We used CTAB as the soft template and tetrabutyl titanate, Thiourea, and Ytterbium nitrate as raw materials to prepare S–Yb co-doped TiO2 nanoparticles by a hydrothermal method. The structure and properties of the prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy coupled with energy dispersive X-ray spectroscopy (TEM-EDS), ultraviolet–visible spectroscopy (UV-Vis), N2 adsorption/desorption with the Brunauer– Emmett–Teller (BET) method, and photoluminescence (PL). The photocatalytic performance of the sample was evaluated by using methylene blue as a model pollutant and a xenon lamp as the light source. The results showed that TiO2 contained a single anatase phase and Yb and S were successfully doped into the crystal lattice of TiO2. Doping resulted in smaller grains, lower band gap, and larger specific surface area, reducing the probability of recombination of the photogenerated electron-hole. The catalyst with a molar ratio of doped S and Yb of 2:1.5 (2.0%S/1.0%Yb-TiO2) exhibited the best catalytic performance, with a degradation efficiency as high as 97.75 % after being irradiated by a 500 W xenon lamp for 90 min.