after, neutralized

wastewater shall go to Flash Mixer-1 (FM-1). Alum & Poly shall be dosed from Alum Dosing

Tank (ADT) and Poly Dosing Tank (PDT) respectively by gravity into FM-01 to carry out and

flocculation by using a Flash Mixer-1. Then effluent shall be sent to Primary Clarifier (PCL)

where coagulated wastewater shall be settled. Clear supernatant from Primary Clarifier

shall be passed in Aeration Tank-01 (AT-01).

3) Here, Biodegradation of organic matter of the wastewater shall be carried out by bacteria

(suspended growth) in the AT-1. The aeration tank provides proper mixing and supplies

oxygen to the microorganisms in the dissolved form through the fine bubble diffusers. A

constant feed rate shall be maintained in the aeration tank. A sludge percentage of around

25 to 30 % by volume shall be maintained in the aeration tank. Also MLSS and MLVSS ratio

shall be maintained to ensure active microorganisms growth. Various nutrients like Urea

and DAP shall be added from Nutrient Dosing Tanks (NDTs) regularly so as to ensure proper

growth of the microorganisms. Oxygen shall be supplied by 2 nos. of air blowers (B-02)

through diffusers. Air blowers also keep MLSS in suspension.

258

4) Then the overflow of the Aeration Tank-1 shall be diverted into the Secondary Clarifier-1

(SCL-1) for biomass separation. An appropriate retention time is given to the effluent to

ensure proper settling. The sludge settles down into the bottom of the SCL-1 and required

amount of settled sludge shall be recycled back into the aeration tank-1 to maintain desired

concentration of biomass. Excess biomass shall be pumped to sludge sump (SS).

5) Then after, overflow (clear supernatant) of SCL-1 shall be sent to Aeration Tank-2 (AT-2).

Here, again biodegradation of left out organic matter of the wastewater shall be carried out

by bacteria (suspended growth) in the AT-2 and for that oxygen shall be supplied by two

nos. of blowers (B-03) with help of diffusers. Then after, wastewater shall go to Secondary

Clarifier-2 (SCL-2) from AT-2. Here, the suspended solids shall be settled. Activated sludge

shall be removed from bottom of SCL-2 and pumped to AT-2 to maintain MLSS and

remaining will be sent to SS. Nutrients will be added from NDTs to Aeration Tank-2 for

growth of Bacteria if require.

6) Then after, overflow (clear supernatant) of SCL-2 shall be collected in Intermediate Sump

(IS). Then effluent from the IS-1 shall be passed through Multi Grain Filter (MGF) and

Activated Carbon Filter (ACF) to remove SS and other impurities. Filter water is collected to

RO Feed Tank (RFT) and then pumped to RO Unit (large capacity) for further treatment.

Treated water from RO will collected in RO Treated Water Tank (ROTWT-1) and will be

reuse in process. RO reject will be sent to MEE Feed Tank (MFT) for further treatment.

7) The primary and secondary sludge from the sludge sump shall be pumped to the Filter

Presses (FP-01-A/B) for sludge dewatering. We will provide two nos. Filter presses to use

alternately. The sludge cake shall be collected and packed into the plastic bags and stored

in the HWSA for ultimate disposal to TSDF. The leachate from the FP-01-A/B shall be

collected in Drain Pit and then pumped back to collection cum equalization tank (CET-01)

for further treatment.

259

High TDS Stream

1) The high TDS (49 KLD) stream shall be collected in Collection cum Equalization Tank-2 (CET-

2). Pipe grid is provided at bottom of the CET-2 to keep all suspended solids in suspension

and to provide proper mixing. 2 nos. of Air Blowers (B-04) shall supply air through diffusers

to pipe grid.

2) Then after, equalized wastewater shall be pumped to Neutralization Tank-2 (NT-2) where

the continuous addition and stirring of Lime solution is done (to maintain neutral pH of

wastewater) from Lime Dosing Tanks-1 (LDTs-01) as per requirement by gravity. Then after,

neutralized wastewater shall go to Flash Mixer-2 (FM-2). Alum and poly shall be dosed from

Alum Dosing Tank -1(ADT-01) and Poly Dosing Tank (PDT) by gravity into FM-2 to carry out

coagulation by using a Flash Mixer. Then after, coagulated wastewater shall be settled in

Primary Tube Settler (PTS). Sludge settled at bottom shall be sent to Sludge Sump.

3) Clear supernatant from Primary Tube Settler (PTS) shall be collected in Holding Tank (HT).

Then effluent shall be pumped to Stripper (S) for removal of solvent. After that effluent

shall collected in MEE Feed Tank (MFT) where RO reject water shall be mixed with it. Then

effluent shall be sent to four stages Evaporator (MEE). Condensate from MEE shall be

collected in Condensate Tank and then reuse in washing. Solid from Agitated Thin Film

Dryer (ATFD-01) shall be collected and stored in HWSA for ultimate disposal to TSDF.

260

ETP Units (for Low COD Stream) Q= 932 m3/day

Sr.

No.

Name of Unit Nos. Size of Tanks

L x B x D(LD+FB) In m

MOC

1 Screen Chamber (SC) 1 3.5 x2.0 x (0.05+0.5) RCC M25 with A-A Bk. Lining

2 Collection Cum Equalization

Tanks-1 (CETs-1)

1 12.0 x7.8 x (2.5+0.7) RCC M25 with A-A Bk. Lining

3 Neutralization Tank-01 (NT-01) 1 3.0 x 3.0 x (3.5+0.5) RCC M25 with A-A Bk. Lining

4 Flash Mixer-1 (FM-1) 1 3.0 x 3.0 x (3.5+0.7) RCC M25

5 Primary Clarifier (PCL) 1 9.0 dia x (3.5 +0.5) RCC M25

6 Aeration Tank -1(AT-1) 1 24.0 x 13.0 x (4.5+0.5) RCC M25

7 Secondary Clarifier-1 (SCL-1) 1 9.5 dia x (3.5 +0.5) RCC M25

8 Aeration Tank-2 (AT-2) 1 17.0 x 13.0x (4.5+0.5) RCC M25

9 Secondary Clarifier-2 (SCL-2) 1 9.0 dia x (3.5 +0.5) RCC M25

10 Intermediate Sump (IS) 1 6.0 x 4.3 x (3.0+0.5) RCC M25

11 Multi Grain Filter (MGF) 1 48 m3/day MSEP

12 Activated Carbon Filter (ACF) 1 48 m3/day MSEP

13 RO Feed Tank (RFT) 1 12.0 x 7.8 x (2.5+0.5) RCC M25

14 UF & RO Unit (RO) 1 46 m3/hr SS

15 Sludge Sump (SS) 1 6.0 x 4.3 x (3.0+0.5) RCC M25

16 Drain Pit(DT) 1 2.0 x 2.0x (2.0+0.5) RCC M25

17 Filter Press(FP) 2 75 m3/day PP

18 Lime Dosing Tanks (LDTs) 2 2000 lit HDPE

19 Alum Dosing Tank (ADT) 1 1500 lit HDPE

20 Poly Dosing Tank (PDT) 1 1000 lit HDPE

21 Nutrient Dosing Tanks (NDTs) 2 1000 lit HDPE

261

ETP Units (for High TDS Stream) (49 m3/day)

Sr.

No.

Name of Unit Nos. Size of Tanks

L x B x D(LD+FB) In m

MOC

22 Collection Cum Equalization

Tank-2 (CET-2)

1 4.5 x 2.7 x (2.0+0.5) RCC M25 with A-A Bk. Lining

23 Neutralization Tank-02 (NT-02) 1 1.3 x 1.3 x (1.0+0.5) RCC M25 with A-A Bk. Lining

24 Flash Mixer-2 (FM-2) 1 1.3 x 1.3 x (1.0+0.7) RCC M25

25 Primary Tube Settler (PTS-1) 1 2.5 x 2.0 x (1.5 + 1.0

+0.5)

RCC M25

26 Holding Tank(HT-1) 1 5.0 x 3.0 x (3.0+0.5) RCC M25

27 Stripper (ST-01) 1 50 m3/day SS 316L

28 ME Feed Tank (MFT-01) 1 4.0 x 4.0 x (3.0+0.5) RCC M25

29 Multiple Effect Evaporator

(MEE) with strippers &

Agitated Thin Film Dryer

(ATFD)

1 Set 50 m3/hr SS 316 L

262

Schematic Flow Diagram of Effluent Treatment Plant:

263

MEE SYSTEM

PROCESS DESCRIPTION:

Capacity: 331 KL/Day

Industry has installed Multi Effect Evaporator for the treatment of industrial effluent (as an

additional facility) having capacity of 331 KL/Day. The condensate water generated from the

MEE shall be used in process.

Neutral effluent after salt recovery is passed through three stages evaporator (two falling film +

one forced circulation) and the evaporated water and reuse in plant for is collected in an

Evaporated Water Collection Tank and then recycled to plant after filtering through carbon

filter.

In the first effect 7.0 kg/cm2 steam pressure is used to evaporate water. Evaporated water in

the form of steam of 2.0 kg/cm2 is used to evaporating the effluent in second stage at

atmospheric pressure. Evaporated water from the second stage is used for evaporating waste

water in the third stage under vacuum of 650 to 700 mm Hg. Finally evaporated water from the

third stage is condensed in the steam condenser. Condensate is collected in the recovery tank

which is reuse in the plant process.

Concentrated mass (Organic and Inorganic) is sending for the spray dryer.

Design of MEE:

No. of Effects : 3 (2 Falling Film + 1 Forced Circulation)

Waste Handling Capacity : 49 KL/Day

Feed Rate : 16 KL/Hr

Feed Concentration : 12 % TDS

Feed Temperature : 35 o C

Product Rate : 6400 KL/Hr

Product Concentration : 40 %

Product Temperature : 55-65 o

C

Water Evaporation Rate : 9600 KL/Hr

264

Characteristics of Effluent:

Dilute Stream:

Parameter Untreated

(Dilute

Stream)

After

Primary

Treatment

After

Secondary

Treatment

After

tertiary

Treatment

RO

Permeate

pH 3-10 6.5-8.5 6.5-8.5 6.5-8.5 6.5-8.5

Temperature (o

C) 30 31 30 30 30

COD (mg/L) 9,000 3,200 950 250 34

BOD3

(mg/L) 3,600 2,600 600 200 16

TDS (mg/L) 3,500 3,100 2,900 2,500 140

Suspended Solids

(mg/L)

155 90 60 15 10

Concentrated Stream:

Parameter Untreated

(Concentrated

Stream)

After

Solvent

Stripper

After

Neutralized

Effluent

MEE

Condensate

pH 3-10 5-10 6.5-8.5 6.5-8.5

Temperature (o

C) 32 30 30 30

COD (mg/L) 91,500 68,625 48,625 210

BOD3

(mg/L) 15,200 13,500 11,200 25

TDS (mg/L) 74,000 74,000 71,000 220

265

ANNEXURE: 6

DETAILS OF HAZARDOUS SOLID WASTE MANAGEMENT AND DISPOSAL

Sr.

No.

Type of Hazardous

Waste

Quantity Hazardous

Waste

Category

Storage, Collection & Disposal

1. ETP Sludge 1000 MT/Month

35.3 Collection, Storage, Transportation

& and Disposal to nearest TSDF site

(M/s. SEPL)

2. MEE Salt 400 MT/Month 35.3 Collection, Storage, Transportation


(M/s. SEPL)

3.

Sludge from Wet

Scrubber

50 kg/Month 26.1 Collection, Storage, Transportation


(M/s. SEPL)

4. Distillation Residue 215 MT/Month 36.1 Collection, Storage, Transportation

& co-processing in cement

industries or sent to common

Incineration Site (M/s. SEPPL)

5. Spent Carbon 100 kg/Month 36.2 Collection, Storage, Transportation

& co-processing in cement

industries or sent to common

Incineration Site (M/s. SEPPL)

6.

Iron Sludge 500 MT/Month 26.1 Collection, Storage, Transportation

& Sell to Cement Industries

7. Gypsum Sludge 1700 MT/Month 26.1 Collection, Storage, Transportation

& Sell to Cement Industries

8. Inorganic Salt 300 MT/Month -- Collection, Storage, Transportation

& Disposal to nearest TSDF (M/s.

SEPL)

9. Spent Acid

Dilute HCl

(Pigment Green 7 –

25-28%)

1850 MT/Month

26.3

Will be used in production of Direct

Black 40 (Direct Dyes)

Dilute H2SO4

(Alpha Blue – 25-30%)

4600 MT/Month Will be used in production of H

Acid (Dyes Intermediates) & CPC

Blue (Pigments)

266

Spent Phosphoric Acid

(PV 19 or 122)

1500 MT/Month

Collection, Storage, Transportation

& Sell to end user

Aluminum Chloride

Solution

(PG 7 – 28-30%)

2825 MT/Month

-- Collection, Storage, Transportation

& Sell to end user or used in

making Aluminium Hydroxide

Sodium Hypochlorite

(PG 7 – 10-11%)

1400 MT/Month -- Collection, Storage, Transportation

& Sell to end user

Liq. Ammonia

(Indoline)


& Sell to end user

Ammonium

Carbonate (CPC Blue)


& Sell to end user

Sodium Sulphite 25 MT/Month -- Collection, Storage, Transportation

& Sell to end user

Sodium Acetate 25 MT/Month -- Collection, Storage, Transportation

& Sell to end user

Acetic Acid 70 MT/Month -- Will be used in production of

Solvent Red 195 (Solvent Dyes)

10. Used Oil 0.05 MT/Month 5.1 Collection, Storage, Transportation

& Sell to GPCB registered re-

processor or used for low grade

lubrication of machinery

11. Discarded

Drum/Containers/Car

boys Plastic

bags/Liners

Bags:

400 Nos./Month

Drums:

100 Nos./Month

33.3 Collection, Storage, Transportation,

Decontamination & Sell to GPCB

authorized Vendor

267

ANNEXURE: 7

DETAILS OF FLUE & PROCESS GAS EMISSION

Details of Flue Gas Emission:

Sr.

No.

Stack Attached to Type and

Quantity of fuel

Stack

Height (m)

Stack

Dia. (m)

Pollutant Air Pollution

Control Measures

1 Steam Boiler

IBR (3 TPH)

Coal = 10 MT/Day 30 0.6 PM<150 mg/Nm3

SO2<262 mg/Nm3

NOx<92 mg/Nm3

Water scrubber,

Bag Filter, Multi

Cyclone Separator

2 Steam Boiler

IBR (6 TPH x 2)

Coal = 40 MT/Day 30 0.6 PM<150 mg/Nm3

SO2<262 mg/Nm3

NOx<92 mg/Nm3

Water scrubber,

Bag Filter, Multi

Cyclone Separator

3 Thermic Fluid

Heater (TFH)

(10 kcal/hr x 6)

Diesel = 3 KL/Day 12 0.45 PM<150 mg/Nm3

SO2<262 mg/Nm3

NOx<92 mg/Nm3

--

4 Spin Flash Dryer

(SFD)

(0.75 TPH x 7)


--

5

Spin Flash Dryer

(SFD)

(0.3 TPH x 4)

Diesel = 0.4 KL/Day 15 0.45 PM<150 mg/Nm3

--

6 Spray Dryer

(192 Trays x 5)


--

7 Spray Dryer

(1200 lit/hr x 4)


--

Details of Process Gas Emission:

Sr.

No.

Name of the

process vessel

Stack Height

(m)

Stack Dia.

(m)

Pollutant

Air Pollution

Control Measures

1 Process Vent - 1 15 0.15 SO2<40mg/Nm3 Two Stage Scrubber

2 Process Vent - 2 15 0.15 NH3<175mg/Nm3 Two Stage Scrubber

3 Process Vent - 3 15 0.15 HCl<20 mg/Nm3 Two Stage Scrubber

4 Process Vent - 4 15 0.15 HBr<5mg/Nm3 Two Stage Scrubber

268

ANNEXURE: 8

DETAILS OF HAZARDOUS CHEMICAL STORAGE FACILITY

Sr. No. Hazardous Chemicals Type of Hazard MOC of Storage Actual Size Stored Quantity

1 Hydrocholoric Acid Corrosive HDPE/PPFRP 25 MT

(2 Nos.)

50 MT

2 Sulphuric Acid Corrosive MS Tank 20 MT

(2 Nos.)

40 MT

3 Caustic Soda Lye Corrosive MS Tank 20 MT 20 MT

4 Formaldehyde Flammable MS Tank 20 MT

(2 Nos.)

40 MT

5 Liq. Ammonia Toxic MS Tank 10 MT 10 MT

6 Aniline Corrosive Drums 200 kg

(10 Nos.)

2 MT

7 Methanol Flammable MS Tank 10 MT 10 MT

8 o-Xylene Flammable MS Tank 10 MT 10 MT

9 Acetic Acid Corrosive Drums 200 kg

(15 Nos.)

3 MT

10 Nitric Acid Corrosive Tank 5 MT 5 MT

11 Oleum-23 % Corrosive MS Tank 25 MT

(2 Nos.)

50 MT

12 Toluene Flammable MS Tank 10 MT

(2 Nos.)

20 MT

13 Chlorine Toxic Tonner 900 kg

(05 Nos.)

4.5 MT

14 EDC Flammable MS Tank 20 MT 20 MT

269

ANNEXURE: 9

SOCIO - ECONOMIC IMPACTS

1) EMPLOYMENT OPPORTUNITIES

The manpower requirement for the proposed project is expected to generate some permanent

jobs and secondary jobs for the operation and maintenance of plant. This will increase direct /

indirect employment opportunities and ancillary business development to some extent for the

local population. This phase is expected to create a beneficial impact on the local socio-

economic environment.

2) INDUSTRIES

Required raw materials and skilled and unskilled labors will be utilized maximum from the local

area. The increasing industrial activity will boost the commercial and economical status of the

locality, to some extent.

3) PUBLIC HEALTH

The company regularly examines, inspects and tests its emission from sources to make sure that

the emission is below the permissible limit. Hence, there will not be any significant change in the

status of sanitation and the community health of the area, as sufficient measures have been

taken and proposed under the EMP.

4) TRANSPORTATION AND COMMUNICATION

In brief, as a result of the proposed project there will be no adverse impact on sanitation,

communication and community health, as sufficient measures have been proposed to be taken

under the EMP. The proposed project is not expected to make any significant change in the

existing status of the socio - economic environment of this region.

270

ANNEXURE: 10

PROPOSED DRAFT TERMS OF REFERENCE

1. Project Description

• Justification of project.

• Promoters and their back ground

• Project site location along with site map of 5 km area and site details providing various

industries, surface water bodies, forests etc.

• Project cost

• Project location and Plant layout.

• Water source and utilization including proposed water balance.

• Product spectrum (proposed products along with production capacity) and process

• List of hazardous chemicals.

• Mass balance of each product

• Storage and Transportation of raw materials and products.

2. Description of the Environment and Baseline Data Collection

• Micrometeorological data for wind speed, direction, temperature, humidity and rainfall in 5

km area.

• Existing environmental status Vis a Vis air, water, noise, soil in 5 km area from the project site.

For SPM, RSPM, SO2, NOx.

• Ground water quality at 5 locations within 5 km.

• Complete water balance

3. Socio Economic Data

• Existing socio-economic status, land use pattern and infrastructure facilities available in the

study area were surveyed.

4. Impacts Identification And Mitigatory Measures

• Identification of impacting activities from the proposed project during construction and

operational phase.

• Impact on air and mitigation measures including green belt

• Impact on water environment and mitigation measures

• Soil pollution source and mitigation measures

• Noise generation and control.

• Solid waste quantification and disposal.

5. Environmental Management Plan

• Details of pollution control measures

• Environment management team

• Proposed schedule for environmental monitoring including post project

271

6. Risk Assessment

• Objectives and methodology of risk assessment

• Details on storage facilities

• Process safety, transportation, fire fighting systems, safety features and emergency

capabilities to be adopted.

• Identification of hazards

• Consequence analysis through occurrence & evaluation of incidents

• Disaster Management Plan.

7. Information for Control of Fugitive Emissions

8. Post Project Monitoring Plan for Air, Water, Soil and Noise.

9. Information on Rain Water Harvesting

10. Green Belt Development plan

proposed dyes & dyes intermediates, pigments, speciality chemicals & pesticide...

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