1. Micro-Reactor developments
Céline GUERMEUR
Corning SAS
CPAC SATELLITE WORKSHOPS 2007
Micro-reactors and Micro-Analytical – March 19-21, 2007

2. Focus: The reactor and its integration into the production system
C=O R R’
Chemistry
System engineering
Mass and
heat transfer
Reactor engineering

3. Micro reactor for Industrial Production Throughput in metric tons per year per reactor
Targeted product Metric tons/Year per reactor
Flow rate (Kg/hour)
Reactants concentration (wt%) 1 2 3 5 10 12 4 8 20 17 30 7 25 50 21 42 70 6 29 58
100 83
Assumptions
Conversion %
Selectivity 95

4. Reactor engineering process
Reaction network and feed distribution
Thermodynamic & Kinetics
Feed boundaries
Design and sizing
Material selection
Reactor fundamentals
Detailed reactor engineering
Chemistry
know-how
Basic reactor engineering
REACTOR
PRODUCT SYNTHESIS UNIT
CUSTOMER NEEDS
Translation into a mass and heat transfer problem
Let’s go together through an example

5. Detailed reactor engineering Basic reactor engineering
Reactor fundamentals
Detailed reactor engineering
Chemistry
know-how
Basic reactor engineering
Customer needs
Safe and smooth production of 40 kg / week / reactor
Raw material cost > 500 €/kg
More than 95% conversion
Impurities below 2%

6. The chemistry know-how
A + B  C
C + D  E
E + H20  Product + H2
Exothermic
Highly reactive intermediate
No major side products
Exothermic
Maximum temperature 10°C
Safety limit : 50 L batch vessel
Excess of C = Selectivity issue
Exothermic
Hydrogen release

7. Product synthesis unit
Basic reactor engineering
Product synthesis unit
Internal volume < 0.1 Liter
No loading / unloading
Internal volume : 200 Liters
5 loading / unloading A B
PRODUCT
SYNTHESIS
UNIT C D

8. Basic reactor engineering
Basic engineering
Step 1 :
Mixing and heat exchange integrated
Single injection
Step 2 :
No excess of C
Step 3:

9. Data needed: Mass and heat balance
Detailed reactor engineering
19 ml/min
17 g/min
0.5 20°C
Feed 1
20°C
15 W
released
0°C
150 W
released
0°C
480 W
released
Feed 2
29 ml/min
26 g/min
0.5
Feed 3
65 ml/min
58 g/min
0.7
Feed 4
43 ml/min
39 g/min
1.6 0°C

10. Detailed reactor engineering
Hydrodynamic
Detailed reactor engineering

11. Detailed reactor engineering Basic reactor engineering
Reactor fundamentals
Detailed reactor engineering
Chemistry
know-how
Basic reactor engineering
Throughput: 40 kg/week
99 % conversion
Impurities < 1%
Pressure: Up to 18 bars
Temperature : -50°C to 40°C
Internal volume : 70 ml

12. MASS TRANSFER: SINGLE AND MULTI-INJECTION HEAT TRANSFER

13. Single-injection reactor
Reactor fundamentals A
FEED PRE-HEAT/COOL
FEED PRE-HEAT/COOL
REACT B
HE IN
HE OUT
PRODUCT

14. Multi-injection reactor
Reactor fundamentals A
FEED PRE-HEAT/COOL
SPLIT
FEED PRE-HEAT/COOL
REACT B
HE IN
HE OUT
PRODUCT
Acknowledgement:
Michael T. Klein, Dean School of Engineering
Rutgers, The State University of New Jersey

15. Multi-injection: Better temperature management along the flow path
Heat removal
Single -injection
Multi -injection
Heat generation

16. Single and multi-injection
Reactor fundamentals
Examples
B = 1/3
B = 1/3
B = 1/3
B = 1
A = 1
A = 1
A/B = 1
A/B = 1
A/B = 3
A/B = 2
A/B = 1
In both cases, the molar ratio target is reached

17. Pressure drop management and fluid split within the micro-structures
Reactor fundamentals
Multi-injection: Only two pumps are required A B
Pressure drop management and fluid split within the micro-structures
Product

18. Mass and heat transfer are combined
Reactor fundamentals
Mass and heat transfer are combined
Heat transfer
Mass transfer
Heat transfer

19. Optimum heat exchange Reaction circuit: Toluene
Reactor fundamentals
Optimum heat exchange
Reaction circuit: Toluene
Heat exchange circuit: Water
600 W/m2.K

20. Heat exchange performance
Reactor fundamentals
Corning glass micro-reactor
Example of metal mixer
(Internal testing)
Reaction circuit: Toluene – Same flow rate
Heat exchange fluid: Water
Heat exchange: Integrated
Heat exchange: Agitated bath
600 W/m2.K
60 W/m2.K

21. Multi-phase mass transfer
Feeds
Mixing test
Results
Hydrodynamic visualization L
Villermaux method
Villermaux & all, AIChE Symp. Ser. 88 (1991) 6, 286.
Mixing quality > 90% for flow rates > 1.8 L/h
L/L
Polystyrene precipitation
Chem. Eng. Technol. 2005, 28,
Proc. of the 10th APCChE Congress, 2004, 4B-02
nm particle size
L/G
Measure of slug size
Pressure drop in monolith reactors, P. Woehl, R.L. Cerro, Catalysis Today 69 (2001)
Flow patterns in liquid slugs during bubble-train flow inside capillaries, Chem Eng Sci 52 (1997) mm
Hydrodynamic regime adapted to needs

22. Module approach enable bridging
Specific reaction(s)
Synthesis unit kg-lab testing
Dedicated production
Multipurpose production
Standard modules
Test applicability on reaction portfolio

23. Nitration

24. Organometalic reaction

25. Example of Multipurpose production
CAMPAIGN 1
PRODUCTION 1
CAMPAIGN 2

26. Generate value in production, increase safety and product quality using micro-reactors
Courtesy of Lonza