Various compositions of cobalt and sulfur co-doped titania nano-photocatalyst are synthesized via sol–gel method. A number of techniques including X-ray diffraction(XRD), ultraviolet–visible(UV–Vis), Rutherford backscattering spectrometry(RBS), thermal gravimetric analysis(TGA)Raman, N2 sorption, electron microscopy are used to examine composition, crystalline phase, morphology, distribution of dopants, surface area and optical properties o synthesized materials. The synthesized materials consisted of quasispherical nanoparticles of anatase phase exhibiting a high surface area and homogeneous distribution o dopants. Cobalt and sulfur co-doped titania demonstrated remarkable structural and optical properties leading to an efficient photocatalytic activity for degradation of dyes and phenol under visible light irradiations. Moreover, the effect of dye concentration catalyst dose and p H on photodegradation behavior of environmental pollutants and recyclability of the catalyst is also examined to optimize the activity of nano-photocatalys and gain a better understanding of the process. Various compositions of cobalt and sulfur co-doped titania nano-photocatalyst are synthesized via sol-gel method. A number of techniques including X-ray diffraction (XRD), ultraviolet-visible (UV- Vis), Rutherford backscattering spectrometry (RBS) thermal gravimetric analysis (TGA) Raman, N2 sorption, electron microscopy are used to examine composition, crystalline phase, morphology, distribution of dopants, surface area and optical properties o synthesized materials. The synthesized materials consisted of quasispherical nanoparticles of anatase phase exhibiting a high surface area and homogeneous distribution o dopants. Cobalt and sulfur co-doped titania exhibit remarkable structural and optical properties leading to an efficient photocatalytic activity for degradation of dyes and phenol under visible light irradiations. Moreover, the effect of dye concentration catalyst dose and p H on photodegradation behavior of environmental pollutants and recyclability of the catalyst is al so examined to optimize the activity of nano-photocatalys and gain a better understanding of the process.