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Porous phosphide NixCoyP composite nanomaterials are successfully synthesized at different Ni/Co ratios (=0, 0.5, 1, and 2) to reduce 4-nitrophenol. The X-ray diffraction and X-ray photoelectron spectroscopy results demonstrate that the products are CoP, NiCoP/CoP, NiCoP, and NiCoP/Ni2P when the Ni/Co ratio is 0, 0.5, 1, and 2, respectively. The products exhibit different catalytic performance for reduction of 4-nitrophenol at room temperature. Among them, the pure NiCoP delivers a better catalytic efficiency with k app = 677.4 × 10 − 2   min − 1 and k = 338.7   ( Lg − 1 min − 1 ) , due to the synergy between Ni and Co atoms. The sequence of catalytic efficiency of different samples is CoP < NiCoP/CoP < NiCoP/Ni2P < NiCoP.