In-situ synthesised Al2O3/USL-supported NiW-P catalysts were prepared by the incipient-wetness co-impregnation method or the incipient-wetness serial impregnation method with ammonium metatungstate, nickel nitrate and different phosphorus sources including phosphoric acid and diammonium phosphate. The physicochemical properties of the catalysts were characterized by means of XRD, NH3-TPD, H2-TPR, UV-Vis DRS, Roman and nitrogen adsorption-desorption isotherm. Catalytic performances of the catalysts were tested in a high pressure fixed bed microreactor with high sulfurous and nitrous FCC diesel as feed. The evaluation results showed that the activities of hydrodesulfurization and hydrodenitrogenation were obviously enhanced, and sulfur and nitrogen contents in the products were both below 20 μg·g-1 over γ-Al2O3/USL supported-NiW catalyst modified by appropriate content of phosphoric acid.