WO3/ZrO2 solid superacid catalysts were prepared by using Zr(OH)4 as supporter with ultrasonic impregnation and general impregantion,respectively. The catalysts were characterized by means of BET, XRD, NH3-TPD and SEM. The results revealed that the catalyst prepared with ultrasonic impregnation, compard with general impregantion, possessed large surface areas and supported more dispersion tungste active component. Calcined at high temperature, ZrO2 in the catalyst yet existed mainly in the tetragonal phase and the catalyst presented higher acidic strength and acid amounts. Furthermore, the catalyst was dispersed in small particle and gave strong catalytic activity in the catalytic oxidative desulfurization of diesel.