The Fe2O3/SiO2 catalysts have been prepared by an impregnation method and calcined at different temperatures (350, 400, and 450 degrees C). The three obtained catalysts are characterized by X-ray powder diffraction (XRD), temperature programmed reduction (TPR), scanning electron microscopy (SEM) and BET. The results showed that the increase of the calcination temperature promoted the dispersion of Fe particles on the surface of the SiO2 support, which results in the change of the BET surface area, the average pore size, and the pore volume of the Fe2O3/SiO2 catalysts. According to the catalytic reaction results, the Fe2O3/SiO2 catalyst calcined at 400 degrees C show the higher catalytic activities than others, and the COD removal is found to be about 64.6% within 60 min, pH 3, 100 mu L of H2O2 in a 50 mL phenol solution.