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Utilization of Stop-flow Micro-tubing Reactors for the Development of Organic Transformations
Published on: January 4, 2018
Reaction screening using a microreactor
Olivier Naef1, Mathieu Roch, Thierry Chappuis
1Ecole d'ingénieurs et d'architectes de Fribourg, Boulevard de Pérolles 80, CP 32, CH-1705 Fribourg. olivier.naef@hefr.ch
Chimia
|January 29, 2011
Summary
This study optimized an esterification reaction using a microreactor and online infrared spectroscopy. Despite formic acid decomposition catalyzed by the reactor material, the system achieved successful optimization.
Area of Science:
- Chemical Engineering
- Analytical Chemistry
- Process Chemistry
Background:
- Microreactors offer advantages for chemical synthesis and process optimization.
- Online analytical techniques are crucial for real-time monitoring and control of reactions.
- Esterification reactions are fundamental in organic synthesis and industrial applications.
Purpose of the Study:
- To investigate the use of a microreactor coupled with infrared spectroscopy for online reaction screening.
- To optimize an esterification reaction in continuous flow using this setup.
- To evaluate the performance and limitations of the system, particularly concerning reactor material interactions.
Main Methods:
- Utilized a microreactor system for continuous flow chemical synthesis.
- Integrated online infrared (IR) spectroscopy for real-time reaction monitoring.
- Screened and optimized an esterification reaction under various conditions.
- Investigated the influence of the stainless-steel 316Ti microreactor material on reaction pathways.
Main Results:
- Successfully optimized an esterification reaction in continuous mode using the microreactor setup.
- Observed catalytic decomposition of formic acid due to the stainless-steel 316Ti material.
- Demonstrated that optimization is achievable despite the occurrence of side reactions.
- Validated the utility of online IR spectroscopy for monitoring complex reaction mixtures.
Conclusions:
- Microreactor technology combined with online IR spectroscopy is a viable tool for reaction screening and optimization.
- The choice of microreactor material is critical and can influence reaction outcomes, even leading to unexpected catalysis.
- Despite material-induced decomposition, effective process optimization can still be achieved by understanding and managing the reaction system.

