How to Implement a MicroReactor in a Large Scale Production

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How to Implement a Micro-Reactor in a Large Scale
Production

• Vorbach, M.1)
• Bohn, L.2) Kotthaus, M.1) Kraut, M.2)
  Pöchlauer, P.1) Wenka, A. 2) and Schubert, K.2)
• DSM Fine Chemicals Austria 1)
• Forschungszentrum Karlsruhe, Institute for Micro
  Process Engineering (IMVT) 2)

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OVERVIEW

• Introduction of DSM and IMVT
• Goals
• Lab-scale
• Production-scale
• Results and outlook
• Summary

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DSM
Ownership public shareholders 100
Head office Heerlen, The Netherlands
Employees worldwide 21.820
Turnover 8.195 Billion EUR
Operating Profit 808 Mln. EUR
Net profit 527 Mln. EUR
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DSM Fine Chemicals Austria Facts Figures (2005)
Turnover 213,8 Mln. EUR
Export quota 79
Employees 921 439 Workers
438 Employees 44 Apprentices
Production sites / - Pilot plantplants
- Multi Purpose plant -
Mono plant -
Multi Product plant - High Shelf
Storage Facility - Modern RD Center
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DSM over a century of successful transformations
Evolution
Technological competences
1902
1930
1970
1950
1990
2000
Mechanical engineering
Chemical engineering
Polymer technology
Material science
Fine chemicals
Biotechnology
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Forschungszentrum Karlsruhe (FZK)

• 22 Institutes
• Ca. 3800 employees, of these ca. 1400 Scientists
• working in
• 5 research areas comprising 11 Programs
• Cooperation FZK-DSM is covered by
• research area key technologies
• Program Nano-Mikro

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Institute for Micro Process Engineering
Institute for Micro Process Engineering (IMVT)

• Micro process engineering skills
• Micromachining
• Fabrication
• CFD-Simulation
• Characterization
• Application

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We all know that...

• Microreactors provide strictly controlled
  reaction conditions for reactions that
• are very fast
• are exothermic
• use hazardous materials.
• In order to get sizeable amounts of product, we
  do not scale up but number up the machinery.
  

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Goal synthesis of organic intermediate
Chemical issues very fast reaction backmixing
reduces yield forms by-products (presently
35)
Safety issues highly exothermic toxic raw
material and by-product concentrated sulfuric
acid
Fluid mechanics issues large difference in
viscosity quick increase in viscosity
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Experience what did we do?
We used a micro reactor costum designed by IMVT
to develop a scalable lab synthesis of our
product.
IMVT designed a production scale reactor based on
the DSM lab data
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Laboratory Module

• total throughput 1 kg/h
• pressure resistance 20 bar
• max. temperature 180 C
• mixer exchangeable
• (taylor-made for each
• application)
• Prior to production start-up
• shift-workers operated
• the device continuously
• for 48 hours

Laboratory Module with exchangeable mixer
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Design of the MR lab-installation
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MR lab-installation Figures

• Throughput approx. 1 kg/h
• Pressure drop 4 bar
• Allows strict temperature control
• Residence time several seconds
• Yield increased gt 10

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Production Reactor Design Development
Scaling up a microreactor

• Keep the geometrie of the micro structure, but
  add channels up to the required throughput.
• Find a good solution for the flow distribution
  in order to keep local flow patterns equal
  throughout the device.

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Production Reactor Design Development
Adaption
Diffusion bonding
Certification by TÜV
Assembly
Structured foils
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In DSM plant for comparison
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The production reactor (1)
as part of the installation
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The production reactor (2)

• Througput gt1 ton/h reaction mixture
• Modular concept
• Pressure drop Reaction side lt 3 bar
• Water side lt 1 bar
• Volume reaction side 3 liters
• Residence time same as lab
• Cooling capacity several 100 kW
• driving ?T very few degrees

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Results of production

• Produktion reactor was operated during several
  months on commercial scale
• Same improvement of chemical yield as in lab
  saving raw materials and waste costs

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Key success factors of implementation (1)
As a first step of implementation, the
micro-reactor did not replace an existing
installation, but was added to increase
selectivity. ? The change to the production
plant was minimally invasive.
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Key success factors of implementation (2)
The transition from fed batch to continuous
operation was simplified by using the initial
reaction vessel as buffer tank. ? The operation
of the micro reactor was, within limits,
decoupled from the work-up.
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Key success factors of implementation (3)
Soft facts Allow your production manager and
production staff to learn and develop trust in
micro-reaction technology!
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minimally invasive plant reconfiguration
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Key success factors of implementation (4)
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Pinning down further applications
Look for fed batch applications in the
plant (reaction mass is circulated through a
heat exchanger and reagent is added to the loop
at a rate to keep the temperature below
xxC) Look for time consuming operations or
reactions (reagents are mixed at 40-50C and
after 2 hours the mixture is gradually heated to
90C and kept there for 2 more hours to complete
the conversion)
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Summary and Outlook

• Successful application of micro reaction
  technology in production of organic intermediate
• Production reactor delivers equal performance
  as lab reactor
• Better and cheaper product
• OUTLOOK
• Modification of work-up process
• Extension of micro reaction technology to
  other applications

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Acknowledements

• We gratefully appreciate the contribution of
• Österreichische Forschungsförderungsgesellschaft
  (FFG)
• Prof. R. Marr, TU Graz
• Thank you for your attention!