Mesoporous catalyst S‐ZIF‐(1:2.5)@NixSy was prepared using ZIF‐(1:2.5) as a precursor. These composite materials were characterized by using scanning microscope (SEM), transmission electron microscopy(TEM), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS) and N2 adsorption‐desorption techniques, and studied as catalysts for the reduction of 4‐nitrophenol (4‐NP) to 4‐aminophenol (4‐AP), congo red (CR), methyl orange (MO), and methylene blue (MB). The BET specific surface area and pore volume of the catalyst were 167.49 m2/g and 0.32 m3/g respectively. The doping of S improves the catalytic performance of the catalyst. S‐ZIF‐(1:2.5)@NixSy showed an excellent catalytic rate (kapp = 22.3 × 10–3/s) in the experiment of reductive degradation of 4‐NP. In addition, S‐ZIF‐(1:2.5)@NixSy also showed good catalytic activity for the degradation of CR, MB, and MO, completing the catalytic reaction within 60, 60, and 90 s, respectively. The kapp values for CR, MB, and MO are 29.0 × 10–3/s, 44.0.0 × 10–3/s, and 29.2 × 10–3/s, respectively.