Catalysis-in-a-Box: A Micro-flow Catalytic Reactor Integrated within a Gas Chromatograph for Automated Kinetic Measurements

The design and implementation of an autonomous micro-flow-reactor condensing conventional laboratory-scale analogues within a single gas chromatograph (GC) is reported, enabling the control of relevant parameters including reactor temperature and reactant partial pressures directly from the GC. Inquiries into the hydrodynamic behavior, temperature control, and heat/mass transfer were sought to evaluate the efficacy of the micro-flow-reactor for kinetic measurements. A combination of four Brønsted acid catalyzed probe reactions, namely the dehydration of ethanol, 2-propanol, 1-butanol, and the dehydra-decyclization of 2-methyltetrahydrofuran on a solid acid HZSM-5 (Si/Al 140), were carried out in the temperature range 403-543 K for the measurement of apparent reaction kinetics. Product selectivities, proton-normalized reaction rates, and apparent activation barriers were found to be in agreement with measurements performed in conventional packed bed flow reactors. The developed micro-flow-reactor is therefore intended to be used for kinetic investigations in vapor-phase catalytic chemistries, with the key benefits including automation and limited experimental equipment instrumentation.