A sol-gel method was used to prepare TiO_2 and sulfur-TiO_2(S-TiO_2) nanocomposites, which were characterized by N_2 adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy, photoluminescene, ultraviolet visible and transmission electron microscopy measurements. The photocatalytic performance of TiO_2 and S-TiO_2 nanocomposites, 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 TiO_2 nanoparticles. Additionally, the surface area of the S-TiO_2 nanocomposites was observed to be smaller than that of the TiO_2 nanoparticles because of blocked pores caused by doping with S. The S-TiO_2 nanocomposite(0.3 wt% S) exhibited the lowest band gap and the highest photocatalytic activity in the oxidation of cyanide. The photocatalytic performance of S-TiO_2(0.3 wt% S) nanocomposites was stable, even after the fifth reuse of the nanoparticles for the oxidation of cyanide. A sol-gel method was used to prepare TiO_2 and sulfur-TiO_2 (S-TiO_2) nanocomposites, which were characterized by N_2 adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy, photoluminescene, ultraviolet visible and transmission electron microscopy measurements The photocatalytic performance of TiO 2 and S-TiO 2 nanocomposites, 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 TiO 2 nanoparticles. S-TiO_2 nanocomposites was observed to be smaller than that of the TiO_2 nanoparticles because of blocked pores caused by doping with S. The S-TiO_2 nanocomposite (0.3 wt% S) exhibited the lowest band gap and the highest photocatalytic activity in the oxidation of cyanide. The photocatalytic performance of S-TiO 2 (0.3 wt% S) nanocomposites was stable, even after the fifth reuse of the nanoparticles for the oxidation of cy anide.