MCM-41/CeO 2 and MCM-48/CeO 2 were synthesized by direct and indirect methods in solvent media and by grinding method in a solvent-free media. The materials prepared by grinding method are characterized by X-ray diffraction, infrared spectrum analysis, and N 2 adsorption and desorption. Surface areas and pore size of MCM-48 /CeO 2 were obtained with values of 680.9 m 2 Ág −1 and 1.64 nm, respectively, by BET method. The results showed that CeO 2 nanoparticles were introduced into MCM-41 and MCM-48, and there was formation of CeO 2 crystallites as secondary phase in the extra framework of MCM-41 and MCM-48. MCM-41/CeO 2 and MCM-48/CeO 2 materials are used as photocatalysts in degradation of Congo red as a dye pollutant. The MCM-41/CeO 2 and MCM-48/CeO 2 prepared by grinding method showed the higher photoreactivity with 97.6 % and 93.1 %, respectively, of degradation of Congo red. The higher photoreactivity is due to the complete incorporation of cerium ions in mesoporous material of MCMs in a solvent-free media.