Automated synthesis and data accumulation for fast production of high-performance Ni nanocatalysts

Diverse methods have been developed for the synthesis of active nanocatalysts involving various heterogeneous catalytic reactions. Thus far, numerous trial-and-error runs have been done to find the effective and practical ways. In the present work, the All-In-One (AIO) reactor system with a well-designed synthesis program, now in pilot stage, was first exploited as a reliable synthesis tool to find the optimum conditions for the production of Ni nanocatalysts. Using an activated charcoal support, active Ni nanoparticles of 7.8–11.8 nm (labeled A001–A007 in the program) were produced. These were achieved using a melt-impregnation process, which was controlled by variations in the applied gas (N₂ and H₂) and temperature (400 °C, 450 °C, and 500 °C) used as critical factors in the calcination step. Based on the optimization of the reaction sequence, each Ni nanocatalyst could be prepared within 5 h and 22 min. In particular, the optimum Ni nanocatalyst (A006) with the smallest particle size (7.8 nm), prepared under H₂ flow at 400 °C, exhibits the highest catalytic activity (0.748 mmol_4-NP·g_cat⁻¹·s⁻¹) among the Ni catalysts for 4-nitrophenol (4-NP) reduction to 4-aminophenol (4-AP). This activity is much higher than that of conventional supported Ni nanocatalysts (0.551 mmol_4-NP·g_cat⁻¹·s⁻¹) produced using the wetness method.