Abstract: Graphene/Fe-doped titania composite was prepared by one-step thermal hydrolysis of industrial titanyl sulfate solution with graphene oxide solution as priming,and the composite was characterized using XRD,SEM,FT-IR,UV-vis DRS and XPS.The photocatalytic performance of the graphene/Fe-doped titania composite was evaluated by the photooxidation of methylene blue under UV light and visible light irradiation,respectively.The effects of graphene oxide solution concentration,feeding rate and heating rate on the photocatalytic activity of the graphene/Fe-doped titania composite were systematically investigated.The results indicate that the doping-Fe enters TiO₂ lattice in the form of Fe³⁺ to form impurity energy level and extend the spectral response range to visible light of the composite consequently.Graphene is beneficial to separate the photoexcited electron-hole pair and then to improve the quantum efficiency of photocatalysis.The optimal hydrolysis conditions are graphene oxide solution concentration of 0.03 mg/mL,feeding rate of 8 mL/min and heating rate of 1.0 ℃/min.The photocatalytic efficiency of the composite obtained at these conditions can reach 94.15% and 80.89% respectively under UV light and visible light irradiation.