The new composite MoS2/CeO2-Co3O4 showed high efficiency of hydrogen evolution under visible light irradiation, and the synthesis and properties of photocatalyst were also introduced in this paper. The hydrogen evolution of 1%MoS2/CeO2-Co3O4 catalyst reached 221 mu mol in 3 h, and the catalyst still exhibited high activity after 12 h under visible light irradiation of 10%TEOA solution, which indicates that the photocatalyst had excellent photocatalytic activity and light stability. The analysis of XRD, XPS, SEM and TEM showed that MoS2/CeO2-Co3O4 was successfully synthesized. The analysis of BET showed the specific surface area of photocatalyst composite increased due to the addition of CeO2 and MoS2, which was good for EY adsorption, accelerated the electron transfer rate and improved the production of hydrogen. The PL and electrochemical analysis results showed that CeO2-Co3O4 loaded on the surface of MoS2 nanoparticles can significantly promote electron transfer, restrain the recombination of electron and hole and improve the rate of hydrogen production. Therefore, the oxide of the rare-earth element Ce and Co3O4 might be good for the design of a new photocatalyst.