Abstract:ammonium metavanadate, phosphomolybdic acid as active component were used to HMS mesoporous materials by sol-gel method to obtain V/Mo-HMS catalysts, and the modified catalysts were characterized by X-ray differential(XRD), scanning electron microscopy(SEM), N2 adsorption- desorption(BET), H2 temperature-programmed reduction (H2-TPR), X-ray photoelectron spectroscopy (XPS), thermal analysis(TG-DTA). The catalytic performance the V/Mo-HMS was investigated in the oxidation of benzyl alcohol to benzaldehyde using aqueous hydrogen peroxide(mass fraction 30% H2O2) as oxidant and the effect of HMS modified by various matal on catalytic oxidation reaction was tested. The results indicated that the specific surface area, pore volume and mean pore size of V/Mo-HMS were decreased Compared with HMS. The catalytic activity of V/Mo-HMS was better than the HMS modified by other matals. Conversion rate of benzyl alcohol reached 68.16 % with the selectivity of 89.02% to benzaldehyde when benzyl alcohol was 0.1mol, 30% H2O2 was 0.8 mol, catalyst amount was 0.07 g at 90 ℃ for 6h and ethyl acetate as solvent. The catalyst can be recycled and reused.