A sol-gel method was used to prepare TiO2and sulfur-TiO2(S-TiO2)nanocomposites, which were characterized by N2 adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy, photoluminescene, ultraviolet visible and transmission electron microscopy measurements. The photocatalytic performance of TiO2 and S-TiO2nanocomposites, with respect to the photocatalytic oxidation of cyanide under visible light irradiation, was determined. The results reveal that S is well dispersed on the surface of TiO2 nanoparticles. Additionally, the surface area of the S-TiO2nano-composites was observed to be smaller than that of the TiO2nanoparticles because of blocked pores caused by doping with S. The S-TiO2nanocomposite (0.3 wt% S) exhibited the lowest band gap and the highest photocatalytic activity in the oxidation of cyanide. The photocatalytic performance of S-TiO2(0.3 wt% S) nanocomposites was stable, even after the fifth reuse of the nanoparticles for the oxidation of cyanide.