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A high-pressure trickle-bed reactor was used to achieue high productivity and selectivity for the manufacture of a key herbicide intermediate (α-aminomethyl-2-furanmethanol) (amino alcohol, AA) from α-nitromethyl-2-furanmethanol (nitro alcohol, NA). Raney Nickel catalysts of varying activity were prescreened for suitability in tricklebed operation. The effect of operating parameters such as reactant feed concentration, liquid mass uelocity, and temperature on the yield of amino alcohol (A) for RNi-a are discussed. The superiority of trickle-bed reactors ouer others such as semibatch and batch sluny systems is demonstrated. The AA yield increases with decrease in feed reactant concentration and liquid mass velocity, as well as with lowering of the operat ing temperature. A maximum product yield of 90.1% was obtained at 8.3 wt. % feed concentration of nitroalcohol (NA), while at the highest feed concentration of 40 wt. % NA, the maximum product yield was 58%. The volumetric productivity of AA was significantly higher at higher reactant feed concentrations, even though the yield was lower under these conditions. The operating temperature was also an important parameter, with a lower temperature being preferable for trickle-bed experiments. Bed dilution with inert fines improued catalyst utilization and increased the AA yield and productivity in the laboratory-scale trickle-bed reactor.

Conventional strategies for discrimination of intrinsic and apparent kinetics from crushed- and whole-catalyst-pellet experimental data, respectively, do not yield satisfactory results for the reaction network in the manufacture of (α-aminomethyl-2-furanmethanol) (aminoalcohol) from αnitromethyl-2-furanmethanol (nitroalcohol). Laboratory trickle-bed reactor tests in the range of concentration and product yield of commercial interest are utilized to yield a reasonable set of kinetic parameters, which are otherwise unobtainable. This is accomplished by proposing a reaction network, a plausible mechanism, and optimizing the kinetic parameters based on the reactor-model-generated peformance data to fit experimental output concentrations of all species for the entire set of experiments. A complex reaction network for the key reactions in the system is developed based on the reaction scheme in Part I. Fitting of trickle-bed reactor data to this model is attempted to yield an insight into the actual kinetics. The results show promise of obtaining an overall network kinetic model, even with the limited data available.