Investigation of multiphase hydrogenation in a catalyst-trap microreactor

Background: Multiphase hydrogenation plays a critical role in the pharmaceutical industry. A significant portion of the reaction steps in a typical fine chemical synthesis are catalytic hydrogenations, generally limited by resistances to mass and heat transport. To this end, the small-scale and large surface-to-volume ratios of microreactor technology would greatly benefit chemical processing in the pharmaceutical and other industries. A silicon microreactor has been developed to investigate mass transfer in a catalytic hydrogenation reaction. The reactor design is such that solid catalyst is suspended in the reaction channel by an arrangement of catalyst traps. The design supports the use of commercial catalyst and allows control of pressure drop across the bed by engineering the packing density. Results: This paper discusses the design and operation of the reactor in the context of the liquid-phase hydrogenation of o-nitroanisole to o-anisidine. A two-phase 'flow map' is generated across a range of conditions depicting three flow regimes, termed gas-dominated, liquid-dominated, and transitional, all with distinctly different mass transfer behavior. Conversion is measured across the flow map and then reconciled against the mass transfer characteristics of the prevailing flow regime. The highest conversion is achieved in the transitional flow regime, where competition between phases induces the most favorable gas-liquid mass transfer. Conclusion: The results are used to associate a mass transfer coefficient with each flow regime to quantify differences in performance. This reactor architecture may be useful for catalyst evaluation through rapid screening, or in large numbers as an alternative to macro-scale production reactors.