Safety and Process Intensification of Catalytic Reduction of 4-Nitophenol Using Sodium Borohydride in Flow Microreactor System

In this work, a novel approach for the catalytic reduction of 4-nitrophenol to 4-aminophenol using sodium borohydride is proposed. It was shown that a continuous-flow microreactor system is an optimal tool for PdNP synthesis with dimensions of 3.0 ± 0.5 nm, as well as the performance of catalytic tests with high process efficiency, while keeping a high level of safety. The results obtained from the microreactor system allowed for 100% conversion to 4-aminophenol and were compared to processes carried out in a batch reactor, as well as to a hybrid system which was a combination of a microreactor (synthesis of PdNPs) and batch reactor (catalytic test). These investigations were enhanced by kinetic studies, for which a stopped-flow spectrophotometer was applied due to the extremely high rate of the reaction, i.e., formation of PdNPs (2.1 s), as well as to measure in situ the rate of the heterogeneous catalytic process. To visualize the progress of the heterogeneous reaction more precisely, color coding based on transmittance measurements was employed. Furthermore, to deepen the understanding of the process, a detailed mechanism supported by DFT calculations for the conversion of 4-nitrophenol to 4-aminophenol in the presence of PdNPs was proposed.