PRE-FEASIBILITY REPORT - Welcome to...

PRE-FEASIBILITY REPORT

M/s Infinium Pharmachem Pvt. Ltd.Plot No:- 37, 38 & 39, GIDC Sojitra,

Dist: ANAND (Gujarat).

Prepared by:

EXCEL ENVIRO TECH(NABET Accredited EIA Consultant Organization)TF-2 , SUN HOUSE,Near Old High CourtOff Ashram Road,Ahmedabad – 380 009Tele-fax: 079–27542219Cell: +91-98255 88910Email: [email protected] : www.excelenviro.com

Synthetic Organic Chemicals 5(f)

INFINIUM PHARMACHEM PVT. LTD Feasibility Report

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TABLE OF CONTENTSCHAPTER 1 INTRODUCTION TO THE PROJECT 21.1 Project PROPONENTs 2CHAPTER 2 PROJECT DESCRIPTION 32.1 Project Location 32.2 Alternate Sites Considered 42.3 Products & Raw Material Details 52.4 Manufacturing Process 92.5 Details of Air Pollution Management 1592.6 Details water and wastewater 1592.7 Utilities Requirement 1602.8 Manpower Requirement 161CHAPTER 3 SITE ANALYSIS 1613.1 Connectivity 1613.2 Existing Landuse Pattern 1613.3 Topography 1613.4 Social Infrastructure Available: 1623.5 Rehabilitation & Resettlement Plan 1623.6 Landuse Breakup 162CHAPTER 4 PROPOSED ENVIRONMENTAL INFRASTRUCTURE 1634.1 Management of Domestic Waste Water 1634.2 Management of Industrial Waste Water 1634.3 Air Quality Management: 1644.4 Solid & Hazardous Waste Management 1644.5 Hazardous Chemicals Details 1654.6 Waste Minimization Measures 165ANNEXURE 166CC&A COPY 166GIDC Letter 171SEPL Certificate 173NECL Certificate(hazardous waste) 174NECL Certificate(Incineration) 175Plant layout 176


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CHAPTER 1

INTRODUCTION TO THE PROJECT

M/s. Infinium Pharmachem Pvt. Ltd is a Small scale unit established in 2009.Infinium pharmachem is India based pharmaceutical intermediatesmanufacturer which is extremely effective, efficient and professionallymanaged organization. The company also undertakes contractmanufacturing for many products. It can give the assurance of timelydelivery, excellent quality and competitive rates. And that is what they callas our core competence at Infinium pharmachem Pvt. Ltd.

They welcome importers, distributors and agents who help to introduceproducts on their national markets Infinium Pharmachem Pvt. Ltd providescomprehensive range of services as well as prompt and reliable assistancefor all their customers around the world Product Range from infiniumpharmachem Pvt. Ltd.

Each and every functional area of organization is led by professionallyqualified people who had thorough understanding and experience into thatparticular area. That is the way how they keep tab on qualitative measuresby qualified people, thoroughly.

1.1 PROJECT PROPONENTSInfinium pharmachem Pvt. Ltd is a Private Limited Company launched byMr. Sanjay V. Patel, Mr. Mitesh Lavajibhai Chiukhaliya & Mr. PravinBhadabhai Madhani. Directors are young, dynamic and enthusiastic to leadthe task towards completeness.

Currently, the managerial team includes 4 administrative and 10 workingstaff. For proposed expansion/diversification activity, more 6 people may getemployed at full capacity production.


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CHAPTER 2

PROJECT DESCRIPTION

2.1 PROJECT LOCATION

The Project is located at coordinates 22o31’48’’N 72o42’55’’E in, GIDC

Sojitra, Ta-Sojitra, Anand. Plot No:37, 38 & 39 about 20.0 km far from

Anand railway station and 55 km far from Vadodara Airport. The Plant is just

600 m away from State Highway (SH-83) that provides a convenient &

competitive trade gateway to domestic market transportation.

Location Of The Project With Surroundings


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2.2 ALTERNATE SITES CONSIDEREDThe company has not considered any alternate site as it already has an

existing plant for manufacturing of Inorganic Iodine Derivatives at the site.

Necessary permissions from State Pollution control Board for the same have

been obtained. The proposed products are value addition to the existing

products (being organic Iodine Derivatives).

As the unit is located in notified area of GIDC, the site is having all required

infrastructure facilities in form of; water, electricity, and Road available for

the existing as well as proposed activities.

Location of site within 500 m Radius


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Location of site within 5-km Radius

2.3 PRODUCTS & RAW MATERIAL DETAILS

Product Details

The Details of existing and proposed products are given in following table:

Inorganic Iodine Derivatives Quantity(MT/Month)

Existing Products

Potassium Iodide 3.464.8041.74

Sodium Iodide

Ammonia Iodide, Copper Iodide,Zinc Iodide, Calcuim Iodate, Potassium Iodate,Sodium Metaper-Iodate


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Proposed ProductsSodium Iodide, Potassium Iodide, Ammonium Iodide,Copper Iodide, Zinc Iodide, Silver Iodide,Calcium Iodate, Pottassium Iodate, Soidum Iodate,Sodium Meta Par Iodate, Lithium Iodide Hydrate,Nickel Iodide, Lead Iodide, Cadmium Iodide,Thallium Iodide, Antimomny Iodide, Hydroiodic Acid,Calcium Iodide Hydrate, Iodine,Iodine Monochloride, Iodine 0.1n Standard Solution,Cesium Iodide,Iodine Monochloride 40% Solution In Acetic Acid,Iodine Monochloride 40% Solution In MDC,Barium Iodide Dihydrate, Iodic Acid (Solution),Iodic Acid (Crystal),Per-Iodic Acid

50 MT/Month(existingProductsincluded)

Organic Iodine Derivatives Quantity(MT/Month)

Iodobenzene Diacetate,Bis Trifluoro Acetoxy Iodobenzene4-Iodobenzoicacid, 3-Iodobenzoic AcidMethyl Tri Phenyl Phosphonium IodideEthyl Tri Phenyl Phosphonium IodideIso Propyl Tri Phenyl Phosphonium Iodide1-Iodohexane, 1- IodoheptaneCyclo Hexyliodide, 4-Iodoaniline, 2-Fluoro -4-Iodoaniline, 1, 4 – Diiodobenzene4 – Iodophenol, 2 – Iodotoluene,3 , 5 – Diiodosalicylicacid,1,3-Diiodo-5,5-Dimethyl HydantoinN-Iodo Succinimide, 2 – Iodophenol,Iodoform, Tetrabutyl Ammonium IodideTrimethyl Sulfoniumiodide, ChloroiodomethaneDi Iodo Methane,Ethyl Magnesium Iodide - 1m Solution In THFMethyl Magnesium Iodide - 1m Solution In THFThymol Iodide, 1,3 – Diiodopropane1 , 10-Diiododecane, 2-Iodoethanol1-Bromo 2-Iodobenzene, 1-Bromo 4-Iodobenzene,3-Iodo-N-Phenyl Carbazole, 4-Fluoro Iodobenzene2-Nitro Iodobenzene, 2-Iodo Aniline2-Butyl-3(3,5-Diiodo-4-Hydroxy Benzoyl) BenzofuranMethyl Ammonium Iodide, 1,3-Diiodo Benzene5-Iodo Uracil, 1,4-Diiodo Butane2-Iodoacetic Acid, 3- Iodo Pyridine4- Iodo Pyridine, Iodophor, Povidone – Iodine PowderPropidium Iodide, Diiodoethane, 6- Iodo Indazole,4-Bromo-2-Iodoaniline, 3-Iodotrifluoride,3-Iodoaniline, Diiodo Fluro Methane

Overallquantity

50 MT/month


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RAW MATERIAL DETAILS (APPROX. CONSUMPTION)

Raw Materials Consumptionkg Raw Materials Consumption

kgPotassium hydroxide 622.4 Charcoal 6Iodine 2570.4 Toluene 1670Formic acid 276.5 Catalyst -AIBN 0.4Dimethyl sulfate 538.2 N-Chloro Succinimide 130Potassium iodide 155 Sodium iodide 190Sodium hydroxide 193.8 Acetone 17831-Propanol 102.8 2 –Aminophenol 10Red phosphorous 36.1 Hypo 242-Propanol 100 Chloroform 19.21-Butanol 111 Aluminium chloride 0.06Phosphorous 19.9 Tri butyl amine 19.5Hydriodic acid 1031 Ethyl acetate 143Allyl alcohol 110 Dichloro methane 80Dimethyl sulfoxide 105 TFH 160Aniline 114.6 Magnesium metal 5Sodium nitrite 434 Thymol 30Soda ash 89.1 1,3 – Dibromopropane 203- Toluidine 100 6-Amino indazole 9.2Methyl anthranilate 14 HCL 351Dilute sulphuric acid 507 3-Trifluoro methyl aniline 8.5Potassium bromated 20 3-Nitro aniline 13.8Acetic anhydride 83 Iron powder 7.4Hydrogen peroxide 30 Ammonia solution 2.5Ethylene dichloride 24 4-Bromo aniline 14.3Iodobenzene diacetate 2 Iodine monochloride 13.5Trifluroacetic acid 2 Acetic acid 1604-Amino benzoic acid 13 1 ,10 – Decanediol 45Isopropyl alcohol 25 2-Chloroetanol 103- Amino benzoic acid 15 DMF 35IPA 25 2-Bromo aniline 8.7Tri phenyl phosphine 168 4- Bromoaniline 81,3-Dibromo5,5-dimethyl hydantoin 40 3-Amino-N-phenyl

carbazole 26

Xylene 15 Methylene dichloride 50N –Hexanol 12.8 4-Fluoroaniline 141– Heptanol 14.2 2-Nitroaniline 14Cyclohexanol 11.7 2-Nitro iodobenzene 22.1Sodium bicarbonate 24.8 Sodium sulphide 57N – heptane 280 2-Butyl-3benzofuran 602-Fluoro aniline 13.2 Sodium acetate 534 – iodo aniline 10 Sodium bisulfite 16EDC 323 40%Monomethylamine 80Cyclohexane 30 Phosphorus 6.74 – Aminophenol 11 Meta phenelyne diamine 60Sulphuric acid 53 Uracil 25


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Raw Materials Consumptionkg Raw Materials Consumption

kgMDC 401 Tetra hydro furan 302 – Toluidine 20 5% Sodium bisulfite 10Salicylic acid 43 EDC Solvent 10Methanol 1770.5 4-Amino pyridine 8Chloro acetic acid 50 Phosphoric acid 23-Amino pyridine 8 Phosphate buffer powder 125


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2.4 MANUFACTURING PROCESS:[1] SODIUM IODIDE

(A) Raw material input:

Iodine = 100 kg Sodium hydroxide = 37 kg Formic acid = 23-25 kg M/L of previous batch = 125 ltr

Output of Sodium iodide = 118 kg(B) Chemical reaction:

2 NaOH + I2 + HCOOH + Water 2 NaI + 2 H2O

(C) Process :

In a vessel, charge M/L of previous batch followed by sodium hydroxide. To the clear solution, addformic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature tillcomplete conversion in to product. Concentrate the product solution to certain specific gravity. Chill tocrystallize the product. Filter product and dry in dryer. Collect mother liquor for recycling in next batch.Process and pack the finish product. i.e. Sodium iodide

(D) Flow sheet diagram :

Sodiumhydroxide

WaterFormic acid

Iodine

Filter

M/L for recycle

Dryer Sodium iodide

(E) Mass Balance:

18 hrs Sodium iodide = 118 kg M/L to recycle

Sodium hydroxide = 37kg

Iodine = 100 kg

Formic acid = 23 kg

M/L of previous batch = 125 ltr


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[2] POTASSIUM IODIDE

(A) Raw material inputs:

Iodine = 100 kg Potassium hydroxide = 47 kg Formic acid = 18-25 kg M/L of previous batch = 150 ltr

Output of Potassium iodide= 128 kg(B) Chemical reaction:

2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

(C) Process :

In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution, addformic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature tillcomplete conversion in to product. Concentrate the product solution to certain specific gravity. Chill tocrystallize the product. Filter product and dry in dryer. Collect mother liquor for recycling in next batch.Process and pack the finish product. i.e. Potassium iodide


Pot. hydroxide

WaterFormic acid

Iodine

Filter

M/L for recycle

Dryer Potassium iodide

(E) Mass balance:

Potassiumhydroxide = 47kg

Iodine = 100 kg

Formic acid = 23 kg


20 hrsPotassium iodide = 128 kg

M/L to recyclein next batch


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[3] AMMONIUM IODIDE

(A) RAW MATERIAL :

Iodine = 100 kg Ammonium hydroxide = 157 kg Hydrogen peroxide = 28 kg M/L of previous batch = 125 ltr

Output of Ammonium iodide = 110 kg(B) Chemical reaction:

2 NH4OH + I2 + H2O2 + Water 2 NH4I + 2 H2O

(C) Process :

In a vessel, charge M/L of previous batch and then ammonium hydroxide. To the solution, add hydrogenperoxide at room temp..With stirring charge iodine at elevated temperature. Maintain temperature tillcomplete conversion in to product. Concentrate the product solution to certain specific gravity. Chill tocrystallize the product. Filter product and dry in dryer. Collect mother liquor for recycling in next batch.Process and pack the finish product. i.e. Ammonium iodide


Amm.hydroxide

Water

Hydrogenperoxide

Iodine

Filter

M/L for recycle

Dryer Ammonium iodide

(E) Mass balance:

Ammoniumhydroxide = 157kg

Iodine = 100 kg

Hydrogenperoxide= 28 kg


20 hrsAmmonium iodide= 110 kg

M/L to recycle innext batch


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[4] COPPER IODIDE

(A) Raw material input:

Sodium hydroxide = 28 kg Iodine = 76 kg Formic acid = 18-23 kg Copper sulfate = 147 kg Sodium bisulfite = 28-35 kg Water = 125 ltr

Output of Copper iodide = 111 kg(B) Chemical reaction:

2 NaOH + I2 + HCOOH + Water 2 NaI + 2 H2O + CO2

2 CuSO4.5H2O + 2 NaI + NaHSO3 2 CuI + 3 NaHSO4 + Water

(C) Process :

In a vessel, charge Water followed by sodium hydroxide. To the clear solution, add formic acid at roomtemp. With stirring charge iodine at elevated temp. Maintain temperature till complete conversion in toproduct. This is ready solution of sodium iodide to use in next step. To this clear solution, add coppersulfate at room temp. And at elevated temp. with stirring charge sodium bisulfite. Maintaintemperature till complete conversion in to product. Cool to crystallize the product. Filter product anddry in dryer. Drain M/L for ETP. Process and pack the finish product. i.e. Copper(I) iodide


Water

Sodium hydroxide Iodine

Formicacid

Coppersulfate

SBS

M/L to ETP

Filter Dryer Copperiodide

Sodiumiodidesolution


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(E) Mass balance:

Sodium hydroxide = 28.2 kg

Iodine = 76.3 kg

Formic acid = 15.3 kg

Water = 120 ltr

12 hrs Sodium iodide = 90kg in water solution

+ Coppersulfate = 147 kg

+ Sodiumbisulfite = 28 kg

Copper iodide= 111 kg

11 hrs Waste water =120 ltr to ETP

[5] ZINC IODIDE

(A) RAW MATERIAL :

Iodine = 100 kg Zinc metal = 29 kg Hydrogen peroxide = 8-12 kg M/L of previous batch = 115 ltr

Output of Zinc iodide = 148 kg(B) Chemical reaction:

2 Zn + I2 + H2O2 + Water 2 ZnI + 2 H2O

(C) Process :

In a vessel, charge Water followed by zinc metal. To the slurry, add hydrogen peroxide at room temp.With stirring charge iodine at elevated temp. Maintain temperature till complete conversion in toproduct. Concentrate the product solution to certain specific gravity. Chill to crystallize the product.Filter product and dry in dryer. Collect mother liquor for recycling in next batch.

Process and pack the finish product. i.e. Zinc iodide


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Water

Zinc metal

Hydrogen

peroxide

Filter Dryer

M/L for recycle

Iodine

Zinc iodide

(E) Mass balance:

Zinc metal = 29 kg

Iodine = 100 kg

Hydrogen peroxide= 10 kg


16 hrsZinc iodide =148 kg


[6] SILVER IODIDE

(A) RAW MATERIAL :

Silver nitrate = 10 kg Iodine = 7.6 kg Potassium hydroxide = 3.6 kg Formic acid = 1.6 kg Water = 30 ltr

Output of Silver iodide = 13.8 kg(B) Chemical reaction:

2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

AgNO3 + KI + Water AgI + KNO3


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(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. This solution is ready to use as potassium iodide solution for next step.

To this clear solution, add silver nitrate at elevated temperature. Maintain temperature till completeprecipitation of product. Concentrate the product solution to certain volume. Chill to crystallize theproduct. Filter product and dry in dryer. Collect mother liquor for silver recovery and send it to ETP.


Pot. hydroxide

W aterForm ic acid

Iodine

Potassium iodidesolution

M/L for recovery

Filter Dryer

Silvernitrate

Dry Silveriodide

(E) Mass balance:

Potassiumhydroxide = 3.6 kg

Iodine = 7.6 kg


Water = 12 ltr

20 hrs Potassium iodide =9.7 kg in water

+ Silver nitrate = 10 kg

+ Water = 48 ltr

8 hrs Waste water = 60 ltr

Silver iodide = 13.8 kg


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[7] CALCIUM IODATE

(A) Raw material:

Calcium chloride = 40 kg Potassium hydroxide = 28.4 kg Iodine = 60 kg Hydrogen peroxide = 84.4 kg Water = 80 ltr

Output of Calcium iodate = 88 kg

(B) Chemical reaction:

2 KOH + I2 + H2O2 2 KIO3

2 KIO3 + CaCl2 + Water Ca( IO3 )2 + 2 KCl

(C) Process :

In a vessel, charge water followed by potassium hydroxide. To the clear solution, add iodine followed bynitric acid in small lots at elevated temp. Maintain temperature till complete conversion in to product.Transfer this mass in another vessel and add Calcium chloride till pH comes to neutral. Chill to crystallizethe product. Filter product and dry in dryer. Collect mother liquor for 2nd crop and potassium chloriderecovery.

Process and pack the finish product.


M/L for KClrecovery

Filter Dryer

Water

Iodine

PotassiumhydroxideNitric acid

Hydrogen peroxide Calcium chloride

Calcium iodate


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(E) Mass balance:

Iodine = 100 kg


Hydrogen peroxide = 195 kg

Nitric acid = 75 kg

Water = 190 ltr

16 hrs Potassium iodate =136 kg In water

Calciumchloride =40 kg to neutral pH

4 hrs

Calcium iodate = 166 kgWaste water afterevaporation = 360 ltr

[8] POTASSIUM IODATE

(A) RAW MATERIAL :

Iodine = 100 kg Potassium hydroxide = 96 kg Water = 190 ltr Nitric acid = 75 kg Hydrogen peroxide = 195 kg

Output of Potassium iodate = 166 kg


2 KOH + I2 + Water + HNO3 + H2O2 2 KIO3 + KNO3 + 2H2O

(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, add at room temp.,with stirring charge iodine at elevated temp. Maintain temperature till complete solution in to product.Add nitric acid and then hydrogen peroxide. Now shift solution in to another vessel and adjust pH toneutral by adding potassium hydroxide.

Concentrate the product solution to specific volume. Chill to crystallize the product. Filter product anddry in dryer. Collect mother liquor for recovery of second crop and then send for potassium nitraterecovery. Process and pack the finish product.


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(D) Flow sheet diagram:

M/L forPotassiumnitraterecovery

Filter Dryer

Water

IodinePotassiumhydroxide

Nitric acid Hydrogen peroxide Potassiumhydroxide

Potassium iodate

(E) Mass balance:

Iodine = 100 kg



Nitric acid = 75 kg

Water = 190 ltr

16 hrs Potassium iodate =136 kg In water

Potassium hydroxide= 50 kg to neutralpH

4 hrs

Ptassium iodate =166 kg

Waste water afterevaporation = 360ltr

[9] SODIUM IODATE

(A) RAW MATERIAL :

Iodine = 100 kg Sodium hydroxide = 88 kg Water = 190 ltr Nitric acid = 75 kg Hydrogen peroxide = 195 kg

Output of Potassium iodate = 153 kg


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2 NaOH + I2 + Water + HNO3 + H2O2 2 NaIO3 + NaNO3 + 2H2O

(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, add at room temp.,with stirring charge iodine at elevated temp. Maintain temperature till complete solution in to product.Add nitric acid and then hydrogen peroxide. Now shift solution in to another vessel and adjust pH toneutral by adding potassium hydroxide.

Concentrate the product solution to specific volume. Chill to crystallize the product. Filter product anddry in dryer. Collect mother liquor for recovery of second crop and then send for potassium nitraterecovery. Process and pack the finish product.


M/L for Sodiumnitrate recovery

Filter Dryer

Water

Iodine

Sodium hydroxideNitric acid

Hydrogen peroxideSodium hydroxide

Sodium iodate

(E) Mass balance:

Iodine = 100 kg

Water = 190 ltr

Sodium hydroxide = 33 kg


Nitric acid = 75 kg

16 hrs Mix iodate = 124kg in water

+ Sodium hydroxide= 51 kg

4 hrs

Sodium iodate = 153 kg M/L = 318 ltrfor secondcrop recovery


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[10] SODIUM METAPERIODATE

(A) RAW MATERIAL :

Iodine = 100 kg Sodium hydroxide = 137 kg Sodium persulfate = 156 kg Nitric acid = 80 kg Water = 195 ltr

Output of Sodium metaperiodate = 165 kg


8 NaOH + I2+ 2Na2S2O8 +H2O2 + 2 HNO3 2NaIO4 +4Na2SO4 +NaNO3 +4H2O

(C) Process :

In a vessel, charge sodium hydroxide + water. To it, very slowly at room temp., with stirring chargeiodine followed by nitric acid. Heat to elevated temp and add hydrogen peroxide. After getting productin process analysis, shift solution in to crystallizer. Concentrate the product solution to specific volume.To the solution add sodium persulfate and then add sodium hydroxide. Heat at elevated temperature.Adjust pH to neutral by nitric acid. Cool mass and filter crystals of product. Send mother liquor forsodium sulfate & sodium nitrate recoveries. Dry wet cake, process and pack the final product. i.e.Sodium metaperiodate.


Filter

M/L to ETP

Dryer

Sod.persulfate

NitricacidSod.hydroxide

W ater

Iodine

Nitric acid

Hydrogen peroxideSodiumhydroxide

Sodium metaperiodate


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(E) Mass balance:

Sodiumhydroxide = 37 kg

Iodine = 100 kg

Water = 90 ltr


Nitric acid = 67 kg

16 hrs Sodium iodate =155 kg in water

+ Sodium persulfate = 156 kg

+ Sodium hydroxide = 100 kg

+ Nitric acid = 13 kg

8 hrs

Sodium metaper iodate

= 165 kg

M/L = 310 ltrto ETP

[11] POTASSIUM METAPER IODATE

[A] Raw materials:

Iodine = 50 kg Potassium hydroxide = 71.8 kg Hydrogen peroxide = 72 kg Potassium persulfate = 59 kg Nitric acid =33 kg Water = 90 ltr

Output of Potassium meta periodate= 88 kg

[B] Chemical Reaction :

8 KOH + I2+ 2K2S2O8 +H2O2 + 2 HNO3 2KIO4 +4K2SO4 +KNO3 +4H2O

(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, at room temp., withstirring charge iodine at elevated temp. Maintain temperature till complete solution in to product. Addnitric acid and then hydrogen peroxide. Now shift solution in to another vessel and adjust pH to neutralby adding potassium hydroxide. To the solution add potassium persulfate and then add potassiumhydroxide. Heat at elevated temperature. Adjust pH to neutral by nitric acid. Cool mass andfilter crystals of product. Send mother liquor for sodium sulfate & sodium nitrate recoveries.Dry wet cake, process and pack the final product. i.e. Potassium metaperiodate


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[D] Flow Sheet Diagram:

Filter

M/L to ETP Potassiummetaper iodate

Dryer

Potassium persulfate

NitricacidPotassiumhydroxide

Water

Iodine

Nitric acid Hydrogen peroxide

Potassiumhydroxide

(E) Mass balance:

Potassium hydroxide = 26 kg

Iodine = 50 kg

Water = 90 ltr


Nitric acid = 20 kg


+ Potassium persulfate = 59 kg

+ Potassium hydroxide = 46 kg


Potassium metaper iodate

= 88 kgM/L = 155 ltrto ETP

12 hrs


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[12] LITHIUM IODIDE- HYDRATE

[A] Raw materials :

Lithium hydroxide = 75 kg Water = 280 ltr Iodine =193 kg Formic acid = 54 kg

[B] Chemical reaction:

2 LiOH + I2 + HCOOH + Water 2 LiI. x H2O + 2 H2O + CO2

[C] Process:

In a vessel, charge Water followed by lithium hydroxide. To the clear solution, add formic acid at roomtemp. With stirring charge iodine at elevated temp. Maintain temperature till complete conversion in toproduct.

Concentrate the product solution to certain specific gravity. Chill to crystallize the product. Filterproduct and dry in dryer. Collect mother liquor for recycling in next batch. Process and pack the finishproduct. i.e. Lithium iodide hydrate

[D] Flow sheet diagram :

WaterLithium hydroxide

Formic acid

Iodine

Filter Dryer

M/L to recycle in next batch

Lithium iodideHydrate

(E) Mass balance:

Lithium hydroxide = 75 kg

Iodine = 193 kg

Water = 280 ltr

Formic acid = 54 kg

Lithium iodidehydrate = 525 kg


23 hrs


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[13] NICKEL IODIDE

[A] Raw materials:

Nickel hydroxide = 10 kg Hydriodic acid = 29 kg

Output of Nickel Iodide = 26 kg


Ni(OH)2 + 2 HI NiI2 + 2H2O

[C] Process:

Charge hydriodic acid in a vessel and slowly add Nickel hydroxide till it completely dissolves . Stir forfew hours and then heat to evaporate all water to get dry residue as product. Collect dry powder ofproduct and pack.

[D] Flow sheet diagram:

Water

Nickel hydroxide

Hydriiodic acid

Water evoparation

Nickel iodide

(E) Mass balance:

Nickel hydroxide = 10 kg

Hydriodic acid = 29 kgNickel iodide = 32 kg

18 ltr waterevaporation afterreaction. No M/L.

8 hrs


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[14]LEAD IODIDE

[A] Raw material:

Lead nitrate = 3.5 kg Water = 10 ltr Potassium iodide = 4.0 kg

Output of Lead iodide = 4.6 kg


Pb(NO3)2 + 2KI + Water PbI2 + 2KNO3

[C] Process:

Charge water followed by lead nitrate. Slowly add potassium iodide at RT and heat to elevatedtemperature for few minutes. Evaporate water totally to get dry residue. Unload the dry residualpowder and pack.


Leadnitrate

Water

Potassiumiodide

Lead iodide

Water evaporation

(E) Mass balance:

Lead nitrate = 3.5 kg

Potassiumiodide = 4.0 kg

Water = 10 ltrLead iodide = 4.6 kg

10 ltr waterevaporation afterreaction. No M/L.

8 hrs


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[15] CADMIUM IODIDE

[A] Raw materials:

Cadmium sulfate = 2.6 kg Water = 10 ltr Potassium iodide = 3.5 kg

Output of Cadmium iodide = 3.6 kg

[B] Chemical Reaction:

CdSO4 + 2 KI CdI2 + K2SO4

[C] Process:

Charge water followed by cadmium sulfate. To this solution add Potassium iodide slowly. Heat toelevated temperature and evaporate maximum water to get slurry of product. Filter and wash withlittle water. Treat M/L for Cadmium salt recovery. Unload wet cake, dry in dryer to get dry powder andpack.


Water

Potassiumiodide

Filter

M/L for Cadmiumrecovery

Dryer

Water evaporation

Cadmium sulfate

Water

Cadmium iodide

(E) Mass balance:

Cadmium sulfate = 2.6 kg

Potassium iodide = 3.5 kg

Water = 10 ltr

Cadmium iodide = 4.4 kg M/L for Cadmiumrecovery

10 hrs


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[16]THALLIUM IODIDE

[A] Raw materials:

Thallium sulfate = 2.5 kg Water = 40 ltr Potassium iodide = 1.9 kg

Output of Thallium iodide = 2.8 kg


Tl2SO4 + 2 KI 2 TlI + K2SO4

[C] Process:

Charge water followed by thallium sulfate. To this solution add Potassium iodide slowly. Heat toelevated temperature and evaporate maximum water to get slurry of product. Start evaporation ofwater completely to get dry powder of product. Unload and if required, dry in dryer to get dry powderand pack.


Water

Potassiumiodide

Water evaporation

Thallium sulfate

Thallium iodide

(E) Mass balance:

Thallium sulfate = 2.5 kg


Water = 16 ltr

6 hrs Dry Tahllium iodide =2.8 kg

Evaporation of waterafter reaction. NoM/L.


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[17] ANTIMONY IODIDE

[A] Raw materials:

Antimony metal = 7 kg Iodine = 14.8 kg Toluene = 140 lit

Output of Antimony iodide = 27.9 kg


2 Sb + 3 I2 2 SbI3

[C] Process:

Charge toluene then Antimony metal and heat to elevated temperature. Slowly add iodine powder andreflux for few hours. Cool to down temperature .Filter. Dry product in dryer. Send M/L for toluenerecovery.


Iodine

Filter Dryer

Antimony metal

Toluene

M/L for Toluene recovery

Antimony iodide

(E) Mass balance:

Antimony metal = 7 kg

Iodine = 14.8 kg

Toluene = 140 ltr

19 hrsAntimony iodide = 27.9 kg M/L 140 ltr for

toluene recovery


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[18] HYDROIODIC ACID

[A] Raw materials

Iodine = 6.2 kg Water = 180 ltr Phosphorous = 3.1 kg

Output of HYDROIODICACID = 105.5 kg


3 I2 + 6 H2O + 2 P 6 HI + 2 H3PO4

[C] Process:

Charge iodine followed by phosphorous. In portions add water and heat to elevated temperature forfew hours. Start distillation when all iodine dissolved. Separate low density HI fraction duringdistillation. Collect the main fraction of HI and pack. Residue send for iodine recovery.


Water

Phosphrous

Iodine

Dist.

receiver

Low strengthfraction to recycle

Pure Hydriodic acidResidue to recyclein next batch

(E) Mass balance:

Iodine = 62 kg

Water = 180 ltr

Phosphorous = 3.1 kg

28 hrsHydriodic acid= 105.5 kg Distillate +residue to

recycle in next batch


30

[20] CALCIUM IODIDE HYDRATE

(A) Raw material inputs:

1. Hydriodic acid = 11.5 kg

2. Calcium carbonate = 2.5 kg

Output of Calcium iodide hydrate = 9.9 kg


2 HI + CaCO3 CaI2. X H2O + CO2

(C) Process:

Charge hydriodic acid in a vessel and slowly add Calcium carbonate till it completely dissolves . Stir forfew hours and then heat to evaporate all water to get dry residue as product. Collect dry powder ofproduct and pack.


Hydriiodic acid

Water evoparation

Calcium iodidehydrate

Calcium carbonate

(E) Mass balance:

Calcium carbonate = 2.5 kg

Hydriodic acid = 11.6 kgCalcium iodidehydrate = 9.9 kg

5ltr waterevaporation afterreaction. No M/L.

9 hrs


31

[21] IODINE

(A) Raw material:

Iodine = 110 kg

Output of pure Iodine = 100.0 kg

(B) No chemical reaction but just change in physical appearance.

(C) Process:

In a clean and dry vessel, charge Iodine and heat to some elevated constant temp for few hrs to startsublimation. Collect sublimed pure iodine on the other side receiver.

Pack the pure sublimed iodine.


Io d in e c ru d e

P u re S u b l im e d Io d in e

R e c e iv e r

R e s id u e f o rS o d iu m io d id e b a tc h

(E) Mass balance:

Crude Iodine = 110 kg 6 hrsPure iodine = 100 kg

Residue +water to Sodiumiodide batch

[22] IODINE MONOCHLORIDE

(A) Raw material:

1. Iodine = 100kg

2. Chlorine gas = 40 kg

3. Heptane = 200 ltr

Output of Iodine monochloride = 115 kg


I2 + Cl2 2 ICl


32

(C) Process:

In a clean vessel, charge Iodine and with maintaining critical temp., pass chlorine gas. After passingsufficient gas, cool mass to RT and add solvent heptane. Filter slurry of product. Air dry in dryer andpack. Send heptane M/L for caustic treatment followed by recovery of heptane.


Iodine

Chlorine

Filter Iodine monochloride

M/L for Heptane recovery

Heptane

(E) Mass balance:

Iodine = 100 kg

Chlorine = 40 kg

Heptane = 200 ltr

12 hrsIodine monochloride = 115 kg

M/L for heptane

recovery

[23] 0.1 N STANDARD IODINE SOLUTION

(A) Raw material:

1. Iodine = 1.8 kg

2. Potassium iodide = 3.6 kg

3. Distilled water = 94.6kg

Output of Iodine solution = 100 kg

(B) No chemical reaction, just dissolution of solid in water.


33

(C) Process:

In a clean vessel, charge water followed by potassium iodide. Heat to warm and add iodine. Stir verywell to dissolve all iodine. Check clarity and normality of formed solution. Pack. No waste during thisprocess.


Water

Potassiumiodide

Iodine

o.1 N Iodine solution

(E) Mass balance:

Water = 94.6 kg


Iodine = 1.8 kg

Standard 0.1 N Iodine

water solution

3 hrs

[24] IODIC ACID

(A) Raw material:


Output of Iodic acid crystals = 128 kg


2 KOH + I2 + Water + 2HNO3 + H2O2 HIO3 + 2KNO3 + H2O

(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, add at room temp.,with stirring charge iodine at elevated temp. Maintain temperature till complete solution in to product.Add nitric acid and then hydrogen peroxide.


34

Concentrate the product solution to specific volume. Chill to crystallize the product. Filter product anddry in dryer. Collect mother liquor for recycle in next batch. Process and pack the finish product.


Filter Dryer

Water



Iodic acidcrystals

M/L to recycle in next batch

Water evaporation

(E) Mass balance:

Iodine = 100 kg



Nitric acid = 75 kg

Water = 190 ltr

12 hrs Iodic acid = 128 kg Inwater

Cryastalline

Iodic acid = 128 kgM/L = 160 ltr torecycle in next batch

Water evaporation = 200 ltr16 hrs

[25] IODIC ACID 40% SOLUTION

(A) Raw material:


Output of 40% Iodic acid solution = 320 kg


35


2 KOH + I2 + Water + 2HNO3 + H2O2 HIO3 + 2KNO3 + H2O

(C) Process :

In a vessel, charge Water followed by potassium hydroxide. To the clear solution, add at room temp.,with stirring charge iodine at elevated temp. Maintain temperature till complete solution in to product.Add nitric acid and then hydrogen peroxide.

Concentrate the product solution to specific volume. Chill to crystallize the product. Filter product anddry in dryer. Collect mother liquor for recycle in next batch. Process and pack the finish product.


Water



Iodic acid40% solution

Water evaporation

(E) Mass balance:

Iodine = 100 kg



Nitric acid = 75 kg

Water = 190 ltr

12 hrs Iodic acid = 128 kg Inwater

Iodic acid 40%solution = 320 kg

Water evaporation = 130 ltr10 hrs

[26] PERIODIC ACID

(A) Raw material:

Iodine = 100 kg Sodium hydroxide = 137 kg


36

Sodium persulfate = 156 kg Nitric acid = 80 kg Water = 195 ltr Sulfuric acid = 21 kg

Output of Periodic acid = 133 kg


8 NaOH + I2+ 2Na2S2O8 +H2O2 + 2 HNO3 2NaIO4 +4Na2SO4 +NaNO3 +4H2O

2NaIO4 + H2SO4 HIO4 + Na2SO4

(C) Process :

In a vessel, charge sodium hydroxide + water. To it, very slowly at room temp., with stirring chargeiodine followed by nitric acid. Heat to elevated temp and add hydrogen peroxide. After getting productin process analysis, shift solution in to crystallizer. Concentrate the product solution to specific volume.To the solution add sodium persulfate and then add sodium hydroxide. Heat at elevated temperature.Adjust pH to neutral by nitric acid. Cool mass and filter crystals of product. Send mother liquor forsodium sulfate & sodium nitrate recoveries.

Take wet cake in water and with cooling slowly add sulphuric acid to form periodic acid. Stir withheating for few hrs and then chill. Filter crystals of periodic acid. Send M/L to ETP.


37


Filter

M/L to ETP

Sod.persulfate

NitricacidSod.hydroxide

Water

Iodine

Nitric acid

Hydrogen peroxideSodiumhydroxide

Wet cake of Sodiummetaperiodate

WaterSulfuricacid

FilterM/L to ETP

DryerPer iodic acid


38

(E) Mass balance:

Sodiumhydroxide = 37 kg

Iodine = 100 kg

W ater = 90 ltr


Nitric acid = 67 kg


+ Sodium persulfate = 156 kg



8 hrs

Sodium metaper iodate

= 165 kg

M/L = 310 ltrto ETP

+ Sulfuric acid = 21 kg

+ W ater = 50 ltr

Periodic acid = 133 kg W aste water = 50 ltr withsodium sulfate to ETP


39

[27] BARIUM IODIDE

(A) Raw material:

1. Barium carbonate = 6.4kg

2. Hydriodic acid = 16.8 kg

Output of Barium iodide = 10 kg


BaCO3 + 2HI BaI2 + CO2 + H2O

(C) Process:

In a vessel charge Hydriodic acid and with stirring add slowly Barium carbonate at little elevated temp.Continue addition till pH of reaction mass becomes almost neutral from basic. Simple filter the formedclear solution and take clear filtrate in to evaporation vessel. Evaporate mass to get dry powder ofproduct. Pack it.


Hydriodicacid Bariumcarbonate

Barium iodide

(E) Mass balance:

Hydriodicacid= 16.8 kg

Bariumcarbonate=6.4 kgBarium iodide = 10 kg Water to evaporate = 13 kg

4 hrs 4 hrs


40

[28] IODINE MONOCHLORIDE 40% SOLUTION IN ACETIC

(A) Raw material:

1. Iodine monochloride = 42 kg

2. Acetic acid = 62 kg

Output of Iodinemonochloride solution = 104 kg

(B) Chemical reaction: No chemical reaction but dissolution of solid in solvent.

(C) Process:

In a vessel, charge acetic acid and slowly in portions add iodine monochloride with stirring. Stir well tillit becomes very clear solution. Check % and pack. No effluent in this process.


Aceticacid Iodinemonochloride

Iodinemonochloride solution

(E) Mass Balance:

4 hrsAcetic acid= 62 kg

Iodine

monochloride = 42 kg

Iodinemono

chloride solution = 104 kg


41

[29] IODINE MONOCHLORIDE 40% SOLUTION IN MDC

(A) Raw material:

1. Iodine monochloride = 42 kg

2. MDC = 62 kg

Output of Iodine monochloride solution = 104 kg

(B) Chemical reaction: No chemical reaction but dissolution of solid in solvent.

(C) Process:

In a vessel, charge MDC and slowly in portions add iodine monochloride with stirring. Stir well till itbecomes very clear solution. Check % and pack. No effluent in this process.


MDC Iodinemonochloride

Iodinemonochloride solution

(E) Mass balance:

5 hrsMDC = 62 kg

Iodine

monochloride = 42 kg

Iodinemono

chloride solution = 104 kg


42

[30] CESIUM IODIDE

(A) Raw materials:

Caesium carbonate = 33.0 kg Water = 66 ltr Hydriodic acid = 47.5 kg

Output of Caesium iodide = 52 kg


Cs2CO3 + 2 HI 2 CsI + H2O + CO2

(C) Process:

In a vessel, charge water followed by caesium carbonate. Now start addition of hydriodic acid andadjust pH to almost neutral. Stir reaction solution for few hours. Under vacuum distil out watercompletely to get dry powder of product. Distilled water can be recycled in next batch. Unload the drypowder of product and pack.


CaesiumcarbonateWater

Hydriodicacid

Dist.

Rec.

Dry pureCaesium iodide

Didtilled water torecycle

(E) Mass balance:

Caesiumcarbonate= 33 kg

Water = 66 ltr

Hydriodic acid =47.5 kg

Caesiumiodide = 62 kgExcess water = 76 ltr to

distill and recycle3 hrs 7 hrs


43

[31] METHYL IODIDE

(A) Raw material: Potassium hydroxide = 51 kg Iodine = 108 kg Formic acid = 25 kg Dimethylsulfate = 65 kg Water = 160 ltr

Output of Methyl iodide = 111 kg

(B) Chemical reaction:2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4(C) Process :Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature and addiodine followed by formic acid. To this solution, add dimethyl sulfate slowly. Reflux mass for fewhours. Distil out product, i.e. Methyl iodide. Send residual water to ETP.(D) Flow sheet diagram:

WaterIodine

PotassiumhydroxideFormicacid

Dimethylsulfate

Residue to ETP Methyl iodide

Dist.

Rece.


44

(E) Mass balance:

Pot.hydroxide = 51 kg

Water = 160 ltr

Iodine = 108 kg

Formicacid = 25 kg

8 hrs KI = 138 kg in 160ltr water

10 hrs

+ Dimethylsulfate =65 kg

Pure Methyl iodide= 111 kg

Residue to ETP =298 Kg

[32] ETHYL IODIDE

(A)Raw material:

Potassium iodide = 51 kg Iodine = 108 kg Diethyl sulfate = 81 kg Sodium hydroxide = 25 kg Water = 160 ltr

Output of Methyl iodide = 129 kg

(B) Chemical reaction:KI + ( C2H5 )2SO4 C2H5I + (C2H5)KSO4(C) Process :Charge water in a vessel and dissolve potassium iodide. Heat to elevated temperature and addsodium hydroxide to get basic pH. Add diethyl sulfate slowly. Reflux mass for few hours. Distil outproduct, i.e. Ethyl iodide. Send residual water to ETP.(D) Flow sheet diagram:

WaterIodine


Diethylsulfate

Residue to ETP Ethyl iodide

Dist.

Rece.


45

(E)Mass balance:


Water = 160 ltr

Iodine = 108 kg

Formicacid = 25 kg


10 hrs

+ Diethylsulfate = 81 kg

Pure Ethyl iodide = 129 kg Residue to ETP =296 kg

[33] 1- IODO PROPANE

(A) Raw material: Iodine = 220 kg 1-Propanol = 100 kg Red phosphorous = 12 kg Water = 70 ltr

Output of 1-IodoPropane = 280 kg

(B) Chemical reaction:10 (CH3CH2CH2-OH) + 5 I2 + 2 P 10 (CH3CH2CH2-I ) + 2 H3PO4 + 2H2O(C) Process :In a vessel, charge 1-Propanol followed by red phosphorous and at elevated temperature addiodine. Reflux for 6-8 hours for complete conversion in to product. Add water and distil out productas pure 1-Iodo propane. Send residual mass of reaction vessel to ETP.


46


IodinePhosphorous

1-Propanol

Dist.

Receiver

Residue to ETP

1-Iodopropane

W ater

(E)Mass balance:

Water = 70 ltr

Iodine = 220 kg

Phosphorous = 12 kg

1-Propanol = 100 kg

30 hrs Pure 1-Iodopropane =280 kg

Residual wastewater = 122 kg

[34] 2-IODOPROPANE

[A] Raw Materials :

Iodine = 220 kg 2-Propanol = 100 kg Red phosphorous = 20 kg Water = 70ltr

Output of 2-Iodopropane = 290 kg


CH 3

CH 3

O H + Phosphrous + Iodine

CH 3

CH 3

I H 3 PO 4+ + 2H 2 O

[C] Process :In a vessel, charge 2-propanol followed by red phosphorous and at elevated temperature addiodine. Reflux for 6-8 hours for complete conversion in to product. Add water and distil out productas pure 2-Iodo propane. Send residual mass of reaction vessel to ETP.


47


Phosphorous

Iodine

Dist.

Receiver

Residue water to ETP

2-Iodopropane

2-Propanol

(E) Mass balance:

Water = 70 ltr

Iodine = 220 kg

Phosphorous = 20 kg

2-Propanol = 100 kg

30 hrs Residual wastewater = 120 kg

Pure 2- Iodopropane= 290 kg

[35] 1- IODO BUTANE

(A) Raw material: Iodine = 179 kg 1-Butanol = 100 kg Phosphorous = 12 kg Water = 70 ltr

Output of 1-Iodo butane = 225 kg

(B) Chemical reaction:10 (CH3CH2CH2-OH) + 5 I2 + 2 P 10 (CH3CH2CH2-I ) + 2 H3PO4 + 2H2O(C) Process :In a vessel, charge 1-butanol followed by red phosphorous and at elevated temperature add iodine.Reflux for 6-8 hours for complete conversion in to product. Add water and distil out product aspure 1-Iodo butane. Send residual mass of reaction vessel to ETP.


48

(D) Flow sheet diagram:W ater

IodinePhosphorous

1-Butanol

Dist.

Receiv er

Residue to ETP

1-Iodobutane

(E)Mass balance:

Water = 70 ltr

Iodine = 179 kg

Phosphorous = 12 kg

1-Propanol = 100 kg

30 hrs Pure 1-Iodobutane= 225 kg

Residual wastewater = 136 kg

[36] ALLYL IODIDE [ Hydriodic acid route ]

(A) Raw material: Hydriodic acid = 350 kg Allyl alcohol = 100 kg


(B) Chemical reaction:CH2=CH-CH2-OH + HI CH2=CH-CH2-I + H2O(C) Process :In a vessel, charge hydriodic acid followed by Allyl alcohol. Allow to stand for few hours. Reflux atelevated temperature to complete reaction. Distil out product as pure allyl iodide. Send residualliquor for recovery of excess hydriodic acid by distillation and send distilled water to ETP.


49


Pure A llyl iodide

Dilute Hydriodic acid forrecov ery by distillation

Dist.

Rec.

A llylalcohol

Hydriodic acid

Residue to ETP

(E) Mass balance:

A l ly l io d id e = 1 0 0 k g

H y d r io d ic a c id = 3 5 0 k g1 9 h rs

A l ly l io d id e = 2 6 0k g

D i lu te h y d r io d ica c id = 3 0 0 k g

R e c o v e re d P u reh y d r io d ic a c id =1 6 5 k g to re c y c le

D is t . w a te r = 1 8 5l t r + R e s id u e toE T P

[ Iodine route ]

[A] Raw Materials :

Allyl alcohol = 10 kg Red phosphorous = 1.3 kg Iodine = 13.2 kg Water = 8 ltr

Output of ALLYL IODIDE = 17.3 kg


CH2

OH

+ Phosphorous + IodineCH2

I

+

+

2H2O

H3PO4


50

[C] Process :Charge Allyl alcohol and Phosphorous at elevated temperature. Add iodine and reflux for fewhours. Add water and distil out pure product. Residue mass send for iodine recovery and then ETP.[D] Flow Sheet Diagram :

Phosphorous

Iodine

Dist.

Rec.

Resdue water to ETP

Allyl iodide

Allyl alcoholWater

(E) Mass balance:

Allyl alcohol = 10 kg

Iodine = 13.2 kg


Water = 8 ltr

13 hrsAllyl iodide = 17.3 kg Waste water =

15.2 kg to ETP

[37] TRIMETHYL SULFOXONIUM IODIDE

(A) Raw material: Iodine = 104 kg Potassium hydroxide = 49 kg Formic acid = 25 kg Water = 155 ltr Dimethyl sulfate = 155 kg Dimethyl sulfoxide = 105 kg

Output of Trimethyl sulfoxonium iodide = 161 kg

(B) Chemical reaction:2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4CH3I + CH3SOCH3 (CH3)3S+(O) I-


51

(C) Process :Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature andadd iodine followed by formic acid. To this solution, add dimethyl sulfate slowly. Reflux massfor few hours. Distil out product, i.e. Methyl iodide. Use this Methyl iodide in next step. Sendresidual water to ETP. In a vessel, charge dimethyl sulfoxide followed by methyl iodide. Allowto stand for few hours. Heat at elevated temperature to complete reaction. Cool and filter theslurry of product. Send mother liquor for excess dimethyl sulfoxide and iodine recoveries.(D) Flow sheet diagram:

Filter Dryer

M/L for DMSO & iodine recovery

WaterIodine

Formicacid

Dimethylsulfate

Residue toETP

Methyl iodide

Dist.

Rec.

Dimethylsulfoxide

Trimethylsulfoxonium iodide

(E) Mass balance:


Water = 155 ltr

Iodine = 104 kg

Formicacid = 25 kg


10 hrs

+ Dimethylsulfate= 155 kg

Pure Methyl iodide= 129 kg

Residue after DMSO/Iodine reco. to ETP =432 kg

+ Dimethyl sulfoxide= 105 kg

30 hrs

Trimethyl sulfoxoniumiodide = 161 kg

M/L for DMSO &Iodine recovery


52

[38] IODO BENZENE

(A) Raw material: Aniline = 100 kg Sodium nitrite = 86 kg Potassium hydroxide = 69 kg Iodine = 147 kg Formic acid = 26 kg Hydrochloric acid = 320 ltr Water = 420 ltr Sodium hydroxide = 28 kg Soda ash = 33 kg

Output of Iodobenzene = 201 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2C6H5-NH2 + NaNO2 + HCl + KI + Water C6H5-I + NaCl + KNO2 + H2O(C) Process :In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step. In another vessel, charge water and hydrochloric acid. Add aniline and atcold temperature, add sodium nitrite. Stir and then charge potassium iodide solution and maintainfor few hours. Distil out product from the reaction mass. Treatment of Soda ash and sodiumhydroxide followed by high vacuum distillation gives pure product. i.e. Iodo benzene.

(C) Flow sheet diagram:

Pot. hydroxide

WaterFormic acid

Iodine

Potassiumiodidesolution

HClWater

Sodiumnitrite

Residual water to ETP

Dist.

Rec.

Iodobenzene

Aniline


53

(F) Mass balance:Water = 220 ltr

Iodine = 147 kg

Formicacid = 26 kg


Potassium iodide =189 kg in water

7 hrs

+ Aniline = 100 kg

+ Sodium nitrite = 86 kg

+ Hydrochloric acid = 300 ltr

+ Water = 200 ltr

+ Soda ash = 33 kg


12 hrs

Pure Iodobenzene= 201 kg

waste water to ETP

= 1028 kg

[39] 3-IODO TOLUENE

(A) Raw material: 3- Toluidine = 100 kg Sodium nitrite = 76 kg Potassium hydroxide = 61 kg Iodine = 129 kg Formic acid = 23 kg Hydrochloric acid = 290 ltr Water = 345 ltr Sodium hydroxide = 24 kg Soda ash = 30 kg

Output of 3-Iodo toluene = 185 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2CH3-C6H4-NH2 + NaNO2+ HCl+ Kl + WaterCH3-C6H4-I+NaCl+KNO2 +H2O(C) Process :In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acidat room temp. With stirring charge iodine at elevated temp. Maintain temperature till complete


54

conversion in to product. Concentrate the product solution to certain specific gravity. Thissolution is ready for next step. In another vessel, charge water and hydrochloric acid. Add 3-toluidine and at cold temperature, add sodium nitrite. Stir and then charge potassium iodidesolution and maintain for few hours. Distil out product from the reaction mass. Treatment of Sodaash and sodium hydroxide followed by high vacuum distillation gives pure product. i.e. 3-Iodotoluene.(D) Flow sheet diagram:

Pot. hydroxideWater

Formic acid

Iodine


3-ToluidineHCl

Water

Sodiumnitrite


Dist.

Rec.

3-Iodotoluene


55

(E) Mass balance:

Water = 195 ltr

Iodine = 129 kg

Formicacid = 23 kg


Potassium iodide =166 kg in water

7 hrs

+ 3-Toluidine = 100 kg



+ Water = 150 ltr

+ Soda ash = 30 kg

+ Sodiumhydroxide = 24 kg

12 hrs

Pure 3-Iodotoluene= 185 kg

Waste water to ETP

= 893 kg

[40] 2-IODO METHYL BENZOATE

(A) Raw material :

Methyl anthranilate = 14.0 kg Dilute sulphuric acid = 70 ltr Sodium nitrite = 7.0 kg Water = 40 ltr Potassium hydroxide = 9.5 kg Iodine = 21 kg Formic acid = 4 kg

Output of 2-Iodo methyl benzoate = 27 kg

(B) Chemical reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NH2

O

OCH3

+ +NaNO2 KI

+ NaOH

I

O

O CH3


56

(C) Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step. In another vessel charge dilute sulphuric acid and at low temp add methylanthranilate. To this solution add sodium nitrite solution slowly at low temp. Stir for few minutesand transfer this reaction mixture in a solution of potassium iodide at ambient temp. Filterproduct, wash with water and dry in dryer to get 2-Iodo methyl benzoate.(D) Flow sheet diagram :

M/L to ETP

waterSulfuricacid

MethylanthranilateSodium nitrite

FilterDryer 2-Iodomethylbenzoate

Pot. hydroxide

Water

Formic acid

Iodine


(E) Mass balance:


Iodine = 20.3 kg


Water = 10 ltr

3 hrsPotassiumiodide= 26 kg in water

+ Methylanthranilate = 14 kg

+ Sodium nitrite = 7.0 kg

+ Dilute sulfuric acid = 70 kg

+ Water = 10 ltr

6 hrs

Pure 2-Iodomethylbenzoate = 27 kg

Waste water to

ETP = 138.5 kg


57

[41] 2-IODO BENZOICACID(A) Raw material :

Methyl anthranilate = 14.0 kg Dilute sulphuric acid = 70 ltr Sodium nitrite = 7.0 kg Potassium iodide = 26 kg Water = 39 ltr Sodium hydroxide = 9.7 kg

Output of 2-Iodobenzoic acid = 23.8 kg(B) Chemical Reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2N H 2

O

OC H 3

+ +NaNO 2 KI

+ NaOH

I

O

O H

(C) Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step. Charge dilute sulphuric acid and at low temp add methyl anthranilate. To thissolution add sodium nitrite solution slowly at low temp. Stir for few minutes and transfer thisreaction mixture in a solution of potassium iodide at ambient temp. Filter product, wash withwater and take this wet cake for hydrolysis with sodium hydroxide solution at elevated temp.Acidify this hydrolysed reaction mass up to 6.5 pH by adding dil sulphuric acid. Filter the formedslurry of 2-Iodo benzoic acid. Wash with little water. Dry in dryer and pack as finish product. SendM/L to ETP.(D) Flow sheet diagram:

Methylanthranilate Sodium hydroxide

2-Iodobenzoic acid

waterSulfuricacid

Sodium nitrite

FilterW etcake

Dil. Sulfuricacid

Filter

M/L to ETP

Dryer

Pot. hydroxide

W ater

Form ic acid

Iodine

Potassium iodidesolution

M/L to ETP


58

(E)Mass balance:Potassiumhydroxide = 9.5 kg

Iodine = 20.3 kg


Water = 10 ltr




+ Dilute sulfuric acid = 70 kg

+ Water = 10 ltr

6 hrs

2-Iodomethylbenzoate = 27 kg

Waste water to

ETP = 121.9 Kg

+ Sodium hydroxide = 9.7 kg

+ Dil. sulfuric acid = 10 kg

Waste water to

ETP = 20 Kg

Pure 2-Iodobenzoic acid

= 23.8 kg

5 hrs

[42] DESS-MARTIN PERIODINANE(A) Raw material :

Methyl anthranilate = 14.0 kg Dilute sulphuric acid = 70 ltr Sodium nitrite = 7.0 kg Potassium hydroxide = 9.5 kg Water = 72 ltr Formic acid = 3.7 kg Iodine = 20.3 kg Potassium bromated = 20 kg Acetic anhydride = 52 kg Sodium hydroxide = 7 kg


59

Output of Dess-Martin Periodinane = 31 kg

(B) Chemical reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NH2

O

OCH3

+ +NaNO2 KI

+ NaOH

I

O

OH

+ KBrO3

+ Water

IO

O

OOH

+Acetic anhydride

I

O

O

OO

CH3

O

OCH3

O

O

CH3

Dess-Martin Periodinane

(C) Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step.Charge dilute sulphuric acid and at low temp add methyl anthranilate. To this solution add sodiumnitrite solution slowly at low temp. Stir for few minutes and transfer this reaction mixture in asolution of potassium iodide at ambient temp. Filter crude product and hydrolyse in hot solution ofsodium hydroxide at elevated temp for few hrs. Then adjust pH 6.5-7.0 by adding dil sulphuric acidand filter the formed slurry of 2-Iodo benzoic acid. This pure 2-Iodobenzoic acid in sulphuric acidtreated with potassium bromated at high temp with stirring for few minutes and then cooled toroom temp. Product filtered and washed with water, wet cake used directly without drying for nextstage.Wet cake of above and acetic anhydride mixed and heated to elevated temp for few hrs. Chilled todown temp and filtered as finish product.


60


Methylanthranilate Sodiumhydroxide

2-Iodobenzoic acid

waterSulfuricacid

Sodium nitrite

FilterWetcake

Dil. Sulfuricacid

Filter

M/L to ETP

Dryer

Pot. hydroxide

Water

Formic acid

Iodine


M/L to ETP

2-Iodobenz.aciddil.Sulfuricacid

Pot.bromate

Filter

M/L to ETP

Wetcake

Aceticanhydride

Filter

M/L for acetic acid& 2ndcrop recovery

Dryer

Ether

Dess-Martin periodinane


61

(F) Mass balance:

Potassium hydroxide = 9.5 kg

Iodine = 20 kg


Water = 10 ltr




+ Sodium nitrrite = 7 kg

+ Sodium hydroxide = 7.0 kg

+ Water = 72 ltr

5 hrs

6 hrs

+ Potassium bromate = 20 kg

+ Water = 10 ltr

Waste water =

12.5 Kg to ETP

14 hrs

+ Acetic anhydride = 52 kg M/L for Acetic acidrecovery = 52 kg

Pure Dess-Martin periodinane

= 31 kg

Waste water 180Kg to ETP

[43] IODOBENZENE DIACETATE

(A) Raw material :

Aniline = 3.6 kg Sodium nitrite = 3.0 kg Potassium hydroxide = 2.4 kg Iodine = 5.2 kg Formic acid = 0.90 kg Water = 20.8 ltr Hydrochloric acid = 11 ltr Acetic anhydride = 31 ltr Hydrogen peroxide = 10 ltr Ethylene dichloride = 24 ltr Ice = 40 kg

Output of Iodobenzenediacetate = 6.0 kg


62

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2C6H5-NH2 + NaNO2 + HCl + KI + Water C6H5-I + NaCl + KNO2 + H2OI

+ (CH3CO)2O + H2O2

I (OCOCH3)2

+CH3COOH + H2O

(C) Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step.In another vessel, charge water and hydrochloric acid. Add aniline and at cold temperature, addsodium nitrite. Stir and then charge potassium iodide solution and maintain for few hours. Distilout product from the reaction mass. Treatment of Soda ash and sodium hydroxide followed by highvacuum distillation gives pure product. i.e. Iodo benzene.Charge acetic anhydride followed by hydrogen peroxide in a vessel. With stirring slowly drop wiseadd iodo benzene at slight elevated temp. Keep mass for stirring for few hours to completereaction. Quench the reaction mass in ice and stir for few hours the resulted product slurry. Filterthe crude product, dry. Send M/L for acetic acid recovery and then send residual volume to ETP.Take crude dry product in EDC and heat to dissolve. Cool the resulted clear solution and get theslurry of pure product. Filter slurry at down temp, dry. Send M/L for EDC & second crop recoveries.Pack the dry product.


63


Pot. hydroxide

WaterFormic acid

Iodine


Aniline

HClWater

Sodium nitrite


Dist.

Rec.

Iodobenzene

Aceticanhydride

Hydrogenperoxide

Iodobenzene

Filter

M/L for Aceticacid recovery,

then to ETP

Dryer

Crudeproduct EDC

Filter

M/L for EDCrecovery

Dryer Iodobenzene diacetate


64

(E) Mass balance:


Iodine = 5.2 kg


Water = 5 ltr

2 hrs Potassium iodide

= 6.6 kg in water

+ Aniline = 3.6 kg


+ Hydrochloric acid = 11 ltrWaste water =17 Kg to ETP

+ Acetic anhydride = 31 ltr

+ Hydrogen peroxide = 10 ltr

+ EDC = 24 ltr

+ Ice = 40 kg

12 hrs

10 hrs

Iodobenzenediacetate = 6.0 kg

M/L for solvent +Acetic acidrecoveries = 128.9kg

[44] BIS TRIFLUORO ACETOXY IODOBENZENE

(A) Raw material :

Iodobenzene diacetate = 6.0 kg Trifluroacetic acid = 6.0 kg

Output of Bis trifluoroacetoxy iodobenzene = 5.4 kg


I (OCOCH3)2

+ 2 CF3COOH

I (OCOCF3)2

+ 2 CH3COOH


65

(C) Process:Make a slurry of Iodo benzene diacetate and trifluoro acetic acid and heat to elevated temp for fewhours. Chill the resulted slurry of pure product. Filter and dry. Send M/L for acetic acid recoveryand then to ETP. Pack the dry finish product.(D) Flow sheet diagram:

Iodobenzenediacetate

Trifluroaceticacid

Filter

M/L for aceticacidrecovery then to ETP

Dryer Bis trifluoroacetoxy iodobenzene

(E)Mass balance:

Iodobenzene diacetate = 6.0 kg

Trifluroaceticacid = 6.0 kg

11 hrsBis trifluoroacetoxyiodobenzene = 5.4 kg

M/L for trifluoro aceticacid recovery = 6.6 kg

[45] 4-IODOBENZOICACID

(A) Raw material:

4-Amino benzoic acid = 13 kg Sodium nitrite = 7 kg Water = 44 ltr Dilute sulphuric acid = 65 ltr Potassium hydroxide = 9.0 kg Iodine = 19 kg Formic acid = 3.5 kg Isopropyl alcohol = 25 ltr

Output of 4-Iodobenzoicacid = 18 kg

(B) Chemical reaction :


66

2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NH2

OOH

+ NaNO2 + KI

I

OOH

+ KNO2

H2O+ + Na2SO4

dil. Sulfuric acid

(C) Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step.In to a chilled dilute sulphuric acid, slowly add 4-Amino benzoic acid and followed by sodiumnitrite solution. After addition stir for few hrs. Transfer this reaction mixture in to a solution ofpotassium iodide solution and heat to elevated temp for few minutes. Cool the formed crudeproduct slurry and filter. Send M/L to ETP. Purify this wet crude product in IPA with heating,followed by chilling to get pure product slurry in IPA. Filter the slurry and dry . Send M/L for IPArecovery. Pack the finish product.(D) Flow sheet diagram:

Pot. hydroxide

WaterFormic acid

Iodine

4-Aminobenzoicacid

Dil. Sulfuricacid Sodiumnitrite

Filter

M/L to ETP

Crude

Product

IPA

Filter

M/L for IPArecovery

Dryer

Pure4-Iodobenzoicacid

PotassiumiodideSolution


67

(E) Mass balance:

Potassium hydroxide= 9.kg

Iodine = 19 kg


Water = 14 ltr

Potassiumiodide= 25 kg in water

+ 4-Aminobenzoicacid =13 kg

+ Sodiumnitrite = 7 kg

+ Dil. sulfuric acid = 65 ltr

+ Water = 30 ltr

+ IPA = 25 ltr

13 hrs

Finish Product 4-Iodobenzoicacid = 18 kg

Waste water =142.5 Kg to ETP

25 Kg washing MLfor IPA recovery

3 hrs

[46] 3-IODOBENZOIC ACID

(A) Raw Materials :

3- Amino benzoic acid = 15 kg Dilute sulphuric acid = 70 ltr Sodium nitrite = 7 kg Potassium hydroxide = 9.0 kg Iodine = 19 kg Formic acid = 3.5 kg IPA = 25 ltr Water = 24 ltr

Output of 3-IODO BENZOIC ACID = 23.8 kg

[B] Chemical reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

OOH

NH 2

+ NaNO 2 + KI

OOH

I

+ KNO 2

H 2 O+ +Na 2 SO 4

dil. Sulfuric acid


68

[C] Process :In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step.Dissolve 3-Amino benzoic acid in dil. Sulphuric acid and cool. Add sodium nitrite solution and stirfor few hours .Transfer this reaction mass into above made potassium iodide solution and heat toelevated temperature for few minutes .Cool and filter crude. Purify crude by recrystallization inIPA. Filter and dry the finish product.[D] Flow sheet diagram :

Pot. hydroxide

WaterFormic acid

Iodine

3-AminobenzoicacidDil. Sulfuricacid Sodiumnitrite

Filter

M/L to ETP

Crude

Product

IPA

Filter

M/L for IPArecovery

Dryer

Pure

3-Iodobenzoic acid



69

(E) Mass balance:

Potassium hydroxide= 9.kg

Iodine = 19 kg


Water = 14 ltr

Potassiumiodide= 25 kg in water

+ 3-Aminobenzoicacid =15 kg



+ Water = 10 ltr

+ IPA = 25 ltr

13 hrs

Finish Product 3-Iodobenzoicacid = 23.8 kg

Waste water =123.7 Kg to ETP

25 Kg washing MLfor IPA recovery

[47]METHYL TRI PHENYL PHOSPHONIUM IODIDE

(A) Raw Materials :

Tri phenyl phosphine = 67 kg Potassium hydroxide = 18.7 kg Iodine = 40 kg Formic acid = 10 kg Water = 60 ltr Dimethyl sulfate = 39 kg Toluene = 150 ltr

Output of METHYL TRI PHENYL PHOSPHONIUM IODIDE = 100 kg

(B )Chemical Reaction :2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4


70

CH3 I + P

Toluene

P

CH3

I

(C) Process :Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature and addiodine followed by formic acid. To this solution, add dimethyl sulfate slowly. Reflux mass for fewhours. Distil out product, i.e. Methyl iodide. Send residual water solution for treatment and then toETP.Charge toluene followed by tri phenyl phosphine .Add methyl iodide at ambient temperature andstir for few hours at ambient temperature . Filter the formed slurry of pure product . Dry and pickM/L for toluene recovery and 2nd crop .(D) Flow Sheet diagram :

WaterIodine

Potassiumhydroxide

Formicacid

Dimethylsulfate

Residue to ETP Mehyl iodide

Dist.

Rec.

Filter Dryer

Methyl triphenyl phosphonoium iodide

Toluene

Triphenyl phosphine

M/L for toluene recovery


71

(E) Mass balance:

Pot.hydroxide = 18.7 kg

Water = 60 ltr

Iodine = 40 kg

Formicacid = 10 kg

8 hrs KI = 51.2 kg inwater

10 hrs

+ Di methylsulfate = 39.1 kg

Methyl iodide = 42 kg Residue to ETP = 175 Kg

+ Triphenyl phosphine = 67 kg

+ Toluene = 150 ltr

Finish Product Methyltriphenylphosphonioum iodide = 100 kg

M/L for toluene +second crop recovery= 109.7 kg

16 hrs

[48] ETHYL TRI PHENYL PHOSPHONIUM IODIDE

(A) Raw materials :

Tri phenyl phosphine =93 kg Potassium hydroxide = 26 kg Iodine = 55 kg Formic acid = 12 kg Water = 80 ltr Diethyl sulfate = 60 kg Toluene = 200 ltr

Output of ETHYL TRI PHENYL PHOSPHONIUM IODIDE = 158 kg

(B )Chemical Reaction :2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4


72

+ P

Toluene

PI

CH3

CH3CH2I

[C] Process :Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature and addiodine followed by formic acid. To this solution, add diethyl sulfate slowly. Reflux mass for fewhours. Distil out product, i.e. Ethyl iodide. Send residual water solution for treatment and then toETP.Charge toluene followed by triphenyl phosphine. Add Ethyl iodide at ambient temperature and stirfor few hours. Filter at ambient temperature, formed slurry of pure product . Dry and pack thefinish product. Send M/L for toluene recovery and 2nd crop recovery.[D] Flow sheet diagram :

WaterIodine

Potassiumhydroxide

Formicacid

Diethylsulfate

Residue to ETP Ethyl iodide

Dist.

Rec.

Filter Dryer

Ethyl triphenyl phosphonoium iodide

Toluene

Triphenyl phosphine



73

(E) Mass balance:


Water = 80 ltr

Iodine = 55 kg

Formicacid = 12 kg

8 hrs KI = 70 kg inwater

8 hrs

+ Di ethylsulfate = 60 kg

Methyl iodide = 42 kg Residue waste waterto ETP = 228 Kg


+ Toluene = 200 ltr

Finish Product Ethyltriphenylphosphonioum iodide = 158 kg

M/L for toluene +second croprecovery = 140 kg

24 hrs

[49] ISO PROPYL TRI PHENYL PHOSPHONIUM IODIDE

[A] Raw Materials :

Iodine = 6.3kg 1-Propanol = 2.8 kg Red phosphorous = 0.6 kg Water = 5 ltr Triphenyl phosphine = 8 kg Xylene = 15 ltr

Output of ISO PROPYL TRI PHENYL PHOSPHONIUM IODIDE = 14.8 kg

[B} Chemical reaction :

CH3

CH3

OH + Phosphrous + Iodine

CH3

CH3

I H3PO4+ + 2H2O


74

+ P PI

CH 3

C H 3

CH 3

CH 3

I

Xylene

[C] Process :In a vessel, charge 2-Propanol followed by phosphorous and at elevated temperature add iodine.Reflux for 6-8 hours for complete conversion in to product. Add water and distil out product aspure 2-Iodo propane. Send residual mass of reaction vessel to ETP.Charge Xylene followed by TPP. Charge 2-iodo propane and heat the mass to reflux for few hours .Cool to 5-10 delicious and filter . Wash wet cake with xylene . Dry and pack the finish product.Send M/L for recovery of xylene + 2nd crop .[D] Flow Sheet diagram:

Phosphorous

Iodine

Dist .

Rec.

Residue waterto ETP

2-Iodopropane

2-Propanol

Filter

M/L for Xylene &2nd crop recovery

Dryer

Xylene

Triphenylphosphine

Isopropyl triphenylphosphonium iodide


75

(E) Mass balance:

2-Propanol = 2.8 kg

Iodine = 6.3 kg


Water = 5 ltr

8 hrs 2-Iodo propane = 6 kg Waste water = 11 kgto ETP

+ Xylene = 15 ltr


24 hrs

F.P. Isopropyl triphenylphosphonium iodide = 14.8kg

M/L for xylenerecovery = 11.9kg

[50] 1-IODOHEXANE

[A] Raw Materials :

N –Hexanol = 12.8 kg Iodine = 13.00 kg Red phosphorous = 1.00 kg Water = 10 ltr

Output of 1-Iodohexane = 20.7 kg

[B] Chemical Reaction :10-[ CH3-(CH2)5-OH ] + 5I2 + 2P 10 [ CH3-(CH2)5-I ] + 2 H3PO4 + 2H2O[C] Process :In a vessel, charge 1-Hexanol followed by phosphorous and at elevated temperature add iodine.Reflux for 6-8 hours for complete conversion in to product. Add water and distil out product aspure 1-Iodo hexane. Send residual mass of reaction vessel to ETP.


76

[D] Flow Sheet Diagram :

Phosphorous

Iodine

Dist.

Rec.

Water to ETP

1-Iodo hexane

1-Hexanol

(E) Mass balance:n-Hexanol = 12.8 kg

Iodine = 13 kg

Phosphrous = 1.0 kg

Water = 10 ltr

22 hrs1-Iodohexane = 20.7 kg

Waste water = 16.1Kg to ETP

[51] 1- IODOHEPTANE

[A] Raw Materials :

1– Heptanol = 14.2 kg Iodine = 13.1 kg Phosphorous = 1.3 kg Water = 8 ltr

Output of 1-IODOHEXANE = 20.9kg

[B] Chemical Reaction :10-[ CH3-(CH2)6-OH ] + 5I2 + 2P 10 [ CH3-(CH2)6-I ] + 2 H3PO4 + 2H2O[C] Process :In a vessel, charge 1-Heptanol followed by phosphorous and at elevated temperature add iodine.Reflux for 6-8 hours for complete conversion in to product. Add water and distil out product aspure 1-Iodo heptane. Send residual mass of reaction vessel to ETP.


77


Phosphorous

Iodine

Dist.

Rec.

Waste water to ETP

1-Ioodheptane

1-Heptanol

(E) Mass balance:

n-Heptanol = 14.2 kg

Iodine = 13.1 kg


Water = 8 ltr

19 hrs1-Iodoheptane = 20.9 kg

Waste water = 15.7kg to ETP

[52] CYCLO HEXYLIODIDE

[A] Raw Materials :

Cyclohexanol = 11.7 kg Iodine = 13 kg Red phosphorous = 1.2 kg Water = 9 ltr

Output of Cyclohexyl iodide = 18 kg


2H2OH3PO4

OH

+ Iodine + Phosphorous

I

+ +


78

[C] Process :In a vessel, charge Cyclohexanol followed by red phosphorous and at elevated temperature addiodine. Reflux for 8 hours for complete conversion in to product. Add water and distil out productas pure Cyclohexyl iodide. Send residual mass of reaction vessel to ETP.[D] Flow Sheet Diagram :

Phosphorous

Iodine

Dist.

Rec.

Waste water to ETP

Cyclohexyl iodide

Cyclohexanol

(E) Mass balance:

Cyclohexanol = 11.7 kg

Iodine = 13 kg


Water = 9 ltr

17 hrsCyclohexyliodide = 25 kg

Waste water =

9.9 kg to ETP

[53]4-IODOANILINE

[A] Raw Materials :

Aniline = 11.00 kg Water = 44 ltr Sodium bicarbonate =12 kg Iodine =24.5 kg N – heptane = 100 lit

Output of 4-Iodoaniline = 23 kg


79


NH2

+ Iodine + NaHCO3

Water

NH2

I

NaI CO2

H2O

+ ++

[C] Process :Charge water and dissolve sodium bicarbonate at RT . Charge aniline and in portion add iodine inreaction mass at RT . Stir for few hours . Filter formed crude product (M/L send to ETP). Dry inair. Purify crude by recrystallization in heptane . Filter the pure product and send M/L forheptanes recovery.[D] Flow Sheet Diagram :

Water

Sod.bicarb

Aniline

Iodine

Filter

M/L for Iodinerecovery then to ETP

Dryer

Crude

Heptane

Filter

M/L for heptanerecovery

Dryer Pure4-Iodoaniline


80

(E) Mass balance:

Aniline = 11 kg

Sodiumbicarbonate = 12 kg

Iodine = 24.5 kg

Water = 44 ltr

8 hrsCrude product = 26 kg Waste water = 76

kg to ETP

+ Heptane = 100 ltr

5 hrs

Pure 4-Iodo aniline = 23 kgM/L for Heptane

recovery = 92.5kg

[54] 2-FLUORO -4-IODOANILINE

[A] Raw Materials :

2-Fluoro aniline = 13.2 kg Sodium Bicarbonate = 12.8 kg Water = 50 ltr Iodine = 25.0 kg n- heptane = 90 ltr

Output of 2-Fluoro-4-iodoaniline = 26.5 kg


NH2

F

+ Iodine + NaHCO3

Water

NH2

I

F

NaI CO2

H2O

+ ++

[C] Process :Charge water and dissolve sodium bicarbonate at RT . Charge2-Fluoro aniline and in portion addiodine in reaction mass at RT . Stir for few hours. Filter formed crude product (M/L send to ETP ).Dry in air . Purify crude by recrystallization in n- heptane.


81


Water

Sod.bicarb

2-Fluoro aniline

Iodine

Filter


Dryer

Crude

Heptane

Filter

M/L for heptanerecovery

Dryer Pure2-Fluoro4-Iodoaniline

(E) Mass balance:

2-Fluoro aniline = 13.2 kg

Sodiumbicarbonate = 12.8 kg

Iodine = 25 kg

Water = 50 ltr

10 hrsCrude product = 28 kg Waste water = 78

kg to ETP

+ Heptane = 90 ltr

6 hrs

Pure 2-Fluoro-4-iodo aniline= 26.5 kg

M/L for Heptane

recovery = 86.5kg


82

[55] 1, 4 – DIIODOBENZENE

[A] Raw Materials :

Aniline = 6.0 kg Sodium carbonate = 6.6 kg Dil. Sulphuric acid = 50 kg Sodium nitrite = 5.3 kg Potassium hydroxide = 4.8 kg Iodine = 23.8 kg Formic acid = 1.9 kg Water = 50 ltr EDC = 30 ltr Cyclohexane = 30 ltr

Output of 1,4-Diiodo benzene= 16.00 kg

[B] Chemical Reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NH2

I

+ NaNO 2 + KIDilute Sulfuricacid

Na 2SO 4

I

I

+ KNO 2

+

[C] Process :In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution of potassium iodide is ready to use in next stepCharge dil. Sulphuric acid and dissolve 4-iodo aniline. Cool to 5 Celsius and add sodium nitritesolution then stir for few minutes. Transfer this mass in a vassal containing potassium iodidesolution. Stir at elevated temperature for few hours. Cool to RT and Extract crude product in EDC .Distil out EDC to get almost dry residue. Recrystallization crude product in cyclohexane to get pureproduct.


83


Water

HCl

Water to ETP

Sodium nitriteEDC

4-Iodoaniline

Recovered EDC for recycleEDC layer

Cyclohexane

M/L for cyclohexane recovery

Dist.

Rec.

Filter Dryer

1,4-Diiodbenzene

WaterIodine

Pot.hydroxide

Formicacid

Potassium iodide in water


84

(E) Mass balance:

Aniline = 6 kg

Sodiumbicarbonate = 6.6 kg

Iodine = 13.5 kg

Water = 25 ltr

8 hrsCrude 4-Iodoaniline =10 kg

Waste water =

34 kg to ETP


+ Dil. sulfuricacid= 50 kg

+ EDC = 30 ltr

+ 13.2 kg Potassiumiodide solution

Crude 1,4 Diiodobenzene

= 19 kg

M/L for EDC

recovery = 44 kg


Iodine = 10.3 kg


Water = 25 ltr

4 hrs

10 hrs

+ Cyclohexane = 30 ltrs

5 hrs

Pure 1,4-Diiodobenzene = 16 kgM/L for cyclohexane

recovery = 26 kg

Waste water = 88.4 kg to ETP

[56] 4 – IODOPHENOL

[A] Raw Materials :

4 – Aminophenol = 11 kg Sulphuric acid = 15 kg Water = 55 ltr Sodium nitrite =7.5 kg Potassium hydroxide = 7.3 kg Iodine = 15.6 kg Formic acid = 2.8 kg MDC = 55 lit

Output of 4-Iodophenol = 20 kg

[B] Chemical Reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2


85

NH2

OH

+ NaNO2 + KIDil. Sulfuricacid

I

OH

+ KNO2 + Na2SO4

[C] Process :In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution of potassium iodide is ready to use in next step.Charge water followed by sulphuric acid. Cool to 5 -10 Celsius and add 4 – Aminophenol. Stir andslowly add sodium nitrite aqueous solution. Stir for few minutes and transfer this reaction mass into potassium iodide solution. After mixing, heat mass to elevated temperature. Cool to RT andextract crude product in MDC. Separate MDC layer. Water layer drain for ETP. Remove MDCcompletely from organic layer till dryness. Collect pure product (i.e. 4 – Iodophenol)[D] Flow Sheet Diagram :

4-Am inophenol

D il.sulfuricacid

Sodium nitrite

Reactionm ass

M DCDist.

W ater layerto ETP

Pot. hydrox ide

W aterForm ic acid

Iodine

Potassium iodideSolution

Pure 4-Iodophenol


86

(E) Mass balance:


Iodine = 15.6 kg


Water = 25 ltr

4 hrs Potassium iodide = 20 kg

in water

+ 4-Aminophenol = 11 kg


+ Water = 30 ltr

+ Sodiumnitrite = 7.5 kg

9 hrs

Crude 4-Iodo phenol = 24 kg

+ MDC = 55 ltrs

6 hrs

Pure 4-Iodophenol = 20 kg M/L for MDC recovery

= 74.2 kg

Waste water

to ETP = 75 kg

[57] 2 – IODOTOLUENE

[A] Raw Materials :

2 – Toluidine = 20 kg Sodium nitrite = 16.2 kg Potassium hydroxide = 12.4 kg Iodine = 26.4 kg Formic acid = 4.7 kg Hydrochloric acid = 60 ltr Water = 120 ltr Sodium hydroxide = 5.2 kg Soda ash = 6.1 kg

Output of 2 – iodotoluene = 35.8 kg


87

[B] Chemical reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO22-CH3-C6H4-NH2 + NaNO2 + HCl + Kl + Water CH3-C6H4-I +NaCl KNO2 +H2O[C] Process :In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next stepIn another vessel, charge water and hydrochloric acid. Add 2- toluidine and at cold temperature,add sodium nitrite. Stir and then charge potassium iodide solution and maintain for few hours.Distil out product from the reaction mass. Treatment of Soda ash and sodium hydroxide followedby high vacuum distillation gives pure product. i.e. 2-Iodo toluene.[D] Flow Sheet Diagram :

Pot. hydroxide

W aterFormic acid

Iodine

Potassiumiodide solution

W ater

HCl

Dist.

Rec.

W ater waste to ETP

Pure2-Iodotoluene

2-Toluidine

Sodium nitrite

W ater to ETP

Vac.

Rec


88

(E) Mass balance:


Iodine = 26.4 kg


Water = 40 ltr

5 hrs Potassium iodide = 33.8 kg

in water

+ 2-Toluidine = 20 kg

+ HCl = 60 ltr


+ Water = 80 ltr

+ Sodiumhydroxide = 5.2 kg

+ Soda ash = 6.1 kg

12 hrs

Pure 2-Iodotoluene = 35.8 kgWaste water = 235.2kg to ETP

[58] 3 , 5 – DIIODOSALICYLICACID

[A] Raw Materials :

Salicylic acid = 43 kg Iodine = 85.5 kg Methanol = 1200 ltr Sulphuric acid = 19 kg Hydrogen peroxide = 20 kg Charcoal = 1.0 kg

Output of 3,5- di iodo salicylic acid = 110 kg

[B] Chemical reaction :

O OH

OH

+ I I + H2O2

H2SO4+

Methanol

O OH

OH

II

+ 2H2O


89

[C] Process :Charge methanol followed by salicylic acid , iodine and sulphuric acid .Heat to elevatedtemperature and in portions add hydrogen peroxide until reaction completes. Stir for few hours.Distil out excess methanol and cool the formed slurry to RT. Filter and dry the crude product, M/Lto drain for ETP. Purify the crude in methanol with charcoal treatment. Filter. M/L for methanolrecovery and 2nd crop recovery. Dry and pack the pure product.[D] Flow Sheet Diagram :

Methanol

Salicylicacid

Sulfuricacid

Iodine

Hydrogenperoxide

Methanoldist.

Methanol to recycle

Filter

M/L to ETP

Dryer Crudeproduct

Methanol/Carbon

Filter

Crystalliser

Filter

M/L for 2nd crop /methanol recovery

DryerPure 3,5-Diiodo

salicylicacid


90

(E) Mass balance:

Salicylic acid = 43 kg

Methanol = 430 ltr

Iodine = 85.5 kg

Sulfuric acid = 19 kg


Crude Product = 119 kg Methanol distilled torecycle = 423 kg

19 hrs

+ Methanol = 770 ltr

+ Charcoal = 1 kg

Pure 3,5-Diiodo

salicylicacid = 110 kg

8 hrs

Methanol M/L

to recycle = 833kg

Charcoal as

solid waste= 2.5 kg

[59] 1,3-DIIODO-5,5-DIMETHYL HYDANTOIN

[A] Raw Materials :

1,3-Dibromo5,5-dimethyl hydantoin = 40 kg Iodine = 45 kg Catalyst -AIBN = 0.40 kg EDC = 200 ltr Potassium hydroxide = 22 kg Water = 32 ltr

Output of DIDMH product = 51.8 kg

[B] Chemical reaction :

N

NCH3

CH3

O

O

Br

Br

+ I I + CatalystEDC

KOH N

NCH3

CH3

O

O

I

I

2KBr

H2O

++

[C] Process :Charge EDC then dibromo dimethyl hydantoin in small portions at ambient temperature. Chargeiodine followed by small amount of catalyst. After complete addition with cooling stir mass for fewhours. Filter the formed slurry of product. Dry and pack. M/L treat with potassium hydroxide-water solution and then distil out EDC to recycle in next batch at low temperature under vacuum.Send residual water layer for ETP.


91


DBDMH

EDC

Iodine

Catalyst

Filter

M/L for EDC recovery

after KOH treatment

Filter Dryer DryDIDMH

(E) Mass balance:

DBDMH = 40 kg

Iodine = 45 kg

Catalyst = 0.4 kg

EDC = 200 ltr

18 hrs Pure Product DIDMH

= 51.8 kg

EDC M/L

+ Potassium

hydroxide = 22 kg

+ Water = 32 ltr

Pure EDC to recycle

in next batch after drying

= 232.6 kg

Water = 55 kg to ETP


92

[60] N-IODO SUCCINIMIDE

(A) Raw material: N-Chloro Succinimide = 130 kg Sodium hydroxide = 50 kg Water =200 ltr Iodine = 136 kg Formic acid = 30 kg Acetone = 780 ltr

Output of N-Iodo succinimide = 175 kg


O

O

N Cl + K I

O

O

N I + K Cl

(C) Process :In a vessel, charge acetone followed by N-Chloro succinimide . Add acetone solution of potassiumiodide and at elevated temperature maintain for 2 to 3 days. Add additional acetone and filterinorganic salt. Send it for iodine and potassium chloride recoveries. From mother liquor distil outacetone up to certain concentration. Chill residue and filter the slurry to isolate product. i.e. N-Iodosuccinimide.


93


W a te rIo d in e

S o d iu m h y d r o x id e

F o r m ic a c id

S o d iu m io d id e d r y p o w d e rA c e to n e

N - C h lo r o s u c c in im id e

F i l t e rP r o d u c t in M /L

S o l id f o r K C l r e c o v e r y

D is t .

R e c .

D is t i l l e d

A c e to n e t o r e c y c le

F i l t e rA c e to n e M /L t o r e c o v e r y

D r y e r

N - Io d o s u c c in im id e

(E) Mass balance:


Iodine = 136 kg

Formic acid = 30 kg

Water = 200 ltr

23 hrsSodium iodie dry powder

= 160 kg

275 kg water M/L


+ N-Chloro succinimide = 130 kg

+ Acetone = 780 ltr

65 hrs

N-Iodo succinimide = 175 kg Acetone M/L = 795 kg

for recovery

Saodium chloride =

81 kg as waste


94

[61] 2 – IODOPHENOL

[A] Raw Materials:

2 –Aminophenol = 10 kg Sodium nitrite = 7.0 kg Water = 40 tr Potassium hydroxide = 6.8 kg Iodine = 14.5 kg Formic acid = 2.6 kg Water = 22 ltr Sulphuric acid =19 kg EDC = 30 ltr N – Heptane = 20 ltr

Output of 2 – Iodophenol = 18.7 kg

[B] Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

OHNH2

+ NaNO2 + KIDil. Sulfuricacid

OHI

+ KNO2 + Na2SO4

[C] Process:In a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next stepIn a vessel, charge water followed by potassium hydroxide. To the clear solution, add formic acid atroom temp. With stirring charge iodine at elevated temp. Maintain temperature till completeconversion in to product. Concentrate the product solution to certain specific gravity. This solutionis ready for next step. Charge water followed by sulphuric acid. Cool to down temp and add 2 –Aminophenol. Stir and slowly add sodium nitrite aqueous solution. Stir for few minutes andtransfer this reaction mass in to potassium iodide solution. After maxing heat mass to elevatedtemperature. Cool to RT and extract crude product in EDC. Separate EDC layer. Water layer drainfor ETP. Remove EDC completely from organic layer till dryness U/V. Chill residue and unloadmass to get pure product. Dry in air and pack.


95


2-Aminophenol

Dil.sulfuricacid

Sodiumnitrite

Reactionmass

MDCDist.

Water layerto ETP

Pot. hydroxide

WaterFormic acid

Iodine


Pure 2-Iodophenol


96

(E) Mass balance:


Iodine = 14.5 kg


Water = 22 ltr


= 18.6 kg in water

+ 2-Aminophenol = 10 kg


+ Water = 30 ltr


11 hrs

Crude 4-Iodo phenol = 24 kg

+ EDC = 30 ltrs

4 hrs

Pure 2-Iodophenol = 18.7kg

M/L for EDCrecovery = 40 kg

Waste water

to ETP = 113.2 kg

[62] IODOFORM

[METHOD-I] BY HYPO

[A] Raw materials:

Potassium iodide = 6.0 kg Water = 10 ltr Acetone = 3 kg Hypo = 24 ltr

Output of Iodoform = 4.8 kg

[B] Chemical Reaction:CH3COCH3 + 3KI + 3 NaOCl CHI3 + CH3COONa + 3KCL + 2NaOH[C] Process :


97

In a vessel charge water followed by potassium iodide at RT . Add acetone and then with stirringdrop wise add hypo After complete addition worm reaction mixture for minutes . Cool to RT andFilter the formed slurry of pure product. Dry product in dryer and pack. M/L to drain in ETP.[D] Flow Sheet Diagram:

W ater

A ce tone

M /L to E T P

F ilte r D rye r D ry P ureIodo fo rm

W ate rP o tassium hydrox ideF orm icac id

Iod ine

P o tassium iod ideH ypo

(E) Mass balance:

Iodine = 4.6 kg

Potassium hydrox ide = 6.0 kg

Form icacid = 1.0 kg

W ater = 7 ltr


= 6.0 kg9 Kg water ev aporation

after reaction to dryness

3 hrs

+ Hyo = 24 ltr

+ Acetone = 3 ltr

+ W ater = 10 ltr

Iodoform = 4.8 kgM /L = 41.8 kg wastewater to ETP


98

[METHOD-II] BY METHYLIODIDE

[A] Raw materials:

Chloroform =1.2 kg Potassium hydroxide = 17 kg Iodine = 36 kg Formic acid = 8.3 kg Water = 53 ltr Dimethyl sulfate = 35.7 kg Chloroform = 18 kg Aluminium chloride =0.060 kg Methanol = 108 ltr

Output of Iodoform = 34 kg

[B] Chemical Reaction:2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4CHCl3 + 3 CH3I + AlCl3 CHI3 + 3 CH3Cl + AlCl3[C] Process:Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature and addiodine followed by formic acid. To this solution, add dimethyl sulfate slowly. Reflux mass for fewhours. Distil out product, i.e. Methyl iodide. At RT mix chloroform , aluminium chloride and methyliodide . Heat the mixture for few hours. To the formed product slurry at cooling temperature, addmethanol. Stir for few hours at down temperature. Filter the formed slurry. Wash with methanol toget pure product. Unload dry in dryer and pack. Send M/L for Iodine & methanol recoveries.


99


W a te rIo d in e

P o ta ss iu m h y d ro x id eF o rm ic a c id

D im e th y lsu lfa te

R e sid u e toE T P P u re M e th y l io d id e

D is t.

R e c .

C h lo ro fo rm

A lu m in iu m c h lo r id e

F ilte r

M /L fo r io d in e re c o v e ry

th e n to E T P

D ry e r P u re d ryIo d o fo rm


100

(E) Mass balance:

Potassiumhydroxide = 17 kg

Iodine = 36 kg

Formicacid = 8.3 kg

Water = 53 ltr


in water

+ Dimethyl sulfate = 35.7 kg

7 hrs

Methyl iodide = 38 kg

+ Chloroform = 18 kg

+ Aluminium chloride = 60 gm


11 hrs

Iodoform = 34 kg

Waste water = 117kg to ETP

M/L for methanol

recovery = 126.26 kg

[63] TETRABUTYL AMMONIUM IODIDE

[A] Raw materials

Tri butyl amine = 19.5 kg Ethyl acetate = 98 ltr 1-Butanol = 11 kg Iodine = 19.5 kg Phosphorous = 2.1 kg Water = 10 ltr

Output of Tetra butyl ammonium iodide = 33 kg

[B] Chemical Reaction:10 (CH3CH2CH2-OH) + 5 I2 + 2 P 10 (CH3CH2CH2-I ) + 2 H3PO4 + 2H2O


101

( C4H9)3N + C4H9I ( C4H9)4N + I -[C] Process:In a vessel, charge 1-butanol followed by red phosphorous and at elevated temperature add iodine.Reflux for 6-8 hours for complete conversion in to product. Add water and distil out product aspure 1-Iodo butane. Send residual mass of reaction vessel to ETP.Charge ethyl acetate followed by tri butyl amine and 1-Iodobutane. Heat the mixture to reflux forfew hours. After complete reaction, cool to low temperature and filter the formed slurry of pureproduct. Send M/L for Ethyl acetate and 2nd crop recovery. Dry the wet cake and pack.[D] Flow Sheet Diagram:

W ater

Iod ine

P hosphorous

1-B utano l

D ist.

R ece iv er

R esidue to E T PP ure1-Iodobutane

E thy lace ta te

T ribu ty lam ine

F ilte r D ryerD ry pure T e trabu ty lam m onium iod ide

M /L fo r 2nd c rop /e thy lace ta te recov ery


102

(E) Mass balance:

1-Butanol = 11 kg


Iodine = 19.5 kg

Water = 10 ltr

12 hrs1-Ioodbutane = 17 kg Waste water = 14.1

kg to ETP

+ Tributylamine = 19.5 kg

+ Ethylacetate = 98 ltr

50 hrs

Tetra butylammonium iodide

= 33 kg

M/L for 2nd crop + Ethyl

acetate recovery = 113kg

[64]TRIMETHYL SULFONIUMIODIDE

[A] Raw materials

Dimethyl sulfide = 21 kg Potassium hydroxide = 24.6 kg Iodine = 52 kg Formic acid = 12 kg Dimethyl sulfate = 51.6 kg Water = 77 ltr Methanol = 110 ltr

Output of Trimethyl sulfonium iodide = 71 kg

[B] Chemical Reaction:2KOH + I2+2HCOOH + ( CH3 )2SO4 2CH3I + K2SO4CH3 – S – CH3 + CH3I + Methanol ( CH3)3 S+ I -[C] Process:Charge water in a vessel and dissolve potassium hydroxide. Heat to elevated temperature and addiodine followed by formic acid. To this solution, add dimethyl sulfate slowly. Reflux mass for fewhours. Distil out product, i.e. Methyl iodide. Send residual water to ETP.At RT , Charge methanol then dimethyl sulfide. Charge methyl iodide at RT and stir for few hours.Heat to reflux and maintain for few hours. Chill the slurry of product and filter the pure product.Send M/L for methanol recovery and 2nd crop recovery. Dry wet cake in dryer and pack.


103


WaterIodine


Dimethylsulfate

Residue to ETP Pure Methyl iodide

Dist.

Rec.

Dimethylsufide

Methanol

Filter

M/L for methanolrecovery

Dryer Dry pure Trimethylsulfonium iodide


104

(E) Mass balance:


Iodine = 52 kg

Formicacid = 12 kg

W ater = 77 ltr

8 hrsPotassium iodide in

water

+ Dimethylsulfate = 51.6 kg

Mthyliodide = 55 kg

9 hrs


+ Dimethyl sulfide = 21 kg

38 hrs

Trimethyl sulfonium iodide =74 kg

M/L for 2nd crop

+ Methanol

recovery = 128.6 kg

W aste water =148.6 kg to ETP

[65] CHLOROIODOMETHANE

[A] Raw materials

Dichloro methane = 40 kg Potassium hydroxide = 28 kg Iodine = 59 kg Formic acid = 11 kg Acetone = 450 ltr Water = 300ltr Soda ash = 10 kg

Output of Chloroiodo methane = 79 kg

[B] Chemical Reaction :2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2CH2Cl2 + KI Cl- CH2-I + KCl


105

(C) Process :In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.Chill to crystallize the product. Filter product and dry in dryer. Collect mother liquor for recyclingin next batch. Process and pack the finish product. i.e. Potassium iodide.In a vessel, charge acetone and then charge above made potassium iodide. Heat and at elevatedtemperature, add dichloro methane. Maintain reflux for few hours. Distill out acetone. To theresidue, add water and separate layers. Wash product with soda ash solution. Fraction distil undervacuum, to get pure product. i.e. Chloro iodo methane. Send aqueous layer for iodine & potassiumchloride recoveries.[D] Flow Sheet Diagram :

PureChloroiodomethaneResidue for

KCl + Iodinerecovery

Pot. hydroxide

WaterFormic acid

Iodine

Potassium iodide powder

Acetone

Dist.

Receiver

Dichloromethane

Soda ash


106

(E) Mass balance:


Iodine = 59 kg

Formic acid = 11 kg

Water = 90 ltr


M/L =138 kg torecycle in nextbatch

+ Dichloromethane = 40 kg

+ Acetone = 450 ltr

+ Water = 200 ltr

+ Soda ash = 10 kg

20 hrs

Chloroiodomethane = 79 kgAcetone 2nd croprecovery = 401 kg

Residue waste water = 280 kg

to ETP

[66] DI IODO METHANE

(A)Raw material: Dichloro methane = 40 kg Potassium hydroxide = 55 kg Iodine = 117 kg Formic acid = 21 kg Acetone = 300 ltr Water = 200 ltr Soda ash = 10 kg


(B)Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2CH2Cl2 + 2 KI CH2I2 + 2 KCl(C) Process :In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintaintemperature till complete conversion in to product. Concentrate the product solution to certainspecific gravity. Chill to crystallize the product. Filter product and dry in dryer. Collect motherliquor for recycling in next batch. Process and pack the finish product. i.e. Potassium iodide.


107

In a vessel, charge acetone and then charge potassium iodide. Heat and at elevated temperature,add dichloro methane. Maintain reflux for few hours. Distill out acetone. To the residue, addwater and separate layers. Wash product with soda ash solution. Fraction distil under vacuum, toget pure product. i.e. Di iodo methane. Send aqueous layer for iodine & potassium chloriderecoveries.(D) Flow sheet diagram:

Pure Di iodomethaneResidue forKCl + Iodinerecovery

Pot. hydroxide

WaterFormic acid

Iodine

Potassium iodide powder

Acetone

Dist.

Receiver

Dichloromethane

Soda ash


108

(E) Mass balance:


Iodine = 118 kg

Formic acid = 22 kg

Water = 150 ltr


M/L to recyclein next batch

= 181 kg

+ Dichloromethane = 40 kg

+ Acetone = 300 ltr

+ Water = 50 ltr

+ Soda ash = 20 kg

30 hrs

Di iodomethane = 140 kg

M/L = 322 Kg for2nd crop /Acetone recovery

Residue waste water = 100 Kg

to ETP

[67] ETHYL MAGNESIUM IODIDE - 1M SOLUTION IN THF

(A) Raw materials; Potassium hydroxide = 6.6 kg Iodine = 14 kg Formic acid = 3.2 kg Diethyl sulfate = 15.3 kg Water =20 ltr THF = 80 lit Magnesium metal = 2.5 kg

Output 1 Molar Ethyl magnesium iodide solution in THF = 91.5 kg

(B) Chemical Reaction:KI + ( C2H5 )2SO4 C2H5I + (C2H5)KSO4C2H5I + Mg + Tetrahydrofuran C2H5—Mg—I in THF solvent


109

(C) Process:Charge water in a vessel and dissolve potassium iodide. Heat to elevated temperature and addsodium hydroxide to get basic pH. Add diethyl sulfate slowly. Reflux mass for few hours. Distil outproduct, i.e. Ethyl iodide. Send residual water to ETP.Charge THF followed by magnesium metal. With stirring in portions add ethyl iodide. Stir atambient temperature for few hours till all metal dissolves to get clear solution. With precaution ofmoisture pack this solution as finished product.[D] Flow Sheet Diagram:

Diethylsulfate

Residue toETP

Pure Ethyl iodide

Dist.

Receiver

THF

Magnesiummetal

Ethyl magnesium iodidesolution in THF solvent

WaterIodine

Pot.hydroxide

Formicacid


110

(E) Mass balance:


Iodine = 14 kg


Water = 20 ltr

6 hrs Potassiumiodide in water

solution

+ Diethyl sulfate = 15.3 kg

7 hrs

Ethyliodide = 15.6 kg

+ THF- solvent = 80 ltr

+ Magnesium metal = 2.5 kg

Ethylmagnesium iodide THF

Solution = 91.5 kg

Waste water 50.1

kg to ETP

[68] METHYL MAGNESIUM IODIDE - 1M SOLUTION IN THF

[A] Raw materials; Potassium hydroxide = 7 kg Iodine = 14.7 kg Formic acid = 3.5 kg Dimethyl sulfate = 14.6 kg THF solvent = 80 ltr Magnesium metal = 2.5 kg Water = 22 ltr Output 1 Molar Methyl magnesium iodide solution in THF = 96.3 kg

[B] Chemical Reaction:KI + ( CH3 )2SO4 CH3I + (CH3)KSO4CH3I + Mg + Tetrahydrofuran CH3—Mg—I in THF solvent


111

[C] Process:Charge water in a vessel and dissolve potassium iodide. Heat to elevated temperature and addsodium hydroxide to get basic pH. Add diethyl sulfate slowly. Reflux mass for few hours. Distil outproduct, i.e. Ethyl iodide. Send residual water to ETP.Charge THF followed by magnesium metal. With stirring in portions add methyl iodide. Stir atambient temperature for few hours till all metal dissolves to get clear solution. With precaution ofmoisture pack this solution as finished product.[D] Flow Sheet Diagram:

Dimethylsulfate

Residue toETP

Pure Methyl iodide

Dist.

Receiver

THF

Magnesiummetal

Methyl magnesium iodidesolution in THF solvent

WaterIodine

Pot.hydroxide

Formicacid


112

(E) Mass balance:

P otassium hydrox ide = 7 kg

Iod ine = 14.7 kg

F orm ic ac id = 3 .5 kg

W ater = 22 ltr

6 hrs P otassium iodide in water

so lu tion

+ D im ethy l su lfa te = 15.3 kg

7 hrs

M ethy liod ide = 15.6 kg

+ T H F - so lv ent = 80 ltr

+ M agnesium m eta l = 2 .5 kg

M ethy lm agnesium iod ide T H F

S olution = 96.3 kg

W aste water 48 kg

to E T P

[69] THYMOL IODIDE

[A] Raw Materials:

Thymol = 30 kg Sodium hydroxide = 16 kg Potassium hydroxide = 13.5 kg kg Iodine = 53.7 kg Formic acid = 3.1 kg Water = 190 ltr

Output of Thymol iodide = 54 kg

[B] Chemical Reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2C H 3

CH 3 C H 3

O H+ I I + KI

2

C H 3CH 3

CH 3C H 3 CH 3

C H 3OO

I

IWater / NaOH


113

[C] Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.Chill to crystallize the product. Filter product and dry in dryer. Collect mother liquor for recyclingin next batch. Process and pack the finish product. i.e. Potassium iodideCharge water then sodium hydroxide. Stir to dissolve. To this solution charge thymol and heat toelevated temperature. In separate vessel take water and add potassium iodide dissolve. Now addiodine into this solution at RT, Stir well to dissolve completely. Mix this KI/I2 solution with thymolsolution at elevated temperature. After mixing ,stir for few hours. Cool to RT. Filter. Wash wet cakewith water. M/L to drain in ETP. Dry and pack as finished product.[D] Flow Sheet Diagram:

WaterIodine

Pot.hydroxide

Formicacid

Potassium iodide

dry powder

WaterIodine

Sodium hydroxide

Water

Thymol


Dry purethymol iodide

Filter Dryer


114

(E) Mass balance:


Iodine = 28 kg


Water = 40 ltr

9 hrsPotassium iodide = 36.8 kg

M/L = 45 kgto recycle innext batch

+ Thmol = 30 kg

+ Iodine = 25.7 kg

+ Water = 150 ltr

+ Sodiumhydroxide = 16 kg

26 hrs

Thymol iodide = 54 kgWaste water M/L = 207.3 kg

to ETP

[70] 1,3 – DIIODOPROPANE

[A] Raw Materials:

1,3 – Dibromopropane = 20kg Sodium iodide = 30 kg Acetone = 250 ltr Water = 125 ltr

Output of 1.3-Diiodopropane = 28.3 kg

[B] Chemical Reaction:2 NaOH + I2 + HCOOH + Water 2 NaI + 2 H2O+ 2 NaBrBr Br + 2 NaI

AcetoneI I

[C] Process:In a vessel, charge M/L of previous batch followed by sodium hydroxide. To the clear solution, addformic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature tillcomplete conversion in to product. Concentrate the product solution to certain specific gravity.Chill to crystallize the product. Filter product and dry in dryer. Collect mother liquor for recyclingin next batch. Process and pack the finish product. i.e. Sodium iodideCharge acetone and 1,3-dibromopropane at RT. With stirring in small lots charge Sodium iodide.After complete addition, Heat to reflux for few hours. Distil out approx 50% acetone. Use thisacetone to recycle in next batch. Cool residue to RT. Separate layer , To organic layer add small


115

amount of water and distil out pure product as azeotrope mixture with water. From distillateseparate product and Dry product with sodium sulfate. Filter and pack. Water layer to drain in ETP.[D] Flow Sheet Diagram:

Sodiumhydroxide

WaterFormic acid

Iodine

1,3-Dibromopropane

Dist.receiver

Reco.acetone torecycle

Water layerto ETP

Organic layer

Water

Dist. waterto ETP

Pure 1,3-Diiodopropane

Dist.

Rec.

Water toETP

Dry sodiumiodide powder

Acetone


116

(E) Mass balance:

8 hrsSodium iodide = 30 kg M/L = 36.7 kg

to recycle

Sodium hydroxide = 9.5kg

Iodine = 25.4 kg


Water = 30 ltr

+ Acetone = 250 ltr

+ 1,3- Dibromopropane = 20 kg

+ Water = 125 ltr

24 hrs

1,3-Di iodopropane = 28.3 kg

Acetone = 221 kg distilled torecycle

Water waste = 139 kg to ETP

[71] 1 , 10-DIIODODECANE

[A] Raw Material:

1 ,10 – Decanediol =45 kg Iodine = 63.4 kg Toluene = 130 kg Phosphorous = 4.5 kg N – Heptane = 70 ltr Water = 50 ltr

Output of 1 , 10 – Diiododecane = 89 kg

[B] Chemical Reaction:5 HO-(CH2)10-OH + 2 P + 5 I2 5 I-(CH2)10-I + 2 H3PO4 + 2 H2O[C] Process:Charge toluene followed by 1 , 10 – decanediol phosphorous and iodine. Heat to reflux andmaintain for few hours. Then cool to RT , Charge water and separate layer. To toluene layer addsmall amount of water and start distillation of water + toluene. Toluene recycle in next batch afterdrying. To residue at down temperature add n-heptane and extract the product. Separate waterlater and drain in ETP. N-heptane layer collect in crystallizer to down temp. , Filter, M/L Collect torecover n-heptane. Wet cake air dry and pack.[D] Flow Sheet Diagram:


117

1,10-Decandiol

TolueneIodine

Phosphorous

Water layerto ETP

Toluenelayer

Water/Heptane

Dist.

Rec

Filter Dryer

M/L for Heptanerecovery

Distil toluene torecycle

Crystalliser

1,10-Diiodo decane

(E) Mass balance:

1,10-Decanediol = 45 kg


Iodine = 63.4 kg

Toluene = 130 kg

Water = 50 ltr

17 hrs

Crude product = 94 kgWaste water = 71 kg

to ETP

+ Heptane = 70 ltr

8 hrs

Pure 1,10-Diiodo decane = 89 kg

Heptane M/L for recovery

of solvent + 2nd crop=83.9 kg

Toluene = 119 kg recovery

[72] 2-IODOETHANOL

[A] Raw materials:

2-Chloroetanol = 10 kg DMF = 35 ltr Sodium hydroxide = 6.3 kg Iodine = 17 kg Formic acid = 4 kg Water = 140 ltr MDC = 60 ltr

Output of 2-iodoethanol = 20 kg


118

[B] Chemical Reaction:2 NaOH + I2 + HCOOH + Water 2 NaI + 2 H2OCl – CH2-CH2-OH + NaI + DMF- Solvent I-CH2-CH2-OH + NaCl[C]Process:In a vessel, charge M/L of previous batch followed by sodium hydroxide. To the clear solution, addformic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature tillcomplete conversion in to product. Concentrate the product solution to certain specific gravity.Chill to crystallize the product. Filter product and dry in dryer. Use this dry Sodium iodide in nextstep.Collect mother liquor for recycling in next batch. Charge DMF and Add 2-chloroethanol.Heat atambient temperature and in portions add sodium iodide. Maintain stirring and temperature for fewhours. Cool to RT, add water followed by MDC. Settle and separate MDC layer. Water layer to drainin ETP.MDC layer dry with the help of sodium sulfate. Distil out MDC under vacuum completely.Recovered MDC can be used for next batch. Residue liquid left is pure product, pack as Finishproduct.[D] Flow Sheet Diagram:

Sodiumhydroxide

WaterFormic acid

Iodine

Dry sodiumiodide powder

DMF

2-ChloroethanolWater/MDC

Water layerto ETP

MDC layer

Dist.

Rec

Pure 2-IodoethanolReco. MDC

to recycle


119

(E) Mass balance:

8 hrs Sodium iodide = 20 kg M/L = 33 kg torecycle


Iodine = 17 kg

Formic acid = 4 kg

Water = 30 ltr

2-Chloro ethanol = 10 kg

DMF = 35 ltr

Water = 110 ltr

MDC = 60 ltr

23 hrs

2-Iodoethanol = 20 kg

Recovered distilled

MDC = 64 kg torecycle


[73]1-BROMO 2-IODOBENZENE

[A] Raw Materials:

2-Bromo aniline = 8.7 kg Hydrochloric acid = 42 ltr Sodium nitrite = 4.5 kg Potassium hydroxide = 4.8 kg Iodine = 10.2 kg Formic acid = 2 kg MDC =5 ltr Water = 19 ltr

Output of 1-Bromo 2-iodobenzene= 12.2 kg[B] Chemical Reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

N H 2

B r+ NaNO 2 + KI HCl / Water B r

I

+ +KCl NaCl


120

[C] Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to a mixture of water + HCl , add 2- Bromo aniline and stir to dissolve. Chill solution and slowlyadd sodium nitrite solution. After complete addition, Stir for few minutes at down temperature.Prepare potassium iodide solution in water and transfer above mass int this solution at RT. Stir andheat for few minutes at elevated temperature Cool and chill to low temperature. Separate layer.Organic layer mix with MDC Washed with water + caustic soda solution. Separate layers. FromMDC layer distil out MDC completely. Residue product mixed with water and distillation purifiedand pack.[D] Flow Sheet Diagram:

H ydrochloricac id

2-B rom oaniline

S odium nitriteW ater

M D C

M D Clayer

W ater layerto E T P

D ist.R ec.

D istilled M D C to recyc le

D istilled waterto recyc le

P ure2-B rom o-1-iodobenzene

W ater

D ist.

R ec.

W aterIod ine

P ot.hydrox ide

F orm icac id

P otassium iod ide in water


121

(E) Mass balance:

Potassiumhydroxide = 4.8kg

Iodine = 10.2 kg

Formic acid = 2 kg

Water = 19 ltr


in water

+ 2-Bromo aniline = 8.7 kg



+ MDC = 5 ltr

13 hrs

1-Bromo-2-iodo benzene = 12.2 kg

Distilled MDC = 5kg to recycle

Waste water = 79 kg

to ETP

[74]1-BROMO 4-IODOBENZENE

[A] Raw Materials:

4- Bromoaniline = 8.0 Kg Hydrochloric acid =24 ltr Sodium nitrite = 4.3 kg Potassium hydroxide = 4.7 kg Iodine = 10.1 kg Formic acid = 1.6 kg MDC = 5 ltr Water = 25 ltr

Output of 1-bromo 4-iodobenzene = 12 kg

[B] Chemical Reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2N H 2

B r

+ NaNO 2 + KI HCl / Water

B r

I

+ +KCl NaCl

[C] Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature


122

till complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to a mixture of water + HCl, Add 4- bromo aniline and stir to dissolve. Chill solution to 0 Celsiusand slowly add sodium nitrite solution. After complete addition, Stir for few minutes at downtemperature. Prepare potassium iodide solution in water and transfer above mass into thissolution at RT. Stir and heat for few minutes at elevated temperature Cool and chill to lowtemperature. Separate layer. Organic layer mix with MDC Washed with water + caustic sodasolution. Separate layers. From MDC layer distil out MDC completely. Residue product mixed withwater and distillation purified and pack.[D] Flow Sheet Diagram:

Hydrochloricacid

4-Bromoaniline

SodiumnitriteW ater

MDC

MDClayer

W ater layerto ETP

Dist.Rec.

Distilled MDC to recycle

Distilled waterto recycle

Pure1-Bromo-4-iodobenzene

W ater

Dist.

Rec.

W aterIodine

Pot.hydroxide

Form icacid



123

(E) Mass balance:


Iodine = 10.1 kg

Formic acid = 2 kg

Water = 25 ltr


in water

+ 4-Bromo aniline = 8 kg



+ MDC = 5 ltr

11 hrs

1-Bromo-4-iodo benzene = 12.kg

Distilled MDC = 5kg to recycle


[75] 3-IODO-N-PHENYL CARBAZOLE

(A) Raw materials:

3-Amino-N-phenyl carbazole = 26 kg Dilute sulphuric acid = 110 ltr Water = 45 ltr Sodium nitrite = 7.0 kg Potassium hydroxide = 7.7 kg Iodine = 16.4 kg Formic acid = 3 kg Methylene dichloride = 50 ltr

Output of 3-Iodo-N-phenyl carbazole = 32.7 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

N

N H 2

+ +NaNO 2KI

N

I

K 2 SO 4

Na 2 SO 4

++

Dil. sulfuricacid


124

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to chilled dilute sulfuric acid, slowly add and dissolve 3-Amno-N-phenyl carbazole. To thismixture add sodium nitrite water solution and stir for few minutes. Now treat this reaction masswith a potassium iodide solution in water at elevated temp. Stir for few hours. Extract product inMDC and separate layers. Send water layer for Iodine recovery and then to ETP. MDC layer take in adistillation assembly and distil out MDC completely to get pure dry product. Further dry it in dryerto remove traces of MDC. Pack the finish product.(D) Flow sheet diagram:

Water

Dil sulfuricacid

Waste water to

ETP

3-IODO-N-PHENYLCARBAZOLE

Sodiumnitrite

3-Amino-N-phenylcarbazole

MDC

Reco. MDC torecycle

Dist

Rec.

Dryer

WaterIodine

Pot.hydroxide

Formicacid



125

(E) Mass balance:


Iodine = 16.4 kg

Formic acid = 3 kg

Water = 45 ltr

3 hrs Potassium iodide = 21 kg

in water

+ 3-Amino-N-phe.carbazole = 26 kg

+ Dil Sulfuric acid = 110 kg


+ MDC = 50 ltr

17 hrsDistilled MDC =50 kg to recycle

3-Iodo-N-phenyl carbazole = 32.7 kgWaste water = 182.4kg to ETP

[76] 4-FLUORO IODOBENZENE

(A) Raw materials:

4-Fluoroaniline = 14.0 kg Hydrochloric acid = 56 ltr Water = 75 ltr Sodium nitrite = 8.80 kg Potassium hydroxide = 9.1 kg Iodine = 19.3 kg Formic acid = 3.5 kg MDC Solvent = 75 ltr

Output of 4-Fluoro iodobenzene = 25.5 kg(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

N H 2

F

+ NaNO 2 + KI HCl / Water

I

F

+ +KCl NaCl


126

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to a mixture of water + HCl , Add 4-Fluoro aniline and stir to dissolve. Chill solution and slowlyadd sodium nitrite solution. After complete addition, Stir for few minutes at down temperature.Prepare potassium iodide solution in water and transfer above mass into this solution at RT. Stirand heat for few minutes at elevated temperature Cool and chill to low temperature. Separatelayer. Organic layer mix with MDC Washed with water + caustic soda solution. Separate layers.From MDC layer distil out MDC completely. Residue is pure product. Collect and pack.(D) Flow sheet diagram:

WaterHCl

Waste water to

ETP

Sodiumnitrite

4-Fluoroaniline

MDC

Reco. MDC torecycle

Dist

Rec.

WaterIodine

Pot.hydroxide

Formicacid


MDC layer

4-Fluoro iodobenzene


127

(E) Mass balance:


Iodine = 19.3 kg


Water = 75 ltr

5 hrs Potassium iodide = 24.8kg in water

+ 4-Fluoro aniline = 14 kg

+ Hydrochloric acid = 56 kg


+ MDC = 75 ltr

13 hrsDistilled MDC =70 kg to recycle

4-Fluoro iodobenzene = 25.5 kgWaste water = 155.2kg to ETP

[77] 2-NITRO IODOBENZENE

(A) Raw materials:

2-Nitroaniline = 14.0 kg Water = 65 ltr Hydrochloric acid = 60 ltr Sodium nitrite = 7.0 kg Potassium hydroxide = 9.3 kg Iodine = 19.5 kg Formic acid = 3.8 kg MDC Solvent = 25 ltr

Output of 2-Nitroiodobenzene = 22.1 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NH2

N+

O-

O

+ NaNO2 + KIHCl / Water

IN

+

O-

O

+ +KCl NaCl


128

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to a mixture of water + HCl , Add 2-Nitro aniline and stir to dissolve. Chill solution and slowlyadd sodium nitrite solution. After complete addition, Stir for few minutes at down temperature.Prepare potassium iodide solution in water and transfer above mass into this solution at RT. Stirand heat for few minutes at elevated temperature Cool and chill to low temperature. Separatelayer. Organic layer mix with MDC Washed with water + caustic soda solution. Separate layers.From MDC layer distil out MDC completely. Residue product mixed with water and on distillationpurified product will obtain. Separate distilled water from product and recycle water in next batch,collect pure product and pack.(D) Flow sheet diagram:

Hydrochloricacid

2-Nitroaniline

SodiumnitriteWater

Water layer to ETP

Dist.

Rec.

Distilled MDC to recycle

Distilled water to ETP 2-Nitro iodobenzene

Water

Dist.

Rec.

WaterIodine

Pot.hydroxide

Formicacid


MDC

MDC Layer


129

(E) Mass balance:


Iodine = 19.5 kg


Water = 75 ltr

5 hrsPotassium iodide = 23.8kg in water

+ 2-Nitro aniline = 14 kg

+ Hydrochloric acid = 60 kg


+ MDC = 25 ltr

15 hrsDistilled MDC =26.5 kg to recycle

2-Nitro iodobenzene = 22.1 kgWaste water = 155kg to ETP

[78] 2-IODO ANILINE

(A) Raw materials:

2-Nitro iodobenzene = 22.1 kg Sodium sulfide = 57.0 kg Methanol = 50 ltr Water = 100 ltr Toluene solvent = 60 ltr

Output 2-Iodoaniline = 16 kg(B) Chemical reaction:

I

N+ O

-O

+ Na2SMethanol / Water

INH2

+ +Na2S2O4 H2O


130

(C) Process:Take water and dissolve sodium sulfide at room temp. Heat this solution at elevated temp andslowly drop wise add solution of 2-Nitro iodobenzene in methanol. After addition, reflux wholemass for few hours.Cool reaction mass to down tem and filter the formed slurry, wash wet cake of crude product withlittle water. Drain M/L to ETP. Take crude wet cake in toluene and dissolve. Wash organic layerwith water and separate layers. Distil out toluene from washed organic layer under high vacuum toget residue as totally dry powder. Collect dry pure product and pack. Distilled toluene recycle innext batch.(D) Flow sheet diagram:

Water

SodiumsulfideMethanol

2-Nitro iodobenzene

M/L toETP Water layer

to ETP

Toluenelayer

Wetcake

Toluene

Pure 2-Iodoaniline

Distilled tolueneto recycle

Dist.

Rec.

Filter

(E) Mass balance:

2-Nitro iodobenzene = 22.1 kg

Sodium sulfide = 57 kg

Methanol = 50 ltr

W ater = 90 ltr

11 hrsCrude product = 17 kg

Recovered distilled

methanol 32 kg to recycle

W ater waste = 180 kg

to ETP

+ Toluene = 60 ltr

+ W ater = 10 ltr Distilled recovered toluene

to recycle = 49 kg

Pure 2-Iodo aniline = 16 kg W ater waste = 12.1kg to ETP

5 hrs


131

[79] 2-BUTYL-3(3,5-DIIODO-4-HYDROXY BENZOYL)BENZOFURAN

(A) Raw materials:

2-Butyl-3(4-hydroxybenzoyl)benzofuran (BBF) = 60 kg Methanol = 190 ltr Sodium acetate = 53 kg Iodine = 123 kg Sodium hydroxide = 18 kg Sodium bisulfite = 16.0 kg Hydrochloric acid = 35 kg Toluene = 120 ltr Water = 150 ltr Charcoal = 5.0 kg

Output of Finish product = 110.0 kg


O CH3

O

OH

+ +Iodine CH3COONa

O CH3

O

OH

I

I

Methanol / Water

(C) Process:Charge methanol and BBF in a vessel, with stirring charge iodine and heat mass to elevated temp.Now charge in portions, sodium acetate. Stir as such for few hrs and then further heat to reflux.Maintain reflux for few hrs till completion of reaction. Cool mass to down temp and add sodiumbisulfite solution and stir for few minutes.Add sodium hydroxide solution to get almost basic pH. Stir for few minutes at down temp. Nowneutralise pH to almost 7 by adding hydrochloric acid. Filter crude product slurry. M/L send to ETPafter iodine recovery. Unload wet cake and in a vessel, mix with toluene. Heat to dissolvecompletely. Add charcoal and maintain for few minutes. Filter hot through filter aid and get clearfiltrate. Cool filtrate to down temp to isolate pure product crystals. Filter formed slurry of product.Send M/L for second crop and toluene recovery. Dry wet cake and pack finish product.


132


Methanol

BBFIodine

Sodium acetate / Sodium hydroxide

Sodium bisulfite / HCl

Filter

M/L to ETP afteriodidne recovery

Toluene /Charcoal

Crude

Filter

Dryer

Dry pure DIBF

Filter

M/L for toluene /second crop recovery

(E) Mass balance:

BBF = 60 kg

Methanol = 190 ltr

Sodium acetate = 53 kg

Iodine = 123 kg


Sodium bisulfite = 16 kg

W ater = 150 ltr


M/L for m ethanol &Iodine recovery = 231kg

W aste water = 330kg to ETP

+ Toluene = 120 ltr

+ Charcoal = 5 kg

8 hrs

Pure DIBF = 110 kg

Charcoal solid waste = 5 kg


= 94 kg


133

[80] METHYL AMMONIUM IODIDE

(A) Raw materials:

40% Monomethylamine = 80 kg Iodine = 135 kg Phosphorus = 6.7 kg Water = 392 ltr Toluene solvent = 760 ltr

Output of product = 153 kg

(B) Chemical reaction:3 I2 + 6 H2O + 2 P 6 HI + 2 H3PO4CH3NH2 + HI CH3NH3+ I-(C) Process:Charge iodine followed by phosphorous. In portions add water and heat to elevated temperaturefor few hours. Start distillation when all iodine dissolved. Separate low density HI fraction duringdistillation. Collect the main fraction of HI and use in next step. Low density fraction + residuerecycle in next batch.In a vessel charge mono methyl amine solution and cool to down temp. To this slowly addhydriodic acid to get neutral pH. Stir few hrs at down temp. Add toluene and start water + tolueneazeotrope distillation. After complete removal of water, cool product slurry to down temp. Filterpure product slurry and wash with little toluene. Send M/L for toluene recovery. Unload wet cakeand dry in dryer. After drying, pack finish product.


134


Water

Phosphrous

Iodine

Dist.

Rec.

Low strengthproduct for recyclePure Hydriodic acid

Residue to recyclein next batch

Monomethylamine

Filter Dryer

Dist.

Rec.

Recover toluene to recycle

Methylammoniumiodide

Toluene



135

(E) Mass balance:

Iodine = 135 kg

Water = 392 ltr


38 hrsHydriodic acid= 230 kg Distillate +residue to


= 140.7 kg

+ Monomethyl amine = 80 kg

+ Touene = 760 ltr

12 hrs

Water distilled 392 Kg

to ETP

Methyl ammonium iodide = 153 kg M/L for toluene recovey &recycle = 688 kg

[81] 1,3-DIIODO BENZENE

(A) Raw materials:

Meta phenelyne diamine = 60 kg Sodium nitrite = 80 kg Potassium hydroxide = 47 kg Iodine = 100 kg Formic acid = 19 kg Dilute sulphuric acid = 138 kg Toluene solvent = 250 ltr Water = 150 ltr

Output of 1,3-Diiodo benzene = 152.8 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2N H 2

NH 2

+ +2 NaNO 2 2 KIDil. sulfuric acid

I

I

++

2 Na 2 SO 4

2 K 2 SO 4

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperature


136

till complete conversion in to product. Concentrate the product solution to certain specific gravity.This solution is ready to use in next step.In to dilute sulphuric acid, dissolve meta phenelyne diamine and cool to down temp. Now slowlyadd solution of sodium nitrite and then stir for few minutes. Then add potassium iodide solution into this reaction mass. Stir mass few hrs at room temp and then heat to elevated temp for few hrs tocomplete the reaction. Cool to down temp and then add toluene to extract the product in toluene.Separate layers. Send water layer to ETP. Take toluene layer in distillation assembly and distil outtoluene completely under vacuum. To the almost dry residue, add methanol. Cool formed slurry tovery down temp and then filter. Send M/L for methanol + second crop recovery. Unload wet cakefrom filter and dry in dryer, then pack the finish product.(D) Flow sheet diagram:

W aterIodine

Pot.hydrox ide

Form icacid


M PDA

Dil.Sulfuricacid

Toluene

W ater layerto ETP

Toluene layer

M ethanol

D ist.

Rec.

Toluene to recycle

F ilter Dryer

1,3-D iiodo benzene

Sodium nitrite


137

(E) Mass balance:


Iodine = 100 kg

Formic acid = 19 kg

Water = 150 ltr

15 hrsPotassium iodide = 128 kgin water

+ MPDA = 60 kg

+ Dil Sulfuric acid =138 kg


+ Toluene = 250 ltr

19 hrs Distilled Tolueneto recycle =194.2 kg

1,3-Di iodobenzene = 152.8 kgWaste water = 497kg to ETP

[82] 5-IODO URACIL

(A) Raw materials:

Uracil = 25 kg Sodium hydroxide = 47.6 kg Iodine = 48.8 kg Acetic acid = 75 kg Water = 190 ltr

Output of 5-Iodo uracil = 47.3 kg


NH

NH

O

O

+ Iodine + NaOHWater

NH

NHI

O

O

+ NaI + H2O


138

(C) Process:In a vessel, charge water and dissolve sodium hydroxide in it. Then charge uracil and stir for fewminutes. Heat mixture to elevated temp and charge iodine. Stir for few hrs at elevated temp tocomplete reaction. Product slurry formed, neutralise it with acetic acid at down temp. Filter theproduct slurry and take wet cake in water. M/L send for ETP. Heat wet cake + water mixture forfew hrs. Cool and filter the pure product. Send water M/L to ETP. Dry wet cake in dryer and packthe finish product.(D) Flow sheet diagram:

WaterSodiumhydroxide

Uracil

Iodine

FilterFilter

M/L to Aceticacid recoverythen to ETP

M/L to ETP

Dryer 5-Iodo uracil

Water

Acetic acid

(E) Mass balance:

Water = 110 ltr


Iodine = 48.8 kg

Uracil = 25 kg

Acetic acid = 75 kg


M/L waste water = 254.1kg for Acetic acidrecovery then to ETP

+ Water = 80 ltr

5 hrs

Pure 5-Iodo uracil = 47.3 kgM/L waste water = 85 kg

to ETP


139

[83] 1,4-DIIODO BUTANE(A) Raw materials:

Potassium hydroxide = 8.9 kg Iodine = 18.7 kg Formic acid = 4.2 kg Water = 28 ltr Phosphoric acid = 17 kg Tetra hydro furan = 30 kg MDC solvent = 18 ltr 5% Sodium bisulfite = 10 ltr

Output of 1,4-Diiodo butane = 19 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2

O+ 2 KI + H3PO4

I I

+ K2HPO4

+ H2O

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.Cool and filter formed slurry of product. Send M/l to use in next batch. Dry wet product in dryerand use in next step.Charge tetrahydro furan, then phosphoric acid and potassium iodide. Heat reaction mass atelevated temp for few hrs. Cool to down temp and MDC. Settle and separate layers. Send waterlayer to ETP. Take MDC layer in vessel and wash it with 5% sodium bisulfite water solution.Separate layers. Send water layer to ETP. Distil out MDC from organic layer completely undervacuum. Residue is pure 1,4- Diiodobutane. Pack this finish product.


140


W a te rIo d in e

P o t .h y d ro x id e

F o rm ic a c id

P o ta s s iu m io d id e d ry p o w d e r

P h o s p h o r ic a c id

T e tra h y d ro f u ra n

M D C

M D Cla y e rW a te r la y e r

to E T P

S o d iu m b is u l f i teS o d iu m s u l f a te

D is t .

R e c .

F i l te r

W a te r la y e r to E T P

1 ,4 -D i io d o b u ta n e

M D C to re c y c le

M /L u s e in n e x t b a tc h

(E) Mass balance:Potassiumhydroxide = 8.9kg

Iodine = 18.7 kg


Water = 28 ltr


+ Tetrahydrofuran = 30 kg

+ Phosphoric acid = 17 kg

+ MDC = 18 ltr

19 hrs M/L for MDC +THF recovery =63.8 kg

+ 5% SBS solution = 10 ltr

Waste water = 16 kg

to ETP

M/L = 36 kg torecycle in next batch

1,4- Diiodo butane = 19 kg


141

[84] 2-IODOACETIC ACID

(A) Raw materials:

Chloro acetic acid = 50 kg Potassium hydroxide = 40 kg Iodine = 84 kg Formic acid = 16 kg Water = 270 ltr MDC solvent = 150 ltr

Output of 2-Iodoacetic acid = 77.7 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2O

OHCl+ KI

MDC O

OHI

KCl+Water

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.Cool and filter formed slurry of product. Send M/l to use in next batch. Dry wet product in dryerand use in next step.Charge MDC then Chloroacetic acid and with stirring add potassium iodide and reflux mixture forfew hrs. Cool to down temp and add water. Separate layers. Send water layer to ETP. From MDClayer, distil out MDC completely to get dry powder product. Add little fresh MDC to product andchill slurry and filter. Send M/L for second crop and MDC recovery. Dry wet cake of product andpack as finish product.


142


W aterIodine

Pot.hydrox ide

Form icacid

Potassium iodide dry powder M /L use in nex t batch

Chloroaceticacid

M DC

W ater

W ater to ETP

M /L for recov ery of2nd crop + M DC

Dist.

Rec.

M DC layerF ilter

D istlled M DC to recycle

Dryer 2-Iodo aceticacid

(E) Mass balance:


Iodine = 84 kg

Formic acid = 16 kg

Water = 120 ltr


+ 2-Cloroaceticacid = 50 kg

+ Water = 150 ltr

+ MDC = 150 ltr

21 hrsWaste water =117 kg to ETP

2-Iodo acetic acid = 77.7 kg M/L for recycle MDC& second croprecovery = 275.3 kg

M/L = 140 kg torecycle in next batch


143

[85] 3- IODO PYRIDINE

(A) Raw materials:

3-Amino pyridine = 8.0 kg Sodium nitrite = 7.3 kg Potassium hydroxide = 0.7 kg Iodine = 1.5 kg Formic acid = 0.3 kg Water = 10 ltr EDC solvent = 5 ltr Hydrochloric acid = 24 ltr

Output of 3-Iodo pyridine = 15.4 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NaNO2 KI

Hydrochloricacid

KClNaClN

NH2

+ +N

I

+ ++ 2H2O 1/2 N2+

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This potassium iodide solution is ready for next step.In a mixture of hydrochloric acid and water, charge 3-amino pyridine at cold temp. Add sodiumnitrite solution in it at down temp. Stir for few minutes and then add solution of potassium iodideand stir for few hrs at high temp. Now add EDC and extract product. Separate layers. Send waterlayer to ETP. Wash EDC layer with water. Distil out EDC form organic layer completely under highvacuum till thick slurry remains as residue. Chill formed slurry to down temp and filter the pureproduct. Send M/L for EDC + 2nd crop recovery. Wet cake dry in dryer and pack powder as purefinish product.


144


W aterIodine

Pot.hydroxide

Form icacid


3-Am inopyridine

HClSodium nitrite

W ater to ETP

EDC layer

M/L for EDCrecovery

Dist.

Rec.

Distilled EDC to recycle

Filter

Dryer 3-Iodo pyridine

EDC

(E) Mass balance:

Potassium hydrox ide =0.7 kg

Iodine = 1.5 kg

Form ic acid = 0.3 kg

W ater = 2 ltr


in water

+ 3-Am ino pyridine = 8 kg

+ HCl = 24 ltr


+ W ater = 10 ltr

+ EDC solv ent = 5 ltr

8 hrs W aste water =38 kg to ETP

3-Iodo pyridine = 15.4 kg M /L for recycle EDC& second croprecov ery = 3.4 kg


145

[86] 4- IODO PYRIDINE

(A) Raw materials:

4-Amino pyridine = 8.0 kg Sodium nitrite = 7.3 kg Potassium hydroxide = 0.7 kg Iodine = 1.5 kg Formic acid = 0.3 kg Water = 10 ltr EDC solvent = 5 ltr Hydrochloric acid = 24 ltr

Output of 4-Iodo pyridine = 16.2 kg

(B) Chemical reaction:2 KOH + I2 + HCOOH + Water 2 KI + 2 H2O + CO2NaNO2 KI

Hydrochloricacid

KClNaClN

NH2

+ +N

I

+ ++ 2H2O 1/2 N2+

(C) Process:In a vessel, charge M/L of previous batch followed by potassium hydroxide. To the clear solution,add formic acid at room temp. With stirring charge iodine at elevated temp. Maintain temperaturetill complete conversion in to product. Concentrate the product solution to certain specific gravity.This potassium iodide solution is ready for next step.In a mixture of hydrochloric acid and water, charge 4-amino pyridine at cold temp. Add sodiumnitrite solution in it at down temp. Stir for few minutes and then add solution of potassium iodideand stir for few hrs at high temp. Now add EDC and extract product. Separate layers. Send waterlayer to ETP. Wash EDC layer with water, soda ash dilute solution and finally with dilute sodiumbisulfite solution. Distil out EDC form organic layer completely under high vacuum till thick slurryremains as residue. Chill formed slurry to down temp and filter the pure product. Send M/L forEDC + 2nd crop recovery. Wet cake dry in dryer and pack powder as pure finish product.


146


WaterIodine

Pot.hydroxide

Formicacid


4-Aminopyridine

HClSodiumnitrite

Water to ETP

EDC layer

M/L for EDCrecovery

Dist.

Rec.


Filter

Dryer 4Iodo pyridine

EDC


147

(E) Mass balance:

Potassiumhydroxide =0.7 kg

Iodine = 1.5 kg


Water = 2 ltr


in water

+ 4-Amino pyridine = 8 kg

+ HCl = 24 ltr


+ Water = 8 ltr

+ EDC solvent = 5 ltr

8 hrs Waste water =37 kg to ETP

4-Iodo pyridine = 16.2 kg M/L for recycle EDC& second croprecovery = 3.6 kg

[87]IODOPHOR

(A) Raw Materials:

Iodine = 25 kg Phosphoric acid = 2.0 kg Water = 100 ltr Phosphate buffer (pH-7) =25 kg Potassium iodide = 25 kg

Output of Iodophor solution = 177 kg

(B) Chemical reaction:Iodine + Water + Phosphoric acid ( stabiliser) + Potassium iodide + Buffer Iodophor(C) Process:Dissolve phosphate buffer powder in water. Add slowly iodine followed by potassium iodide andstir for few hours at elevated temperature, till the mixture becomes homogeneous. Adjust pH toalmost neutral by adding phosphoric acid. To this solution add extra water to get desired strengthof iodine in formed solution.Pack this solution in packing utensil.


148


WaterIodine

Pot.hydroxide

Formicacid


Water

Buffer

Iodine

Phosphoric acid

Iodophor solution

(E) Mass balance:

Water = 100 ltr

Potssiumiodide= 25 kg

Iodine = 25 kg

Phophoric acid = 2 kg

Buffer = 25 kg

Iodophorsolution in waterapprox 177 kg

28 hrs


149

[88] POVIDONE – IODINE POWDER

(A) Raw Materials:

Iodine = 50 kg Phosphate buffer powder = 120 kg

Output of Povidone iodine powder = 170 kg

(B) Chemical reaction:Phosphate buffer powder + Iodine Povidone - iodine(C) Process:Charge Phosphate buffer powder in rotator drum mixture. Add iodine and mix for few hours atelevated temperature, till the mixture becomes homogeneous powder. Send sample of uniformpowder for iodine content. When desired iodine content is achieved of homogeneous powder, packthe finish product in packing utensil.(D) Flow sheet diagram:

Buffer

Iodine

Povidone - iodine powder

Rotacondrum

mixer

(E) Mass balance:

Buffer = 120 kg

Iodine = 50 kg

Povidone-iodinePowder approx170 kg

130 hrs


150

[89] 4-BROMO-2-IODO ANILINE:

(A) Raw material:1. 4-Bromo aniline = 14.3 kg2. Iodine monochloride = 13.5 kg3. Acetic acid = 68 kg4. MDC = 68 kgOutput of 4-Bromo-2-iodo aniline = 22.3 kg.(B) Chemical reaction:

Br

NH2

+I Cl

Br

NH2

I

+ ClH

(C) Process:In a clean and dry vessel, charge Acetic acid followed by 4-Bromoaniline. Heat to warm temp andslowly add Iodine monochloride. Maintain reaction mass for few hrs at same temp and then cool todown temp.Filter the formed product. Collect M/L for Acetic acid recovery + second crop of product. Wash wetcake with chilled MDC. Collect washing M/L for MDC recovery. Dry wet cake and pack.(D) Flow sheet diagram:

4-Bromoaniline

Aceticacid Iodinemonochloride

MDC

M/L for 2nd crop + Solventsrecovery

Filter Dryer 4-Bromo-2-iodo aniline


151

(E) Mass balance:

Aceticacid = 68 kg

4-Bromoaniline = 14.3 kg

Iodinemonochloride = 13.5 kg

8 hrs4-Bromo-2-iodo aniline= Crude = 23 kg

+ MDC = 68 kg

Pure = 22.3 kg

M/L for solvent &

2nd crop recovery

= 73.5 kg

M/L for MDC recovery

= 68 kg

1 hr

[90] DIIODO ETHAN

(A) Raw material:1. Acetylene = 36 kg2. Hydriodic acid = 201 kgOutput of Diiodoethane = 120 kg(B) Chemical reaction:

CH CH + 2 HI ICH2CH2I

(C) Process:In a clean vessel, charge hydriodic acid and with stirring cool to down temp. Slowly pass acetylenewith maintaining temp down. Check reaction mass to completion of reaction. Stir for few hrs. Atdown temp., filter mass. Wash wet cake with water. Send M/L for recovery of hydriodic acidthrough water distillation. Dry product wet cake in dryer. Pack after quality analysis.(D) Flow sheet diagram:

H y d r i o d i c a c i d A c e t y l e n e

M / L f o r w a t e r d i s t i l l a t i o n a n dH I r e c o v e r y

D r y e rF i l t e r D i i o d o e t h a n e


152

(E) Mass balance:

Hydriodic acid = 201 kg

Acetylene = 36 kgDiiodoethane = 120 kg Dilute hydriodic acid to distill

and recover = 117 kg11 hrs

[91] 6- IODO INDAZOLE

(A) Raw material:1. 6-Amino indazole = 9.2 kg2. Potassium iodide = 17.3 kg3. Sodium nitrite = 5.8 kg4. HCl = 25 kg5. Ethyl acetate = 45 kg6. Water = 37 ltrOutput of 6-Iodo indazole = 12.8 kg


NNHNH2

+ +NaNO2 KI HCl NNHI

+ NaCl KNO2

+

+

(C) Process:Charge HCl and water in a vessel and then charge 6-Amino indazole. Cool solution to down temp.With stirring add solution of sodium nitrite to make clear diazo solution.In another vessel, charge water and add potassium iodide and get a clear solution. Warm thissolution and add above made diazo solution. Stir for few hrs and then heat and maintain heatingfor few hrs.Cool to RT and extract product in Ethyl acetate. Separate layers. Send aqueous layer to ETP. DryEthyl acetate layer over sodium sulfate and under vacuum distil out ethyl acetate completely to getdry powder of product. Recycle distilled ethyl acetate in next batch. Dry further product in dryer.Pack it after drying.


153


Water

HCl

6-Aminoindazole

Sodiumnitrite solutionPotassiumiodide solution

Ethyl acetate

6-IodoindazoleDistilledethylacetate

to recycle

Dist.

Rec.

(E) Mass balance:

Water =18 ltr

HCl = 25 kg

6-Aminoindazole= 9.2 kg

Sodiumnitrite = 5.8 kg in8 ltr water

2 hrs

+ Potassium iodide = 17.3 kgin 11 ltr water

Etyl acetate = 45 ltr

Water = 85.5 kg toETP

6-Iodo indazole = 12.8 kg Distilled ethyl acetate = 41 kgto recycle


154

[92] 3-IODO BENZOTRIFLUORIDE(A) Raw material:1. 3-Trifluoro methyl aniline = 8.5 kg2. Potassium iodide = 13.2 kg3. Sodium nitrite = 4.0 kg4. HCl = 33 kg5. EDC = 43 ltr6. Water = 40 ltrOutput of 3-Iodo benzotrifluoride = 12.2 kg(B) Chemical reaction:

NH 2

F

F

F

+ NaNO 2 + HCl KI+F

F

F

I

KNO 2NaCl+ +

(C) Process:In a clean vessel, charge water and then charge HCl. Add 3-Tri fluoromethyl aniline and dissolve.Chill to down temp and slowly add solution of sodium nitrite.In another vessel, make potassium iodide solution in water. Add above clear diazo solution in thispotassium iodide solution. Heat to elevated temp and maintain for few hrs. Now cool the formedproduct mass to RT and add EDC to extract the product in EDC layer. Send water layer to ETP. TakeEDC layer and dry over sodium sulfate. Distil out EDC under vacuum completely to get oily residueof product. Now add water to the residue and steam distil pure product with water. Collect pureproduct from receiver and pack.(D) Flow sheet diagram:

3-Trifluoroaniline

Water

HCl Sodiumnitrite solutionPotassiumiodide solution

EDC

Water layer to ETP3-Iodobenzotrifluoride

Water

Distilledwater

to recycle

Dist.

Rec.


155

(E) Mass balance:

3-Trifluoroaniline = 8.5 kg

Water = 22 ltr

HCl = 33 kg

Sodiumnitrite = 4.0 kg

+ Potassiumiodide = 13.2 kg

+ Water = 14 ltr

+ EDC = 43 ltr

Water = 115.6 kg toETP

+ Water = 10 ltr

3-Iodobenzotrifluoride = 12.2 kg Distilled water to

recycle = 14 kg

[93] 3-IODO ANILINE

(A) Raw material:1. 3-Nitro aniline = 13.8 kg2. Potassium iodide = 16.5 kg3. Iodine = 15.5 kg4. Iron powder = 7.4 kg5. Sodium nitrite = 7.0 kg6. EDC = 20 kg7. HCl = 28.0 kg9. Ammonia solution = 2.5 ltr10. Chloroform = 32.5 kg11. Methanol = 4.5 ltr12. Water = 45 ltrOutput of product 3-Iodoaniline = 17 kg


156


NH2

N+

O-

O

+ NaNO2 HCl KI+ +N

+

O-

O

I

+ +KNO2 NaCl

N+

O-

O

I

+ Fe2+ + HCl

Methanol/ Ammonia

Water/Chloroform

I

NH2

+ Fe2O3

(C) Process:In a vessel, charge water followed by HCl and then with stirring charge 3-Trifluoro anilne. Coolmass to down temp. Add solution of sodium nitrite at down temp to get a clear diazo solution. Inanother vessel, prepare potassium iodide solution at RT and add above made diazo solution in tothis solution. Stir at RT for few hrs then heat to elevated temp and maintain for few hrs. Cool massof product to RT and add EDC to extract intermediate product. i.e. 3-Iodo-nitrobenzene.Separate layers. Water layer send to ETP for treatment. Take EDC layer and distil out EDC undervacuum to get oily residue as crude intermediate. Add water & methanol and then with stirring addiron powder and at last add HCl. Heat to reflux and maintain for few hrs. Cool to RT and adjust pHslight basic using ammonia solution. Filter mass. Take wet cake and dry in dryer.Charge dry powder in chloroform and with heating extract product in chloroform. Filter hotthrough sparkler and wash wet cake with additional chloroform. Discard wet cake of iron to ETP.Collect M/L and under vacuum distil out chloroform to get pure oil as residue. Recycle distilledchloroform in next batch and collect residual pure oily product and pack.


157


2-Nitroaniline

Water

HCl Sodiumnitrite solutionPotassiumiodide solution

EDC

Water layer to ETP

Water/Methanol

Dist.

Rec.

Distilled EDC

to recycle

Iron / HCl

Filter

DryerChloroform

Filter

Wet cake to Solid waste

3-Iodo aniline

Dist.

Rec.

Distilled

chloroform torecycle


158

(E) Mass balance:

3-Nitroaniline = 13.8 kg

Water = 18 ltr

HCl = 26 kg

Sodium nitrite = 7.0 kg

+ Potassium iodide = 16.5 kg

+ EDC = 20 kg

Water layer = 92.2 kg to ETP


= 20 kg

Intermediate product3-Iodonitrobenzene =14.4 kg

+ Water = 27 ltr

+Methanol = 4.5 ltr

+Iron powder = 7.4 kg

+HCl = 2.0 kg

+ Ammonia = 2.5 ltr

+ Chloroform = 32.5 kg

Solid waste = 18.5kg

3-Iodoaniline = 12.2 kg Distilled chloroform

to recycle = 30 kg


159

2.5 DETAILS OF AIR POLLUTION MANAGEMENT

Sr. No Source Fuel Height Parameter

1. Thermic Fluid heater(3 Lac K.Cal) – Existing

Wood 15 m

ParticulatematterSO2

NOx

2 Thermic Fluid heater(3 Lac K.Cal) – Proposed

Wood/Agrowaste 15 m

3 Hot Water Generator(250 lit/hr) - Existing

Coal 09 m

4 Hot Water Generator(250 lit/hr) – Proposed

Coal/Agrowaste 09 m

5 D. G. Set (500 KVA) X 2 Nos. Diesel 8 m

2.6 DETAILS OF WATER AND WASTEWATER

Water consumption

Sr.No Activity/area Existing Proposed

changeProposedchange

1. Domestic 0.800 1.200 2.0002 Boiler 2.540 2.460 5.0003 Cooling 0 2.000 2.0004 Process 2.930 3.070 6.0005 Others 1.000 1.000 2.000

Total 7.270 9.730 17.000

Wastewater generation

Sr.No Activity/area Existing Proposed

changeProposedchange

1. Domestic 0.2 1.3 1.52 Boiler 0 0.5 0.53 Cooling 0 0 04 Process 0.5 4.5 5.05 Others 0 0 0

Total


160

2.7 UTILITIES REQUIREMENTAll utilities required for the project would be developed in the existing

facility and the utility requirements are as under.

Sr.No.

Particulars Details

1 Electrical load 100 HP2 Fresh Water Requirement 17 KL/day3 D. G. Set 500 KVA X 2 Nos.4 Cooling Tower 30 TR X 2 NOs

(one existing +one stand-by)

o Power: Required power would be taken from MGVCL

o Water: Water would be available from GIDC pipeline.

o Fuel : Wood for Thermic Fluid Heater

o Coal for Hot Water Generator

2.8 MANPOWER REQUIREMENTRequired specialized man power & talent would be recruited / hired

locally and supporting services would be made available from our

existing plant. Approximately 22 people will be employed.


161

CHAPTER 3

SITE ANALYSIS

3.1 CONNECTIVITY

District head quarter Anand is well connected by rail, road & air.

Road:

Linked to the National Highway Network through an extension of NH 8

from Anand NH-8, an offshoot of NH 8 connects Delhi, Ahmadabad to

Mumbai.

Rail

Western Railway line is 20 Km away from factory site to connect the

National Railway Network.

Air

Ahmedabad has a fully functional, long airstrip for servicing the needs of

private commercial jets which is proposed to be developed as an air cargo

hub.

Vadodara airport is 55 km from Sojitra GIDC.

3.2 EXISTING LAND USE PATTERN

Currently the land is occupied by GIDC and private owners. No agricultural

activities are done on this. The particular plot 37, 38 & 39 are under the

possession of the company.

3.3 TOPOGRAPHY

The area is flat in nature. It is a build up plot. The average elevation above

mean sea level is 55 m.


162

3.4 SOCIAL INFRASTRUCTURE AVAILABLE:Nearest town Sojitra is well-developed and the following infrastructure

facilities are available.

• Housing colonies

• Public School

• Healthcare Centre

• Children’s Park

• Community Centers

• Pharmacy

• Market

3.5 REHABILITATION & RESETTLEMENT PLANThe land is already in the possession of the project proponent. The NA

permission for the land is obtained by GIDC. Therefore, resettlement and

rehabilitation is not involved.

3.6 LAND USE BREAKUPThis plant will be located in Plot no-37, 38 & 39 having an area of 4098 sq.

m. The breakup of area into different uses is summarized in following table

S No Description of Area Area (Sq. m.)1 Storage of raw material 5002 Plant and machineries 10503 Storage of product 3004 Roads 905 Green belt 12006 Office Building 2007 Open Area 758

Total 4098


163

CHAPTER 4

PROPOSED ENVIRONMENTAL INFRASTRUCTURE

Company has already obtained consent to Operate for the existing unit formanufacturing of Pharmaceutical intermediates & Bulk drug intermediatesfrom Gujarat Pollution Control Board. The company will take into account allenvironmental aspects for expansion also so that no pollution hazard is evercreated in and around the plant. Every effort is being made to keep zero airpollution as well as water pollution. In addition to the above, care has beentaken to provide green belt around the plant.

4.1 MANAGEMENT OF DOMESTIC WASTE WATERThe domestic effluent (1.5 KLPD) shall be disposed through septic tank/

soak pit.

4.2 MANAGEMENT OF INDUSTRIAL WASTE WATERThe industrial effluent generated from various operations is treated in

Effluent treatment plant. The details of ETP are as follows:

ETP Process Description:


164

ETP units:

1. Collection tank (3 m X 3 m X 3 m)

2. Neutralization tank (3 m X 3 m X 3 m)

3. Filter press (24’×24’-24 plates)

4. Holding Tanks (3 m X 3 m X 3 m)

5. Activated Carbon Filter(Dia 1.5 feet and Height 5 Feet)

6. Final treated effluent tank (3 m X 3 m X 3 m)

Final treated effluent shall be partly reused In cooling makeup and

remaining shall utilized for gardening plantation within the premises of the

unit. Alternatively, industry has also got the membership of Sanand Eco

Projects Ltd for disposal of effluent in monsoon season.

4.3 AIR QUALITY MANAGEMENT:The only source of air pollution is Hot Water Generator and Thermic Fluid

Heater, which consumes Coal and hence can be treated as non-polluting.

Plant area has well ventilated, cross air flow and exhaust fans have been

provided for extra air flow.

4.4 SOLID & HAZARDOUS WASTE MANAGEMENTThe details of hazardous wastes generation from the proposed project & its

management & Handling are listed in the following tables. All the

requirements of hazardous waste rules shall be complied with.

Details of Hazardous Waste as per 2008 Rules

SRNo

Detail ofHazardous Waste

ExistingQuantity

Proposedtotal

quantitySCH-I Management of

Waste

1 ETP Waste 1.2MT/Year

2.4 MT/year 34.3 Collection, Storageand Disposal At TSDF

2 Used Spent Oil 0.36KL/Year

0.5 MT/Year

5.1

Collection, Storagereused for lubrication

of machineries inunit.

3DiscardedContainers/Barrels/Liners

10MT/Year

10 MT/Year

33.3

Collection, Storage,Decontamination,

disposal by reuse orreturned to supplier


165

For disposal of hazardous wastes, the industry has become member ofNandesari Enviro Control Ltd for common incineration and land fill site.

4.5 HAZARDOUS CHEMICALS DETAILS

The use and storage of hazardous chemicals is below the specified threshold

quantities. As per Schedule 3 under Rule 68-J of the Gujarat Factories Rules

1963 (2004) and hence the industry is classified as Non Major Accident

Hazard (NMAH) unit.

4.6 WASTE MINIMIZATION MEASURES Metering and control of quantities of active ingredients to minimize

waste.

Reuse of by-products from the process as raw materials or as raw

material substitutes in other processes.

Use of automated filling to minimize spillage.

Use of Close Feed system into batch reactors.

Venting equipment through vapor recovery system.

Use of high pressure hoses for equipment clearing to reduce

wastewater generation for reuse.


166

ANNEXURECC&A COPY


167


168


169


170


171

GIDC LETTER


172


173

SEPL CERTIFICATE


174

NECL CERTIFICATE (HAZARDOUS WASTE)


175

NECL CERTIFICATE (INCINIERATION)


176

PLANT LAYOUT

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