In this present work, we report the green synthesis of mixed bimetal oxides (CuO/NiO) for the efficient reduction of toxic nitrophenols (NP, DNP and TNP) in aqueous medium. The CuO/NiO NPs were synthesized by green hydrothermal method combined calcination process. The physiochemical properties of the synthesized CuO/NiO NPs were systematically characterized by using XRD, XPS, FTIR, SEM, and HR-TEM techniques. The calcinated CuO/NiO NPs XRD pattern and SEM morphology show the high crystalline nature than the non-calcinated. Whereas, the XPS and FTIR results confirmed the formation of the metal oxide bonding and the interaction of the bimetals. The HR-TEM images showed the spherical crystals with average particle size about 25 nm. In addition, the SAED pattern confirmed the polycrystalline nature of CuO/NiO NPs. The catalytic reduction of nitro compounds to amino derivative was studied with reducing agent (NaBH4). The CuO/NiO NPs showed the high catalytic activity and completed the reduction reaction of NP, DNP and TNP with in 2, 5 and 10 min respectively. In addition, CuO/NiO NPS exhibited the excellent kinetic rate constant k value about 1.519, 0.5102, 0.4601 min−1 for NP, DNP and TNP respectively. Furthermore, the conversion product aminophenol was observed for these three nitro compounds. The proposed CuO/NiO NPs showed excellent crystal stability after the nitrophenol reduction reactions. An inexpensive CuO/NiO NPs is a promising catalysts for reduction of toxic nitro compounds to useful products in aqueous or non-aqueous medium.