Herein, two-ligand nickel-based MOF (JUC-85Ni) have been prepared by choosing high N-containing and S-containing ligand. On this basis of the research, the NiS2 nanoparticles dispersed N and S co-doped carbon materials (NiS2@NSC) are fabricated through the sulfidation of JUC-85Ni precursors with thioacetamide (TAA). The rationally designed NiS2@NSC catalysts are conducted a test for catalytically reducing 4-nitrophenol (4-NP) to environment friendly 4-aminophenol (4-AP) under NaBH4 alkaline condition. The superior features endows the catalyst with outstanding catalytic activity and recycling performance, and support it great potential for wastewater treatment.