Microreactors as a Pilot and Production Scale Tool for Chemical Processes Dirk Kirschneck

1. Microreactors as a Pilot and Production Scale Tool for Chemical Processes Dirk Kirschneck

2. Content • Introduction and Driving Forces • Plant Concepts • Project Examplesa) Exothermic Reactionb) Precipitationc) Character Pharma Projectsd) Liquid-Liquid Fine Chemicals • Summary • Investment and Payback • Summary

3. Aim of Microinnova Intensify Chemical Processes and Separation Processes by microstructured Devices

4. Present Situation in Fine Chemicals Market • High Pressure on Costs especially of operation due to competitors from the far east (Change Pressure) Chemical Development • Automated Batch Parameter Optimisation & DOE Scale up and Technology Transfer • Chemistry is fitted into existing batch vessel • Equipm. & Labour intense due to Parameter testing • Time Intense due to Scale-up problems Production and Economics • high Operating Costs due to Change over/Cleanding • large and inefficient Vessels with low utilisation

5. Future Strategies (not exclusive) • Investment in Asia • Massive Reduction of Labour Costs high Automation Level of Plants • Switch from Batch to Conti • Focus on Development a) High Speed Developmentb) High Performance Products (e.g. funct. material…) • Process Intensifaction (Performance, Stability…)

6. Factor Target Impact on Process Intensification Yield Energy 0-40%  5-15%  Profit Switch to Contin. Product. Labor-C. Invest.-C. 10-20%  5-15%  Profit Shorten Time-to-Market Developm. Time Blocking Competitors 10-30%  Novel Products Market Position Longterm Growth Increase Expected Benefits from MicroChemTec

7. Development Aim: Process Quality Process Improvement comes from • Process Possibities • Process Understanding • Process Control Goals: a) Increase in Space-Time-Yield b) Process Economy (e.g. using recycles) Fit the Production Unit to the Chemical Process and not Fit the Chemical Process to the Production Unit

8. Business fields Process Development Engineering & Plants Devices (Distributor)

9. Process development

10. Microinnova Plant Technology

11. Plant Automation

12. Small Scale Production

13. Small scale production • up to 100 kg/h • fits in fume-cupboard • completely automated • production flexibility

14. Project: Particle Precipitation • batch precipitation process • insufficient particel size distribution • additional process step  safety problems • aim: reduction particle size (factor 10) cutting out process step safety improvement

15. Change on production scale precipitation milling final powder safetyofthemillingstepiscritical principleriskofpowderexplosions accident in thehistory 10 times smaller particles

16. Particle formation • nucleation • growth of the particle growth nucleation micromixer case a) Throughput: Lab 20 kg/h (now) Production4000 kg/h (planed) case b)

17. Project: Exothermal Reaction Exothermal Reaction 200 KJ/mol (300°C uncooled) Aim: Safety Improvement Process Steps: 2 Steps to slow speed down Planned Capacity: 500 kg/h

18. Exothermic Reactions • Good Mixinig => Sudden Heat Release • Heat Exchanger usually after the Mixer • Heat Peak Throughput dependent Heat Exchanger Compartment Heat Release HE1 HE2 HE3 Point of Mixing Residence Time

19. Saftey and Production • No adiabatic Temperature rising by high Surface-to-Volume Ratio • Toxic reaction steps can be sealed • Radicals of burning or explosion can be captured by walls • Inherent save devices are under development

20. Character of pharmaceutical synthesis multi step synthesis of relatively small amounts  expensive substances especially in the last steps  yield has got a big impact on costs

21. investment costs pharma plant measurement & automation storage separation microreactor stirred tank reactor energy supply no big impact on investment costs < 5 %

22. Structure of process costs >90% chemical costs

23. Yield improvement assumption  10 % yield improvement plant pay back micro-plant  < 2 years

24. Pharma summary • no difference in investment • >90% chemical costs • production flexibility • higher safety • yield improvement gives a fast return on investment

25. Fine Chemicals Example L/L • 2-step batch reaction • educt A: volatile and toxic • cooled - heated • 10m3 vessel  1600kg/h A + B  C + B  D exothermal endothermal

26. Aims • higher throughput addition to capacity – 2x • implement microreactor for 1st step • energy savings no cooling faster reaction

27. Implementation

28. Realization • reactor design/installation • StarLam3000 / IMM • <3 bar – old pumps used • good product in the first run

29. First test run

30. Benefits • investment costs new batch reactor (10x more) • double capacity • energy savings no cooling for 1st step less energy for heating the 2nd step

31. Conclusions • microinnova focuses on process development and engineering • micro plants are an efficient development tool • pilot and production scale projects have big saving potential • microreactors are flexible and safe production method

32. Dr. Dirk Kirschneck Microinnova Engineering GmbH dirk.kirschneck@microinnova.com www.microinnova.com