nanocatalysts was examined in hydrodesulfurization of thiophene. The nanocatalysts were synthesized via sonochemical technique. The prepared samples were characterized by XRD, FE-SEM, BET, and FTIR analysis. The catalytic activity in hydrodesulfurization reaction was investigated in a batch stirred slurry reactor at 160 • C and atmospheric pressure. The characterizations confirmed highly dispersion of active phase and formation of amorphous AlPO 4 species on the support surface. The results obtained from thiophene hydrodesulfurization showed the nanocatalysts contained 1 wt% of phosphorus had the highest activity. The CoMoP/Al 2 O 3 and NiMoP/Al 2 O 3 nanocatalysts with optimum phosphorus loading nearly gave 100% conversion of thiophene, so that the sulfur compound concentration in final solution was less than 50 ppm.