The Ni-doped Bismuth tungstate（Bi2WO6）microcrystalline was successfully prepared by a facile hydrothermal route. The samples were characterized by XRD, SEM, UV-vis, EDS, BTE and Py-FT-IR. The photocatalytic denitrification performance of Ni/Bi2WO6 catalysts was measured by photocatalytic denitrification of simulation oil containing nitrogenous adopted as the model compound．The results showed that the structure of the catalyst changed by doping with Ni. More stable three-dimensional nanoparticles were found causing compact structure. The scope of the visible spectrum was expanded because of changing of energy gap from 2.67eV to 2.57eV and the photocatalytic activity was improved. The photocatalytic denitrification rate of the Ni/Bi2WO6 powder could reach to 94% under the xenon lamp light irradiation with the following conditions that photocatalytic reaction time was 120 min, 1% Ni2+ doped, and the ratio of catalyst and oil was 2 mg/40ml.