A NiCoP/SiO 2 catalyst was fabricated by solid phase reaction of nickel chloride (NiCl 2 ) and cobalt chloride (CoCl 2 ) with potassium dihydrogen phosphate (KH 2 PO 3 ). The structure and properties of NiCoP/SiO 2 were characterized by X-ray powder diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, thermal gravimetric analysis and Brunauer–Emmett–Teller in detail. A mechanism was postulated based on the results of thermal gravimetric analysis. The as-prepared NiCoP/SiO 2 catalyst had excellent hydrodesulfurization activity, as indicated by using dibenzothiophene as the reactant. Hydrodesulfurization occurred sequentially following hydrogenation of dibenzothiophene and desulfurization in the presence of NiCoP/SiO 2 .