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Developing a bifunctional catalyst with low cost and high catalytic performance in NaBH4 hydrolysis for H2 generation and selective reduction of nitroaromatics will make a significant impact in the field of sustainable energy and water purification. Herein, a low‐loading homogeneously dispersed Pd oxide‐rich Co3O4 polyhedral catalyst (PdO‐Co3O4) with concave structure is reported by using a metal–organic framework (MOF)‐templated synthesis method. The results show that the PdO‐Co3O4 catalyst has an exceptional turnover frequency (3325.6 molH2 min−1 molPd−1), low activation energy (43.2 kJ mol−1), and reasonable reusability in catalytic H2 generation from NaBH4 hydrolysis. Moreover, the optimized catalyst also shows excellent catalytic performance in the NaBH4 selective reduction of 4‐nitrophenol to 4‐aminiphenol with a high first‐order reaction rate of approximately 1.31 min−1. These excellent catalytic properties are mainly ascribed to the porous concave structure, monodispersed Pd oxide, as well as the unique synergy between PdO and Co3O4 species, which result in a large specific surface area, high conductivity, and fast solute transport and gas emissions.

The high‐efficiency multifunctional materials have considerable significance in the area of sustainable energy to developing a cross‐usable and low‐cost catalyst. Nevertheless, substantial challenges are ahead on designing and synthesizing a high performance in a scalable and straightforward manner. Here, we have developed a novel bifunctional catalyst based on Ru/CoP nanoboxes (NBs) prepared using ZIF‐67 as a precursor. The nano hollow box structure and the strong electronic interaction between Ru clusters and CoP component are confirmed. The Ru/CoP NBs as a catalyst show excellent activities for catalytic NaBH4 hydrolysis such as high turnover frequency (1202.2 min−1), and small electrocatalytic H2 evolution overpotential (49 mV@10 mA cm−2) under ambient conditions. Besides, Ru/CoP NBs also display good stability and reusability. The excellent catalytic performance of Ru/CoP NBs is attributed to the synergy between Ru clusters and CoP species as well as the unique morphology that accelerates charge transfer, provides higher active surface area, and facilitates solute transport and gas emission.

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