A B S T R A C TThe degradation of Reactive Red 3 dye (RR3) by Photocatalytic Wet Peroxidation (PCWPO) on Fe-RH-MCM-41 (Si/Fe = 10) catalyst, a mesoporous molecular sieve prepared by direct hydrothermal technique was studied. Rice husk silica was used as silica precursor. The catalyst was investigated by X-ray diffraction, X-ray Fluorescence spectrophotometer, BET and UV-DRs techniques. The catalyst activity was designed by Box-Behnken design (BBD). The effects of initial pH of the solutions, initial H 2 O 2 concentrations and reaction temperature in PCWPO process were investigated by BBD. The characterized results indicate a surface area of about 801 m 2 /g and indicate that ferric was not detected on the surface of RH-MCM-41. Initial pH of dye solution and temperature of reaction were found to be significant on RR3 removal while initial concentration of H 2 O 2 was found to be insignificant. The maximum condition was 48.375 mM for initial H 2 O 2 concentration, 50˚C for reaction temperature, and 3 for initial pH of the solution.