The emergence of a viral pandemic has motivated the transition away from traditional, labor-intensive materials testing techniques to new automated approaches without compromising on data quality and at costs viable for academic laboratories. Reported here is the design and implementation of an autonomous micro-flow reactor for catalyst evaluation condensing conventional laboratory-scale analogues within a single gas chromatograph (GC), 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. As a catalyst material screening example, 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 in agreement with measurements performed on conventional packed bed flow reactors. Furthermore, the developed micro-flow reactor was demonstrated to be about ten-fold cheaper to fabricate than commercial automated laboratory-scale reactor setups and is intended to be used for kinetic investigations in vapor-phase catalytic chemistries, with the key benefits including automation, low cost, and limited experimental equipment instrumentation.
Contains the raw files for experimental data collected on the reported micro-flow reactor along with .json files used for heat/mass transfer calculations on GradientCheck. Additionally, all editable .pptx files of final Schemes and Figures are included.
Sponsorship: The Catalysis Center for Energy Innovation