Green Engineering using Commercial Flow Reaction & Process Intensification Platforms. Vijay Kirpalani. CEO Pi Process Intensification Mumbai

Transcription

1 Green Engineering using Commercial Flow Reaction & Process Intensification Platforms Vijay Kirpalani CEO Pi Process Intensification Mumbai Copyright Pi-Process Intensification Experts LLP 1

2 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 Copyright Pi-Process Intensification Experts LLP 2

3 Process Intensification Reactions Flow Chemistry Other Platforms Process Intensification Extraction Distillation Crystallization Unit Operations Filtration Drying Air Pollution Control - Absorption Effluent Treatment Cavitation Reactors Copyright Pi-Process Intensification Experts LLP 3

4 Copyright Pi-Process Intensification Experts LLP 4

5 Pi Benefits Copyright Pi-Process Intensification Experts LLP 5

6 FLOW Chemistry An 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 Copyright Pi-Process Intensification Experts LLP 6

7 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 Copyright Pi-Process Intensification Experts LLP 7

8 FLOW Reactors TECHNOLOGY Selection of apt reactor technology platform is most important for better cost benefit realization :- a) HEAT Transfer Area cost for Heat Transfer limited process b) 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 Copyright Pi-Process Intensification Experts LLP 8

9 History of Chemical Manufacture Nothing has changed in nearly 500 years Steven Ley, et al Copyright Pi-Process Intensification Experts LLP 9

10 Industry Appeal Higher reaction control translates into : ability to safely handle : hazardous reactions / reagents / unstable-intermediates and highly 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 Copyright Pi-Process Intensification Experts LLP 10

11 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 Copyright Pi-Process Intensification Experts LLP 11

12 Scalable Development Platforms A) Versatile : Limitation : high solid slurries (cont d) Flow-Syn Asia series Copyright Pi-Process Intensification Experts LLP 12

13 Scalable Development Platforms A) Versatile : Limitation : high solid slurries (cont d) Advanced Flow Reactors Labtrix Copyright Pi-Process Intensification Experts LLP 13

14 Scalable Development Platforms A) Versatile : Limitation : high solid slurries (cont d) MMRS from Copyright Pi-Process Intensification Experts LLP 14

15 Scalable Development Platforms B) Versatile : Can handle solids in a slurry! 30% to 50% solids in slurry! ACR - Coflore COBR Oscillatory Baffled Reactor Copyright Pi-Process Intensification Experts LLP 15

16 Scalable Development Platforms C) Reaction specific : H-Cube for Hydrogenation O-Cube for Ozonolysis Copyright Pi-Process Intensification Experts LLP 16

17 Industrial Scale FLOW Reactors Ehrfeld Lonza Flow Plate Micro Reactor from Copyright Pi-Process Intensification Experts LLP 17

18 Industrial Scale FLOW Reactors KiloFlow & PlantriX KiloFlow & Plantrix (SiC) from Copyright Pi-Process Intensification Experts LLP 18

19 Industrial Scale FLOW Reactors Advanced Flow Reactors Alfa Laval ART Plate Reactor Copyright Pi-Process Intensification Experts LLP 19

20 Industrial Scale FLOW Reactors Coflore ATR : Dynamic Agitated Tubular Reactor Copyright Pi-Process Intensification Experts LLP 20

21 Industrial Scale FLOW Reactors Spinning Tube-in-Tube Hydrodynamic CAVITATION Reactor Kreido Hydrodynamics Copyright Pi-Process Intensification Experts LLP 21

22 Industrial Scale FLOW Reactors FUMI Spin Disk Spinning Disk Reactor SpinPro-300 Volume : 300 ml Output : 10 T / day Copyright Pi-Process Intensification Experts LLP 22

23 Industrial Scale FLOW Reactors Oscillatory Tube Reactor Oscillatory Baffled Reactor Copyright Pi-Process Intensification Experts LLP 23

24 Industrial Scale FLOW Reactors Continuous Flow Microwave-assisted Reactors CaMWave Copyright Pi-Process Intensification Experts LLP 24

25 Industrial Applications Reactions GRIGNARD Reactions uses ChemtriX PLANTRIX Micro Reactors made of EKasic (SiC) in a pharma API production plant Grignard Reactions Copyright Pi-Process Intensification Experts LLP 25

26 Industrial Applications Reactions Hydroformylation - Evonik example Evonik s container for hydroformylation at the backbone facility of the INVITE GmbH at Leverkusen, Germany jetloop reactor with integrated 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 Copyright Pi-Process Intensification Experts LLP 26

27 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 Copyright Pi-Process Intensification Experts LLP 27

28 Halogen /Lithium Exchange 1.75 T / month on a 2.5 Ø Disk // 7T / month on a 5 Ø Disk Copyright Pi-Process Intensification Experts LLP 28

29 Halogen /Lithium Exchange 1.23 T / month on a 2.5 Ø Disk // 5 T / month on a 5 Ø Disk Copyright Pi-Process Intensification Experts LLP 29

30 Nitration Example (Novartis) 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)

31 Unit-Ops -- Extraction SpinPro SDE Volume : 300 ml Throughput : 10,000 L / day Copyright Pi-Process Intensification Experts LLP 31

32 Unit-Ops -- Distillation Acetic Acid Methanol Catalyst Reactive Distillation Methyl Acetate Methyl Acetate Reactor Solvent Recovery Methanol Recovery Acetic Acid Splitter Extractive Distillaton Water Sulfuric Acid Methanol Extractor Azeo Column Decanter Flash Column Color Column Reactor Column Impurity Removal Columns Heavies Heavies Water Flash Column Eastman Chemicals Water Water Copyright Pi-Process Intensification Experts LLP 32

33 Unit-Ops -- Intensified Distillation 30 mt column replaced by a 1.5 mt column for MeOH Distn. HiGee Distillation Copyright Pi-Process Intensification Experts LLP 33

34 Unit-Ops -- Crystallization Oscillatory Tube Crystallizer Copyright Pi-Process Intensification Experts LLP 34

35 Unit-Ops -- Filtration Modular Spin Disk Filter Dynamic Membrane Copyright Pi-Process Intensification Experts LLP 35

36 Unit-Ops -- Absorption Pulsed-Jet Dynamic Waveform Absorber Copyright Pi-Process Intensification Experts LLP 36

37 Major Route Design Factors and Their Interactions Safety Quality Durability / Robustness Synthesis Process Cost Environmental Impact T.Y.Zhang, Cem.Rev., 2006, 106, Copyright Pi-Process Intensification Experts LLP 37

38 QUESTIONS? Copyright Pi-Process Intensification Experts LLP 38

39 WISH YOU A GREENER TOMORROW THANK YOU Copyright Pi-Process Intensification Experts LLP 39