In order to more easily separate TiO2 photocatalyst from the treated wastewater, TiO2 was immobilized oil the Surface of coal fly ash by employing three kinds of approaches, sol-gel procedure ambient hydrolysis procedure and hybrid slurry procedure. The effects of loading method oil the structural property of TiO2-coated coal fly ash (TiO2/CFA), such as morphology, crystal structure, porous property and ultraviolet-visible absorption were investigated, and the photocatalytic activity of TiO2/CFA was evaluated by the photocatalytic depigmentation and mineralization of methyl orange solution. The results show that TiO2/CFA particles are easy to precipitate and recover from water. The hybrid slurry procedure is a more proper method to immobilize TiO2 oil coal fly ash than file other two procedures because the TiO2/CFA sample prepared by hybrid Slurry procedure exhibits higher photocatalytic activity and better repeatability. (C) 2009 Elsevier B.V. All rights reserved.