newreka igcw presentation

Your Answers To Green Chemistry Solutions

Newreka Green Synth Technologies Pvt. Ltd.,

Mumbai, (India)

Founders Team of Technocrats from IIT Bombay passionate about Nature

Foundation Principles of Green Chemistry, Green Engineering & Enviropreneurship

Knowledge Base & Over 40,000 experiments conducted by

Experience a dedicated team of 100 Chemists & Chemical Engineers.

Service Customized & Sustainable Solutions to

reduce & E-FACTOR* Recycle solution.

* E-FACTOR = kgs waste generated per kg product

About Newreka

All Unit Processes use H2O / Solvent as a Reaction Medium or Extraction Medium

Reduction, Condensation, Nitration, Diazotization, Hydrolysis, etc.

Use is spread across all Industrial Sectors Pharma, Dyes, Pigments, Specialty & Fine Chemicals, Agro, etc.

High Volume Products generate huge quantities of waste

like H-Acid, DASDA, Paracetamol, Phenylephrine, Pigment CPC, Violet23, Pendimethylene, etc.

Focus: Reducing E-FACTOR (Recycle of Aqueous & Solvent Effluent

Streams)

Solutions to conventional processes to make -

Your Streams Green

Your Solvent Green

Your Chemistry Green

Your Molecule Green

Newreka Solutions

“Prevent Waste: Design chemical syntheses to prevent waste, leaving no waste to treat or clean up”

1st Principle of Green Chemistry

Average Composition of Reaction Mass

Solvent & Water contribute more than 90% of the Reaction Mass

Source Data: ACS GCI Pharmaceutical Roundtable benchmarking exercise 2007

Average composition of Effluents will be similar.

Recycle of Water & Solvent can take care of 90% of problem.

A Journey through Case

Studies of

Neutral Mother Liquor

Recycle

Recycle Solution for Neutral Mother Liquor

Product: Pharma Intermediate (Anti-Aids Drug)Unit Process: ReductionConventional Technology: Catalytic Hydrogenation

A Case Study of…

Case Study – Neutral Mother Liquor

Conventional TechnologyUnit Process : Reduction

Case Study – Neutral Mother Liquor

Unit Process : Reduction Newreka Recycle Solution (NRS)TM

1. Water as “Reaction Medium”

2. Atm. Pr., Nominal pH & Temp

3. Neutral ML Recycled 25 times

4. 95% of Theoretical Yield

5. White to Off-White Amine

6. Freedom from Solvents

7. Energy efficient

8. Safe Raw Materials, No Acids or Alkali

Case Study – Neutral Mother Liquor

1. Solvent as “Reaction Medium”

2. High Pressure

3. Effluent containing Organics

both Solvents & Amine

4. 85% of Theoretical Yield

5. Brown Colored Amine

6. 2 Solvents used

7. Energy Intensive process

8. Hazardous Raw Materials like

Raney Ni & Hydrogen Gas

A Comparison of Conventional Technology & NRS

Impact:

Green Chemistry based Solutions impacted:-

1. Economics2. Environment3. Safety

This solution has saved our customer, Rs.60 lacs

(i.e. USD 150,000) per year.

Safer Process & Enhanced Quality were Bonuses.

Case Study – Neutral Mother Liquor

Product: Pharma Intermediate

(Analgesic & Antipyretic Drug)

Unit Process: Reduction of P-Nitrophenol

to

P-Aminophenol

Recycle Solution for Neutral Mother Liquor

Case Study – Neutral Mother Liquor

Unit Process for PAP Conventional Technology

Case Study-Neutral mother liquor recycle

Unit Process for PAP Newreka Recycle Solution (NRS)TM

STAGE : P-AMINOPHENOL

STATISTICS : P-AMINOPHENOLSr. No. No. of experiment Quantity

* Number of experiments performed 1520

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Melting

range oCDry

product gm

Purity %

Fresh Off White Crystalline Single spot of product 184 42 99.55

R1 Off White Crystalline Single spot of product 184 43.4 99.65

R2 Off White Crystalline Single spot of product 184 44.8 99.70

R3 Off White Crystalline Single spot of product 184 46.9 99.72

R4 Off White Crystalline Single spot of product 184 47.6 99.75

R5 Off White Crystalline Single spot of product 184 49 99.75

A Comparison of Conventional Technology & NRS

1. Solvent as “Reaction Medium”

2. Effluent containing Organics

both Solvents & Amine

3. 85% of Theoretical Yield

4. Brown Colored Amine

5. 2 Solvents used

6. Energy Intensive process

1.Water as “Reaction Medium”

2. Neutral ML Recycled 25 times

3. 95% of Theoretical Yield

4. White to Off-White Amine

5. Freedom from Solvents

6. Energy efficient process.

5-Nitro salicylic acid

To

5-Amino salicylic acid

(Make your chemistry Green)

Case Study

Unit Process of 5-ASA Conventional Reduction Technology(CRT)

5 ASA PFD

• Acidic Mother Liquor recycle around

100 times with R-Cat treatment.

• Increase in yield due to recycle.

• No Purification requires.

• Crude product is of 99% purity.

Benefits by Newreka process

STATISTICS:REDUCTION

Sr. No. No. of experiment Quantity * Number of experiments performed 131

Product characterization in recycle experiments (5-nitro Salicylic Acid)

Recycle No Color Appearance TLC/GC/HPLC Melting range 0C

Dry product

gm

Purity %

Fresh Off white powder Single spot of product 266-270 71 99+

R1 Off white powder Single spot of product 266-270 67.5 99+

R2 Off white powder Single spot of product 266-270 71.2 99+

R3 Off white powder Single spot of product 266-270 70 99+

R4 Off white powder Single spot of product 266-270 70.2 99+

R5 Off white powder Single spot of product 266-270 87 99+

Ortho-Nitrophenol

To

Ortho-Aminophenol

(make your chemistry green)

Case Study – Neutral Mother Liquor

Unit Process for OAP Conventional Technology

Case Study-Neutral mother liquor recycle

Unit Process for OAP Newreka Recycle Solution (NRS)TM

STAGE : O-AMINOPHENOL

Benefits by Newreka process

• 100% Neutral mother liquor recycle.

• 3-5% increase in yield.

• 5-10% reduction in production cost.

• Zero effluent generation .

STATISTICS : O-AMINOPHENOLSr. No. No. of experiment Quantity

* Number of experiments performed 1150

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Melting

range oCDry

product gm

Purity %

Fresh Off White Crystalline Single spot of product 179 28 99.50

R1 Off White Crystalline Single spot of product 179 30.8 99.60

R2 Off White Crystalline Single spot of product 179 33.6 99.62

R3 Off White Crystalline Single spot of product 179 35 99.65

R4 Off White Crystalline Single spot of product 179 36.4 99.70

R5 Off White Crystalline Single spot of product 179 42 99.75

A Comparison of Conventional Technology & NRS

1. Solvent as “Reaction Medium”

2. Effluent containing Organics

both Solvents & Amine

3. 85% of Theoretical Yield

4. Brown Colored Amine

5. Two Solvents used

6. Energy Intensive process

1.Water as “Reaction Medium”

2. Neutral ML Recycled 25 times

3. 95% of Theoretical Yield

4. White to Off-White Amine

5. Freedom from Solvents

6. Energy efficient process.

A Comparison of Conventional Technology & NRS

Meta Nitro Acetophenone

To

Meta Amino Acetophenone

(make your synthesis green)

Case Study – Neutral Mother Liquor

Unit Process for MAA Conventional Technology

CASE STUDY OF NEUTRAL MOTHER LIQUOR RECYCLE

• Acidic Mother Liquor recycle around 100

times without any treatment.

• Increase in yield up to theoretical due to

recycle.

• Safe Process as compare to

conventional.

Benefits by Newreka process

STATISTICS:MAASr. No. No. of experiment Quantity

* Number of experiments performed 325

Product characterization in recycle experiments ( MAA)Recycle No Color Appearance TLC/GC/HPLC Melting

range0CDry product

gmPurity %

Fresh Yellow Powder Single spot of product 92-96 24.5 99.20

R1 Yellow Powder Single spot of product 92-96 34.0 99.72

R2 yellow Powder Single spot of product 92-96 35.2 99.62

R3 yellow Powder Single spot of product 92-96 35.3 99.72

R4 yellow Powder Single spot of product 92-96 36.3 99.84

R5 yellow Powder Single spot of product 92-96 40. 0 99.52

N-ethyl 3- Nitro carbazole

To

N-ethyl 3- Amino carbazole

(Neutral ML Recycle)

Case Study

Unit Process of REDUCTION Conventional Reduction Technology(CRT)

PDILIT PFD NRTCASE STUDY OF NEUTRAL

MOTHER LIQUOR RECYCLE

STAGE:REDUCTION

• Water Layer recycle in highly multiphase reaction.

• 4-5% increase in yield as compare to conventional

process.

• Easy handling.

Benefits by Newreka process

1.Recycle of Water Layer

2. No formic acid used.

3. 95% of Theoretical Yield

4. Filtration Time Low

5. Energy efficient

1. High Liquid Effluent.

2. Formic Acid used.

3. 90% of Theoretical Yield

4. Filtration Time High

5. Energy Intensive process

A Comparison of Conventional Technology & NRT

A Comparison of Conventional Technology & NRS

STATISTICS:REDUCTIONSr. No. No. of experiment Quantity -

* Number of experiments performed 1203

Product characterization in recycle experiments (N-ethyl 3-nitro carbazole)

Recycle No Color Appearance Filtration Time Amine content in ODCB Layer

Batch size 55gm

Fresh Dark brown Liquid 6 min 34.01 gm

R1 Dark brown Liquid 8 min 35.78 gm

R2 Dark brown Liquid 4 min 36.68 gm

R3 Dark brown Liquid 6 min 37.65 gm

R4 Dark brown Liquid 5 min 35.49 gm

R5 Dark brown Liquid 4 min 37.69 gm

Para Chloro Nitro Benzene

To

Para Chloro Aniline

(Neutral ML Recycle)

Case Study

Unit Process of PCA Conventional Reduction Technology(CRT)

CASE STUDY OF NEUTRAL MOTHER LIQUOR AND SOLVENT

RECYCLE

• Water Layer recycle in highly multiphase reaction.

• Increase in yield as solvent and water layer being

recycled.

• Isolation of product is easier as compare to Conventional

Process.

• High yield as compare to conventional.

• Almost theoretical yield is achieved as compared to

theoretical.

Benefits by Newreka process

STATISTICS:REDUCTIONSr. No. No. of experiment Quantity

* Number of experiments performed 202

Product characterization in recycle experiments ( Para Chloro Aniline)

Recycle No Color Appearance TLC/GC/HPLC Filtration Time

Amine content

Fresh Greenish Liquid Single spot of product 10 min 50.81 gm

R1 Greenish Liquid Single spot of product 12 min 69.58 gm

R2 Greenish Liquid Single spot of produce 22 min 66.05 gm

R3 Greenish Liquid Single spot of product 10 min 89.17 gm

R4 Greenish Liquid Single spot of product 10 min 50 .48 gm

R5 Greenish liquid Single spot of product 10 min 79.79gm

Newreka Recycle Solution For

Sulphonic Series Compounds

(Acidic ML Recycle)

Newreka Recycle Solution For

3,5-DNBA To 3,5-DABA(Acidic ML Recycle)

Unit Process for 3,5-DNBA Reduction Conventional Technology

Case Study – Acidic Mother Liquor

ISOLATOR

R NO2

Water

CIP

FILTERATION

REDUCTIONEXTRACTION

Water

Neutral isolation mass

55% Yield Iron Oxide Spent

Case Study-Acidic mother liquor recycle

Unit Process for 3,5-DNBA Reduction Newreka Recycle Solution (NRS)TM

ISOLATOR

NEWREKA REDUCTION CATALYST (NRC)

CATALYST (NGC)NEWREKA GREEN

REDUCTION

SPENT NRC

CENTRIFUGE GREEN AMINE

Mother LiquorStorage

1000lit and 1,00,000lit

FILTER

65%yield

STAGE: 3,5-DNBA Reduction

• Increase in yield 10% as compare to conventional process.

• Profitability in quality like off-white color.

• Reduces production cost.

• Water is conserved by recycling of ML.

• Mild or neutral pH condition(6 TO 7).

• Effluent down by Minimum 50%(Air +Water +Solid).

• Energy down by minimum 25%(Fuel + power).

Benefits by Newreka process

STATISTICS :3,5-DNBA ReductionSr. No. No. of experiment Quantity

* Number of experiments performed 200

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Dry

product gm

Purity %

Fresh Off white Powder Single spot of product 45.5 98.50

R1 Off white Powder Single spot of product 71 98.34

R2 Off white Powder Single spot of product 59 97.28

R3 Off white Powder Single spot of product 75 98.19

R4 Off white Powder Single spot of product 71.5 98.04

R5 Off white Powder Single spot of product 70 96.97

1.Recycle of ”Reaction Medium” 40times

2.65% of Theoretical Yield.

3.Effluent down by minimum 50%.

4.Mild or neutral pH condition

(6 To 7).

5. Energy efficient

1. Highly Acidic Liquid Effluent

2.55% of Theoretical Yield

3.There is no solution of effluent

A Comparison of Conventional Technology & NRS for 3,5-DNBA to 3,5-DABA

Energy Intensive process

4.Highly acidic solution(4pH)

5.

A Comparison of Conventional Technology & NRS

Newreka recycle solution for

4,4-Di Nitro Stilbene-2,2-di sulphonic acid (DNSDA)

To

4,4-Di amino stilbene-2,2-di sulphonic acid (DASDA)

(Acidic ML Recycle)

Unit Process for Reduction Conventional Technology for DASDA

Case Study – Acidic Mother Liquor

ISOLATOR

Water

CIP

FILTERATION

REDUCTIONEXTRACTION

Water

Neutral isolaton mass

78% Yield Spent

DNSDA

Case Study-Acidic mother liquor recycle

Unit Process for Reduction for DASDA Newreka Recycle Solution (NRS)TM

ISOLATOR

NEWREKA REDUCTION CATALYST (NRC)

CATALYST (NGC)NEWREKA GREEN

REDUCTION

SPENT NRC

CENTRIFUGE GREEN AMINE

Mother LiquorStorage

1000lit and 1,00,000lit

FILTER

80%yield

Comparison of E-factor in Reduction for DASDA

• Increase in yield as compare to conventional

process.

• Better economic process.

• Zero discharge process.

• Effluent load reduced by 50%.

• Energy efficiency improved by 25% (Fuel + power).

Benefits by Newreka process in DASDA

STATISTICS :Reduction in DASDASr. No. No. of experiment Quantity

* Number of experiments performed 200

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Dry product gm Purity %

Fresh Lemon yellow Powder Single spot of product 33 96.45

R1 Lemon yellow Powder Single spot of product 33 95.27

R2 Lemon yellow Powder Single spot of product 34 94.89

R3 Lemon yellow Powder Single spot of product 36 96.02

R4 Lemon yellow Powder Single spot of product 36 95.74

R5 Lemon yellow Powder Single spot of product 37 95.85

1. Recycle of ”Reaction Medium”

25times.

2. 80% of Theoretical Yield.

3. Effluent down by minimum

50%.

4. Energy efficient.

1. Highly Acidic Liquid Effluent.

2. 78% of Theoretical Yield.

3. There is no solution of

effluent.

4. Energy intensive process.

A Comparison of Conventional Technology & NRS for DASDA productionA Comparison of Conventional Technology & NRS

Newreka recycle solution for

4-Nitro Di-phenylene amine-2-Sulphonic acid

To

4,4-Di amino Di phenylene-2-Sulphonic acid (FC Acid)

(Acidic ML Recycle)

Unit Process for Reduction Conventional Technology for FC Acid

Case Study – Acidic Mother Liquor

ISOLATOR

NADPSA

Water

CIP

FILTERATION

REDUCTIONEXTRACTION

Water

Neutral isolaton mass

Spent Iron OxideProduct yield 84%

Case Study-Acidic mother liquor recycle

Unit Process for Reduction in FC Acid Newreka Recycle Solution (NRS)TM

ISOLATOR

NEWREKA REDUCTION CATALYST (NRC)

CATALYST (NGC)NEWREKA GREEN

REDUCTION

SPENT NRC

CENTRIFUGE GREEN AMINE

Mother LiquorStorage

1000lit and 1,00,000lit

FILTER

Yield 88%

E-Factor of Reduction process in FC Acid

Benefits by Newreka process in FC Acid

• Increase in yield by 4% as compare to conventional

process.

• Better economic process.

• Zero discharge process.

• Energy efficiency improved by 50%(Fuel +Power).

• Effluent load reduced by 50%(Air + Water + Solid).

STATISTICS In FC AcidSr. No. No. of experiment Quantity

* Number of experiments performed 200

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Dry product gm Purity %

Fresh violet Amorphous Single spot of product 40 94.4

R1 violet Amorphous Single spot of product 41 93.4

R2 violet Amorphous Single spot of product 41 92.5

R3 violet Amorphous Single spot of product 47 93.6

R4 violet Amorphous Single spot of product 37 93.0

R5 violet Amorphous Single spot of product 44.5 92.0

1. Recycle of ”Reaction Medium”10 times

2. 88% of Theoretical Yield

3.Consistent 94% purity in all batches.

4.Effluent load reduced by 50%.

5.Mild pH condition(6.0 to 6.5)

6.Energy efficient

1. Highly Acidic Liquid Effluent

2. 84% Theoretical Yield

3. 94% purity only in fresh batch.

4. There is no solution for effluent.

5. Highly alkaline solution.

6.Energy Intensive process

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

Newreka recycle solution for

Meta- phenylene Di-Nitro 4-sulphonic Acid

To

Meta phenylene Di- Amine 4-sulphonic Acid(MPDSA)

(Acidic ML Recycle)

Unit Process for Reduction Conventional Technology for MPDSA

Case Study – Acidic Mother Liquor

ISOLATOR

Water

CIP

FILTERATION

REDUCTIONEXTRACTION

Water

Neutral isolaton mass

Product yield of 60%

Acidic effluent

Spent

MPDNSA

Case Study-Acidic mother liquor recycle

Unit Process for Reduction Newreka Recycle Solution (NRS)TM

ISOLATOR

NEWREKA REDUCTION CATALYST

CATALYST NEWREKA GREEN

REDUCTION

SPENT NRC

CENTRIFUGE GREEN AMINE

Mother LiquorStorage

1000lit and 1,00,000lit

FILTER

Yield 65%

MPDNSA

Comparison of E-Factor in MPDSA

STATISTICS : In MPDSA process

Sr. No. No. of experiment Quantity * Number of experiments performed 300

Product characterization in recycle experiments

Recycle No Color Appearance TLC/GC/HPLC Dry product gm

Purity %

Fresh Off white Semi crystal Single spot of product 25 99.45

R1 Off white Semi crystal Single spot of product 28 99.27

R2 Off white Semi crystal Single spot of product 30 99.39

R3 Off white Semi crystal Single spot of product 30 99.16

R4 Off white Semi crystal Single spot of product 30 99.34

R5 Off white Semi crystal Single spot of product 32 99.52

1. Recycle of ”Reaction Medium” 25times.

2. 65% of Theoretical Yield.

3. Off white Colored Product.

4. Energy efficient & safe process.

1. Highly Acidic Liquid Effluent.

2. 60% of Theoretical Yield.

3. Grey Colored Product.

4. Energy Intensive & hazardous process.

A Comparison of Conventional Technology & NRS for Reduction process of MPDSA

A Comparison of Conventional Technology & NRS

DIAZOTIZATION:

Meta aminoacetophenone

To

Meta hydroxyacetophenone

(make your synthesis green)

Case Study – Acidic Mother Liquor

Unit Process : Diazotization Conventional Technology

Unit Process : Diazotization Newreka Recycle Solution (NRS)TM

Case Study-Acidic mother liquor recycle

STAGE:DIAZOTIZATION

STATISTICS : DIAZOTIZATION

Sr. No. No. of experiment Quantity * Number of experiments performed 283

Product characterization in recycle experiments

Recycle No Color Appearance TLC/GC/HPLC Melting range oC

Dry produc

t gm

Purity %

Fresh Off White Amorphous Single spot of product 95 70 99.50

R1 Off White Amorphous Single spot of product 95 72 99.60

R2 Off White Amorphous Single spot of product 95 75 99.59

R3 Off White Amorphous Single spot of product 95 80 99.60

R4 Off White Amorphous Single spot of product 95 83 99.65

R5 Off White Amorphous Single spot of product 95 85 99.68

1. Recycle of ”Reaction Medium” 75 times.

2. 95% of Theoretical Yield.

3. Yellow Colored Product.

4. Green solvent as Extraction Medium.

5. Energy efficient.

1. Highly Acidic Liquid Effluent.

2. 70% of Theoretical Yield.

3. Brown Colored Product.

4. Class 1 Solvent as Extraction Medium.

5. Energy Intensive process.

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

Newreka recycle solution for

PNCB To Na-PHENOLATE

(Alkaline ML Recycle)

Unit Process for PNP Conventional Technology

Case Study – Alkaline Mother Liquor

Case Study-Alkaline mother liquor recycle

Unit Process for PNP Newreka Recycle Solution (NRS)TM

STATISTICS OF Na-PHENOLATESr. No. No. of experiment Quantity

* Number of experiments performed 136

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Dry product gm

Fresh Yellow Powder Single spot of product 94

R1 Yellow Powder Single spot of product 95.6

R2 Yellow Powder Single spot of product 96

R3 Yellow Powder Single spot of product 95.2

R4 Yellow Powder Single spot of product 96.3

R5 Yellow Powder Single spot of product 96.8

STAGE for PNP

1. Recycle of ”Reaction Medium” 15 times.

2. 25% Savings in Sodium Hydroxide.

3. 99% of Theoretical Yield.

5. Yellow Colored Product.

6. Energy efficient since effluent treatment not

needed.

Benefits of NRS for Alkaline ML Recycle

Newreka recycle solution for

Na-PHENEOLATE To PNP(Acidic ML Recycle)

Unit Process for PNP Conventional Technology

Case Study – Acidic Mother Liquor

Case Study-Acidic mother liquor recycle

Unit Process for PNP Newreka Recycle Solution (NRS)TM

STATISTICS OF PNPSr. No. No. of experiment Quantity

* Number of experiments performed 136

Product characterization in recycle experimentsRecycle No Color Appearanc

eTLC/GC/HPLC Melting

range oCDry

product gm

Purity %

Fresh Yellow Crystalline Single spot of product 112-114 142 99.04

R1 Yellow Crystalline Single spot of product 112-114 146 99.18

R2 Yellow Crystalline Single spot of product 112-114 140 98.94

R3 Yellow Crystalline Single spot of product 112-114 144 99.36

R4 Yellow Crystalline Single spot of product 112-114 142 99.27

R5 Yellow Crystalline Single spot of product 112-114 146 99.09

STAGE for PNP

1. Recycle of ”Reaction Medium” 15 times

2. 30% Savings in Sulphuric Acid

3. Saleable Na2SO4 by product

4. 95% of Theoretical Yield

5. Yellow Colored Product

6. Useful acidic reaction medium

1. Highly Acidic Liquid

Effluent

2. Low yield of product

3. Solid waste mixture of (Na2SO4 + NaCl)

4. 90% of Theoretical Yield

5. Brown Colored Product

6. Waste disposal needed

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

Case Studies of

Green Nitration Technology

(Salicylic acid to 5-Nitro salicylic acid)

Unit Process for Nitration Conventional Technology for Salicylic acid

Case Study – Nitration

ISOLATOR

FILTERATION

NITRATION

ICE

Acidic effluentsolution

Reaction mass

Gl. Acetic Acid

Salicylic acid

5-Nitro Salicylic acid

Nitrating Mixture

ISOLATOR

FILTERATION

NITRATION

Recycle Acidic ML

Reaction mass

HNO3

Salicylic acid

5-Nitro Salicylic acid

Case Study-Acidic mother liquor recycle

Unit Process : Nitration Newreka Recycle Solution (NRS)TM

Acidic ML

STAGE:NITRATION – SALICYLIC ACID

STATISTICS:NITRATIONSr. No. Particulars No. of experiments performed

* Number of experiments performed 288

Product characterization in recycle experiments (salicylic acid)Recycle No Color Appearance Melting range0C Dry product gm

Fresh Yellowish white Amorphous 180 – 190 53

R1 Yellowish white Amorphous 185 – 192 54.7

R5 Yellowish white Amorphous 180 – 192 50

R10 Yellowish white Amorphous 180 – 190 53.2

R15 Yellowish white Amorphous 185 – 190 52.8

R20 Yellowish White Amorphous 180- 192 54

R25 Yellowish white Amorphous 190 – 195 54

R30 Yellowish white Amorphous 190 – 200 54

R35 Yellowish white Amorphous 195- 205 52.7

R40 Yellowish white Amorphous 185 -190 53.2

R45 Yellowish white Amorphous 185 – 190 53.7

R50 Yellowish white Amorphous 185 -190 52.3

• Recycle of acidic mother liquor.

• Savings in consumption of Nitric acid.

• No use Sulphuric acid in nitration.

• Consistent quality up to 50th recycle.

• Consistent yield.

Benefits by Newreka process

Case Studies of

Green Nitration of

Acetophenone (Make Your synthesis Green)

Unit Process for Acetophenone Conventional Technology

Case Study – Nitration

ISOLATOR

Mix acid

FILTERATION

NITRATION

ICE

acidicsolution

Reaction mass

98%H2SO4

Acetophenone

71% YIELD

WATER

Case Study-Nitration of Acetophenone

Unit Process for Acetophenone Newreka Nitration Solution

ISOLATORNITRATION

GREEN NITRO

Yield 82%

98%H2SO4 Mixed acid

Acetophenone

FILTERATION

Ice

STAGE: Acetophenone Nitration

STATISTICS: NITRATIONSr. No. No. of experiment Quantity

* Number of experiments performed 300

Product characterization in recycle experimentsRecycle

NoColor Appearance TLC/GC/HPLC Dry

product gmM.P 0C

Fresh cream Amorphous powder Single spot of product 28.8 76

Fresh cream Amorphous powder Single spot of product 28.2 77

Fresh cream Amorphous powder Single spot of product 27.5 78

Fresh cream Amorphous powder Single spot of product 28.9 79

Fresh cream Amorphous powder Single spot of product 27.9 77

Fresh cream Amorphous powder Single spot of product 28 78

1. Overall addition or maintain time is 12 hrs.

2. 82% of Theoretical Yield

3. 25% Savings in Sulfuric Acid

4. Energy efficient & safe process.

5.Minimise effluent (25%)

6.25% more batch size capacity in same reactor

1. Overall addition or maintain

Time is 15 to 16hrs.

2. 71% of Theoretical Yield

3. Sulfuric Acid – 1.5Times

4. Energy Intensive process

5. No effluent minimize

6. No more capacity of batch size.

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

Case Study of

Green Nitration of Benzoic

Acid (Make Your Chemistry Green)

Unit Process for MNBA Conventional Technology

Case Study – Nitration

ISOLATOR

FILTERATION

NITRATION

acidicsolution

Reaction mass

Benzoic acid

98% HNO3

90% YIELD

COOL WATER98% H2SO4

Case Study-Nitration

Unit Process for MNBN Newreka Nitration Solution

ISOLATORNITRATION

GREEN NITRO

Yield 95%

98%H2SO4Benzoic acid98% HNO3

FILTERATION

Cool water

STAGE: Meta nitro benzoic acid

STATISTICS: Meta nitro benzoic acid

Sr. No. No. of experiment Quantity

* Number of experiments performed 100

Product characterization in recycle experimentsRecycle No Color Appearance TLC/GC/HPLC Dry

product gm

M.P0C

Fresh OFF WHITE Crystalline powder

Single spot of product 120 142

Fresh OFF WHITE Crystalline powder Single spot of product 118.5 139

Fresh OFF WHITE Crystalline powder Single spot of product 124 140

Fresh OFF WHITE Crystalline powder Single spot of product 115 141

Fresh OFF WHITE Crystalline powder Single spot of product 120 141

Fresh OFF WHITE Crystalline powder Single spot of product 119 139

1. Overall addition or maintain time is 8.5 hrs.

2. 92% of Theoretical Yield

3. 25% Savings in Sulfuric Acid

4. Energy efficient

5.Minimise effluent (25%)

6.25% more batch size capacity in same reactor

1. Overall addition or maintain Time is 12 to 14hrs.

2. 90% of Theoretical Yield

3. Sulfuric Acid – 1.5 Times

4. Energy Intensive process

5. No effluent minimize

6. No more capacity of batch size.

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

A Case study

Of

Green Intermediate Synthesis

For Anti-AIDS Drug

Make Your Molecule Green

Unit Process for Diazotization Conventional Technology

Case Study – Acidic Mother Liquor

Unit Process : Diazotization Newreka Recycle Solution (NRS)TM

Case Study-Acidic mother liquor recycle

Unit Process : Nitration Conventional Technology

Case Study – Neutral Mother Liquor

Case Study-Neutral mother liquor recycle

Unit Process : Nitration Newreka Recycle Solution (NRS)TM

Unit Process for Chlorination Conventional Technology

Case Study – Acidic Mother Liquor

Case Study-Acidic mother liquor recycle

Unit Process for Chlorination Newreka Recycle Solution (NRS)TM

Case Study – Neutral Mother Liquor

Conventional TechnologyUnit Process : Reduction

Case Study – Neutral Mother Liquor

Unit Process : Reduction Newreka Recycle Solution (NRS)TM

Stage IIIChlorination

Stage IVReduction

Stage VStage IINitration

Stage IDiazo. & Hydrolysis

Stage VI

Stage IINitration

Stage IIIChlorination

Stage IVReduction

Stage IDiazo &Hydrolysis

Stage VIStage V

Case Study: Reducing E-Factor & Improving Yield

DRUG : Anti – Retroviral Drug CUSTOMER : A fast growing Indian Pharma Company

CONVENTIONAL SYNTHETIC CHEMISTRY PROCESS

E-Factor 32 38 28 4

Effluent 1920 TPA 2280 TPA 1680 TPA 240 TPA (for 60TPA plant)

GREEN CHEMISTRY SOLUTION BY NEWREKA

E-Factor 6 6 1 4Effluent 360 TPA 360 TPA 60 TPA 240 TPA

Case Study: Reducing E-Factor & Improving Yield

Benefits by Newreka process

STAGE 1: DIAZOTIZATION

• Red solvent replaced by green solvent. • Technology set in recycle loop.

• 100% effluent is recycle with 95% yield.

STAGE 2: NITRATION

• Red solvent replace by green solvent.

• Yield increased by 15%.

Benefits by Newreka process

STAGE 3: CHLORINATION

• Increase in yield by 15% as compare to

conventional process.

• 80% of Solvent recovery & recycle.

• Reduces production cost.

• Replaces class 1 solvent with green solvent.

Benefits by Newreka process

STAGE 4: REDUCTION

• 2 Red solvent replace by water as reaction media.

• Yield increased by 25%.

• High pressure reaction replace with atm. Pressure process.

• Energy efficient process.

• Safe raw material.

1. Recycle of ”Reaction Medium” infinite times

2. 95% of Theoretical Yield

3. Ecofriendly solvent as Extraction Medium 4. Energy efficient

1. Acidic Liquid Effluent

2. 85% of Theoretical Yield

3. Harmful Solvent asExtraction Medium

4. Energy Intensive process

A Comparison of Conventional Technology & NRS

A Comparison of Conventional Technology & NRS

A Case study

Of

Green Intermediate Synthesis

For Decongestant Drug

Make Your Molecule Green

Unit Process for Acetophenone Conventional Technology

Case Study – Nitration

ISOLATOR

Mix acid

FILTERATION

NITRATION

ICE

acidicsolution

Reaction mass

98%H2SO4

Acetophenone

71% YIELD

WATER

Case Study-Nitration of Acetophenone

Unit Process for Acetophenone Newreka Nitration Solution

ISOLATORNITRATION

GREEN NITRO

Yield 82%

98%H2SO4 Mixed acid

Acetophenone

FILTERATION

Ice

Case Study – Neutral Mother Liquor

Unit Process for MAA Conventional Technology

CASE STUDY OF NEUTRAL MOTHER LIQUOR RECYCLE

Case Study – Acidic Mother Liquor

Unit Process : Diazotization Conventional Technology

Unit Process : Diazotization Newreka Recycle Solution (NRS)TM

Case Study-Acidic mother liquor recycle

Stage IIIDiazotization

Stage IIReduction

Stage INitration

Stage IIReduction

Stage IIIDiazotization

Stage INitration

Case Study: Reducing E-Factor & Improving Yield

DRUG : Decongestant Drug CUSTOMER : A fast growing Indian Pharma Company

CONVENTIONAL SYNTHETIC CHEMISTRY PROCESS

GREEN CHEMISTRY SOLUTION BY NEWREKA

Newreka Recycle Solution For

PARATOLUDINE

Unit Process for Paratolidine Conventional Technology

Case Study – Catalytic Hydrogenation

Case Study : Green Reduction

Unit Process for Paratoludine Newreka Recycle Solution (NRS)TM

Isomer Free

• Matrix Laboratories Ltd. Hyderabad.

• Rakshit Drugs Pvt.Ltd Hyderabad.

• Jupiter Bioscience Ltd. Hyderabad.

• Smilax Laboratories Ltd. Hyderabad.

• Pidilite Industries Ltd, Vapi.

• Medilux Laboratories Ltd. M.P.

• Aptuit Laurus Pvt. Ltd. Hyderabad.

• Metrochem API Pvt. Ltd. Hyderabad.

• Phanicare Pharmaceuticals Pvt. Ltd. Hyderabad.

• SMS Pharma Pvt Ltd, Hyderabad.

Customers of Newreka

• Vapi - belt of dyes.

• Solapur - to Hyderabad belt of pharmaceuticals.

• Mumbai – All India locate.

• Pune – New proposed R & D hub for

Pharmaceuticals.

Infrastructure of Newreka

Strength of Team Newreka

The Deserved Reward by GCNC-2008

Thank You

&

Wish all of You a

“Greener Future”from

Team Newreka