RAPID ONLINE MONITORING OF A HETEROGENEOUS CATALYST BY A PULSED REACTOR COUPLED TO GC-MS

A rapid screening system for heterogeneous catalyst discovery has been developed by coupling an in-house designed and fabricated high temperature vapor phase pulse reactor on-line to a GC-MS. The incorporation of gas chromatography for separation of the products with the mass spectrometry system allowed simultaneous identification and determination of reaction products and substrate conversion. This system was employed to study the vapor phase catalytic hydride transfer reduction (CHTR) of nitrobenzene with methanol as hydrogen donor on an MgO catalyst as a model reaction. Structural information of all the by-products that were formed was useful to understand the reaction mechanism. The products obtained with the new screening technique were in good agreement with conventional bench scale experiments. The rapid online screening provided an efficient methodology for optimization of reaction conditions such as catalyst loading, reaction temperature, and mole ratios. Response Surface Methodology (RSM) was used to optimize the conversion of reactants and selectivity of products.