A series of layered perovskite photocatalysts, ASr 2 Ta x Nb 3−x O 10 (A=K, H; x=0, 1, 1.5, 2 and 3), were synthesized by conventional solid-state reaction followed by an ion-exchange reaction. Pt was incorporated in the interlayer of HSr 2 Ta x Nb 3−x O 10 by the stepwise intercalation reaction. The HSr 2 Ta x Nb 3−x O 10 showed hydrogen production activity and the activities were greatly enhanced by Pt co-incorporating. The x value in HSr 2 Ta x Nb 3−x O 10 had an important effect on the photocatalytic activity of the catalyst. When the x=1, the HSr 2 TaNb 2 O 10 /Pt photocatalyst showed a photocatalytic activity of 208cm 3 g −1 h −1 hydrogen evolution rate in 10vol% methanol solution under irradiation with wavelength more than 290nm from a 100-W mercury lamp at 333K. The HSr 2 TaNb 2 O 10 /Pt photocatalyst exhibited much higher photocatalytic activity than the well-known TiO 2 /Pt photocatalyst under the same conditions.