Rapid Determination of Reaction Kinetics with an Automated Microfluidic System

Kinetic information is used to determine the optimal reaction conditions, to successfully scale up a reaction from the laboratory to the pilot plant, and to improve process control. Obtaining accurate kinetics using conventional benchtop equipment and techniques, however, requires numerous experiments and can be complicated by sluggish mixing and heat-transfer rates. To improve the speed and efficiency in gathering reaction kinetics, we present an automated, silicon microreactor system that uses a sequential experimentation framework driven by model-based optimization feedback for online reaction rate parameter determination. The method, based on Information Theory and Bayesian Statistics, first selects the appropriate global reaction rate expression. After determining the correct rate law, a D-optimal strategy precisely estimates the pre-exponential and activation energy of the rate constant. The approaches are validated experimentally with a model system, the Diels-Alder reaction of isoprene and maleic anhydride in DMF. The benefits of quicldy obtaining this information with an automated microreactor system are further demonstrated by successfully scaling the Diels-Alder reaction by a factor of 500 from a microreactor to a Corning flow reactor.