The C, N, S tri-doped TiO2 with high visible-light photo-catalysis effect was successfully prepared by mixing thiourea with the self-prepared TiO2 powder through calcining for 2h at 450°C. The TiO2 powder was obtained by homogeneous precipitation method using the metatitanic acid instead of expensive chemical reagents contained Ti as raw material. The effect of doping materials and methods on the photo-degradation rate of methylene blue and dyes was studied. The characterizations of the doped TiO2 were analyzed using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-visible absorption spectra (UV-vis). The results showed that this sample was the anatase TiO2 and contained elements C, N, S. The sample exhibited a significant response to ultraviolet and visible light. In the photo-degradation experiment, the C, N, S, tridoped-TiO2 could decolorize methylene blue and textile dyes quickly, and the photo-degradation rate of methylene blue could reach upward 98% after 3 hours under the different light sources.