Fe-doped sulfated titania photocatalysts were prepared by one-step thermal hydrolysis of industrial titanyl sulfate and characterized using XRD, FT-IR, UV-Vis DRS, and N 2 adsorption-desorption techniques. The effects of the volume ratio of pre-adding water to TiOSO 4 on the structure of the titania photocatalysts were investigated. The photocatalytic activities of Fe-doped sulfated titania samples were evaluated using the photooxidation of methylene blue in aqueous solutions under UV light irradiation. The results indicate that Fe-doping induces the red shift of the absorption edge to the visible light range. Meanwhile, sulfur species in the form of sulfate are incorporated into the network of Ti-O-Ti and coordinated to titania in bidentate models, which can effectively promote the separation of the photogenerated electrons and holes. Synergistic effects of both are beneficial for improving the photocatalytic activity of the Fe-doped sulfated titania photocatalysts.Photocatalysis has received considerable attention over the past two decades because of its promising applications such as in renewable energies and environmental protections [1, 2]. As an important semiconductor photocatalytic material, titania has attracted a great deal of research interest due to its good chemical stability, insolubility in water, non-toxicity and cost-effectiveness. However, the relatively high intrinsic band gap of titania (3.2 eV for the anatase) restricts its utilization of solar energy. On the other hand, the photogenerated electrons and holes can easily recombine, which induces the low quantum efficiency. Studies indicate that iron-doping can effectively extend the spectral