Y2Cu2O5photocatalyst was successfully prepared via solid state reaction and further combined with TiO2by a sol-gel method and a solid phase method, respectively. For comparison, Pt particles were loaded to prepare Pt-Y2Cu2O5via a hydrogen reduction method. All the samples were characterized by thermogravimetry and differential thermal analysis (TG/DTA), X-ray diffraction (XRD), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), and scanning electron microscopy (SEM) techniques. Photocatalytic H2evolution activities of the as-obtained samples were evaluated from aqueous oxalic acid solution under simulated sunlight irradiation. The effects of photocatalyst concentration, TiO2content, and composite method on the H2evolution activities of the as-obtained photocatalysts were investigated. The results show that, when the concentration of photocatalyst is 0.8 g L−1, the TiO2-Y2Cu2O5composite photocatalyst prepared by a sol-gel method exhibits the optimized photocatalytic activity, and the H2production rate is 4.35 mmol h−1g−1with 30 wt.% content of TiO2.