Catalytic hydrogenation of o-nitroanisole in a microreactor:: Reactor performance and kinetic studies

Hydrogenation of o-nitroanisole to o-anisidine was conducted in a packed-bed microreactor as a model hydrogenation reaction of importance to the pharmaceutical and fine chemicals industries with the aim of investigating the reactor performance and kinetics of the reaction. The effects of different processing conditions viz. hydrogen pressure, o-nitroanisole concentration, temperature, and residence time on the conversion of o-nitroanisole, space-time yield (STY), and selectivity of o-anisidine were studied using 2% Pd/zeolite catalyst. The kinetic study was undertaken in a differential reactor mode keeping the conversion of o-nitroanisole at less than 10%. During the kinetic study, it was observed that the intermediate 2-methoxynitrosobenzene was present in the reactor at low catalyst loading and low conversions because of short residence time in the reactor. Therefore, for the kinetics study, the overall reaction was treated as comprising two separate reactions: first the reduction of o-nitroanisole to 2-methoxynitrosobenzene and then, the reduction of 2-methoxynitrosobenzene to o-anisidine. Internal and external mass and heat transfer limitations in the microreactor were examined. Different rate laws using different mechanisms from the literature were considered to fit the experimental data. Two rate equations for the two consecutive reactions assuming Langmuir-Hinshelwood mechanism provided the best fit to the experimental data. These two rate equations predicted the experimental rates within 10% error. Experiments were also carried out in an integral reactor, and the reactor performance data were found to be in agreement with the predictions of the theoretical models. (c) 2007 Elsevier Ltd. All rights reserved.