Abstract: The desulfurization of diesel oil was conducted via oxidation-adsorption process, using H₂O₂ as oxidant in the presence of amphiphilic catalyst and mesoporous silica-gel as the adsorbent. The fixed-bed dynamic adsorption method was employed to evaluate the oxidation-adsorption desulfurization capability of the catalysts and the effects of the property of silica-gel, oxidation and adsorption conditions on desulfurization efficiency were investigated. It was proved that the silica-gel possessed the mesoporous structure characterized by small-angle XRD and N₂ adsorption-desorption isotherm. Compared with adsorption process, oxidation-adsorption process could availably increase the adsorptive capacity and selectivity of silica-gel adsorbent to sulfur compounds in diesel oil.The sulfur removal efficiency remained as high as 85.89% when the volume ratio of diesel oil to silica-gel was 15. Sulfur removal efficiency reached up to 94.57% when adsorption temperature, space velocity and volume ratio of diesel oil to silica-gel were 40℃, 6.0 h^-1 and 1 respectively.