Abstract: TiO₂/kaolin composite photocatalysts were prepared from kaolin particles by the titanic chloride hydrolysis method and the structure were characterized by IR，SEM，X-ray and BET techniques. It is showed by the IR and BET results that TiO₂ is partly entered into the layers of kaolin. The composite catalytic activities were evaluated by photocatalytic reaction of oxalic acid. Compared with unloaded nano-TiO₂ ，this preparation leads to a highly active photocatalyst. Meanwhile calcination temperature effecting on photocatalytic activity of the TiO₂/kaolin composite was also studied.