View
3.094
Download
2
Tags:
Embed Size (px)
Citation preview
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