Abstract: A Fe₂O₃-CeO₂/γ-Al₂O₃ catalyst was prepared by the successive impregnating procedure, and the preparation parameters were optimized.BET, X-ray photoelectron spectroscopy (XPS) and X-ray fluorescence spectroscopy (XRF) techniques were performed to characterize the Fe₂O₃-CeO₂/γ-Al2O3 catalyst.The catalytic activity of the prepared catalyst was investigated by catalytic wet peroxide oxidation (CWPO)of azo dyes at room temperature (25℃) and atmospheric pressure.The results showed that Fe₂O₃-CeO₂/γ-Al2O3 catalyst had excellent catalytic activity.For artificial wastewater of methyl orange (dye concentration 500 mg·L^-1), it was possible to remove 88.77% of color, 89.54% of COD and 81.44% of TOC after 3 h of oxidation at 30 g·L^-1 Fe₂O₃-CeO₂/γ-Al₂O₃ and 330 mg·L^-1 H₂O₂.