Abstract: A series of Fe-Ce/ZSM-5 catalysts were synthesized via equivalent-volume co-impregnation of ferric nitrate and cerium nitrate on micro-meso pore ZSM-5. The pore volume impregnation is thought the one with simple operation without complex equipment, and high efficiency. The optimal catalyst preparation condition was evaluated by catalytic oxidation of hydrogen peroxide (H2O2) technology (CWPO) to degrade the methyl orange solution. The results indicate that the best preparation conditions are: co-impregnation solution concentration 2.0 mol/L with the mole ratio of Fe/Ce of 3:1 and the calcination temperature 400 °C. In the presence of H2O2 and reaction time 100 min, more than 85% methyl orange is removed. TEM and XRD results show that Fe-Ce/ZSM-5 remains the ZSM-5 pore structure and the catalytic properties of iron oxides and cerium oxides.