PowerPoint Presentation 2013/gr… · Title: PowerPoint Presentation Author: Savita Kirpalani...

Green Engineering using

Commercial “Flow Reaction” &

Process Intensification Platforms

Vijay KirpalaniCEO

Pi – Process IntensificationMumbai

08-12-2013 Copyright Pi-Process Intensification Experts LLP 1

Twelve Principles of Green Chemistry

• 1. Prevent waste rather than treat/clean it up later• 2. Invoke atom economy• 3. Design safer chemicals• 4. Use & generate less toxic substances• 5. Massively reduce quantities of solvents used• 6. Design syntheses for energy efficiency• 7. Renewable feedstock for large scale processes• 8. Minimize steps in synthesis• 9. Use of highly-selective catalytic reagents• 10. Design materials that innocuously degrade• 11. Real-time monitoring for pollution prevention• 12. Minimise potential for accidents

P.T. Anastas and J.C. Warner, Green Chemistry: Theory and Practice, Oxford University Press: New York, 1998, p.30

8 out of 12 can be achieved through intensification of processes & flow chemistry.


Process Intensification


Process Intensification

Reactions

Flow Chemistry

Other Platforms

Unit Operations

Extraction

Distillation

Crystallization

Filtration

Drying

Air Pollution Control - Absorption

Effluent Treatment – Cavitation Reactors

Pi Benefits


FLOW ChemistryAn established technique for performing reactions under conditions where :

Mixing

Temperature

Pressure and

Reaction Time

are precisely controlled and safely done.

Variables : ● stoichiometry, ● concentration, ● residence-time,

● temperature and ● pressure are easily adjusted and reactions optimized quickly.

Scale-up : nearly linear and usually done by numbering-up


FLOW Reactors

Fast Track to Optimized Processes

Though the use of Continuous processes is widespread for chemical product, the development of processes for Fine chemicals & APIs has historically been restricted to the centuries-old technique of iterative-batch-reactions.

The increasing pressure to quickly discover & deliver compounds using scalable processes has compelled the synthetic chemists to harness Flow Chemistry techniques.

Commercial FLOW REACTORS are now an easily available & common enabling technology for performing synthesis in the laboratory & plant scale.

Cost benefits (↓size / ↑safety / ↑ energy efficiency / ↑ yield / ↑ purity) of flow reactors are so compelling, that the cost of the reactor is of subordinate interest.


FLOW ReactorsTECHNOLOGY

Selection of apt reactor technology platform is most important for better cost benefit realization :-a) HEAT Transfer Area cost for Heat Transfer limited processb) Reactor Volume cost for Mass Transfer & slow kinetically limited process

Key types :

Micro-reactors / Microchannel reactors Falling-film micro-reactors Tubular flow reactors Spinning Tube-in-Tube reactors Spinning Disk reactors Spinning Disk FUMI reactors Oscillatory Tube/Baffled flow reactors Microwave assisted flow reactors Sonication-assisted flow reactors Multi-cell flow reactors Aspirator flow reactors


History of Chemical Manufacture


Nothing has changed in nearly 500 years

Steven Ley, et al

Industry Appeal

Higher reaction control translates into :

● ability to safely handle :hazardous reactions / reagents / unstable-intermediates andhighly exothermic reactions

● consistent good quality & high yields / selectivity

Scalability with FLOW Reactors :

Numbering-up -- Running multiple reactors in parallel is advantageous there is no theoretical limit to the number of reactors that can be used physical conditions are identical whether using 10 or 10,000 reactors

Modular, plug-&-play, quick-fit / release designs


Scalable Development Platforms

A few of the “scalable” Flow Chemistry platforms

available to synthesis development chemists today


A) Versatile : Limitation : high solid slurries

“R-series”“E-series”

for suspensions



A) Versatile : Limitation : high solid slurries (cont’d)

“Flow-Syn” “Asia” series




Advanced

Flow

Reactors

Labtrix




MMRS from



B) Versatile : Can handle solids in a slurry !

“ACR” -

Coflore

COBROscillatory

Baffled Reactor

30% to 50% solids in slurry !



C) Reaction specific :

“H-Cube” for

Hydrogenation

“O-Cube” for

Ozonolysis

Industrial Scale FLOW Reactors


Ehrfeld

Lonza Flow Plate Micro Reactor from



KiloFlow & PlantriX

KiloFlow & Plantrix (SiC) from



Advanced Flow Reactors Alfa Laval ART® Plate Reactor

http://www.alfalaval.com/



Coflore “ATR” : Dynamic Agitated Tubular Reactor



Spinning Tube-in-Tube Hydrodynamic CAVITATION Reactor

Kreido Hydrodynamics



FUMI Spin Disk Spinning Disk Reactor

SpinPro-300

Volume : 300 ml

Output : 10 T / day +



Oscillatory Tube Reactor Oscillatory Baffled Reactor

http://www.google.co.in/imgres?sa=X&biw=1366&bih=637&tbm=isch&tbnid=OUQTpNrjX4CugM:&imgrefurl=http://www.ceb.cam.ac.uk/pages/ofm-process-intensification.html&docid=io7a7cQV__FqhM&imgurl=http://www.ceb.cam.ac.uk/data/images/groups/polymer/OFM/piofr_cut_away.jpg&w=450&h=338&ei=VXejUvnxF8WOrQe1zoGIBQ&zoom=1&ved=1t:3588,r:28,s:0,i:171&iact=rc&page=2&tbnh=191&tbnw=224&start=13&ndsp=21&tx=100&ty=83



Continuous Flow Microwave-assisted Reactors

CaMWave™

Industrial ApplicationsReactions


GRIGNARD Reactions

uses ChemtriX PLANTRIX Micro Reactors

made of EKasic® (SiC) in a pharma API

production plant

Grignard Reactions

Industrial ApplicationsReactions

Hydroformylation - Evonik exampleEvonik’s container for hydroformylation at the backbone facility of the INVITE GmbH at Leverkusen, Germany


jetloop reactor withintegrated membrane

separation

The hydroformylation process in a jetloop with an integrated membrane separation was successfully demonstrated at the INVITE facility in Leverkusen from February to March 2013.

Hydroformylation - Evonik example (cont’d)

Benefits reduced investment costs through standardized & easily

scalable reactor equipment,

reduced operating costs due to maximized space-time, yield & integrated heat management,

high selectivities due to low heat gradients & ideal mixing

improved catalyst lifespan due to separation under process

conditions.


Halogen /Lithium Exchange


1.75 T / month on a 2.5” Ø Disk // 7T / month on a 5” Ø Disk

Halogen /Lithium Exchange


1.23 T / month on a 2.5” Ø Disk // 5 T / month on a 5” Ø Disk

• Highly Exothermic– Batch synthesis delayed 2 months for

DSC information

• Batch scaleup problematic– Yield not reproducible– Increased formation of by-product led to

formation of a gum which was difficult to purify

– Batch synthesis required significantly more time than expected

STRONG EXOTHERM onset

at 130 ºC (1373 J/g)

Nitration Example (Novartis)

http://dx.doi.org/10.1021/op200055r

Unit-Ops -- Extraction


SpinPro SDE-300

Volume : 300 ml

Throughput : 10,000 L / day

+

Unit-Ops -- Distillation


Reactor

SplitterExtractive

Distillaton

Solvent

Recovery

Methanol

Recovery

Extractor

Azeo

Column

Decanter

Flash

Column

Color

Column

Flash

Column

Water

Water

Heavies

Methyl

Acetate

Water

Catalyst

Methanol

Acetic Acid

Reactor

Column

Impurity

Removal

Columns

Water

Heavies

Acetic Acid

Methanol

Sulfuric

Acid

Methyl

Acetate

Reactive Distillation

Eastman Chemicals

Unit-Ops -- Intensified Distillation


HiGee Distillation

30 mt column replaced by a 1.5 mt column for MeOH Distn.

Unit-Ops -- Crystallization


Oscillatory Tube Crystallizer

Unit-Ops -- Filtration


Modular Spin Disk Filter –Dynamic Membrane

Unit-Ops -- Absorption


Pulsed-Jet Dynamic Waveform Absorber

Major Route Design Factors and Their Interactions


Quality

Safety

Cost

Durability / Robustness

Environmental Impact

Synthesis Process

T.Y.Zhang, Cem.Rev., 2006, 106, 2583.

QUESTIONS


?

WISH YOU A

GREENER TOMORROW

THANK YOU


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