The cycloaddition reaction between isoamylene and α-methylstyrene yields indane compounds 1,1,2,3,3,-pentamethylindane and 3-ethyl-1,1,3-trimethylindane, which are intermediate cyclic products used in the synthesis of musk fragrances. This exothermic reaction is usually carried out industrially in large semibatch reactors. The microreactor, with enhanced heat and mass transfer characteristics, was used for the reaction with aqueous sulfuric acid as catalyst. The dependence of reactant conversion, product yield, and average reaction rates on catalyst concentration, temperature, velocity, residence time, and the molar ratio of the reactants in the feed was investigated. A similar study was also performed in the semibatch reactor to compare its performance with that of the microreactor. Higher product yields were obtained in the microreactor, and the average reaction rates in the microreactor were 3 orders of magnitude greater than those obtained in the semibatch reactor.
Catalytic hydrogenation of nitro aromatics is an important class of reactions in the pharmaceutical and fine chemical industries. These reactions are extremely fast and highly exothermic in nature; hence, mass and heat transfer limitations play an important role when these reactions are conducted in conventional batch reactors. The use of a micro-channel reactor for such reactions provides improved mass transfer rates which may ensure that the reaction operates close to intrinsic kinetics. In the present study, the hydrogenation of a model aromatic nitro ketone was conducted in a packed-bed microreactor. The effects of different processing conditions were studied using 5%Pd/Alumina catalyst, viz.: hydrogen pressure, substrate concentration, temperature, and residence time on the conversion of substrate, Space Time Yield (STY), and selectivity of product. Internal and external mass and heat transfer limitations in the microreactor were examined. The kinetic study was undertaken in a differential reactor mode, keeping the conversion of the reactant at less than 10%. The overall reaction was treated as comprising two separate reactions: first, the reduction of the nitro compound to hydroxylamine and then, the reduction of the hydroxylamine to amine. Two rate equations for the two consecutive reactions assuming the Langmuir-Hinshelwood mechanism provided the best fit to the experimental data. These two rate equations predicted the experimental rates satisfactorily and the differences were 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.
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