A series of CdS/M(x)-MCM-41 (M = Zr, Ti, x stands for molar ratio of M/Si) photocatalysts were preprared by hydrotherm, ion-exchange and sulfidation process. The catalysts were characterized by X-ray diffraction, UV-vis spectra and N-2 adsorption-desorption isotherm et al.. The characterization results shown that Zr or Ti was successfully doped into the mesoporous of MCM-41, and CdS was also successfully incorporated into such modified mesoporous. The results of photocatalytic performance for hydrogen production shown that CdS/Zr(0.005)-MCM-41 and CdS/Ti(0.02)-MCM-41 had the highest hydrogen evolution activity in triethanolamine aqueous solution under visible light (gimel > 430 nm) irradiation, which can be explained by the diffusion velocity of the reactants and resultants and the protection which MCM-41 provided for CdS. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.