This study investigated the decolorization of Remazol Black (RBB) using a TiO2 photocatalyst modified by S and Co co-doped TiO2 (S-Co-TiO2) from a single precursor. X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and UV–Vis specular reflectance spectroscopy were used to characterize the photocatalysts. The results revealed that the band-gap energy of the doped and co-doped TiO2 decreased, with the S-Co-TiO2 8% showing the greatest one, and was found to be 2.78 eV while undoped TiO2 was 3.20 eV. The presence of S and Co was also identified through SEM-EDX. An activity study on RBB removal revealed that the S-Co-TiO2 photocatalyst showed the best result compared to undoped TiO2, S-TiO2, and Co-TiO2. The S-Co-TiO2 8% photocatalyst reduced RBB concentration (20 mg L−1) up to 96% after 90 min of visible light irradiation, whereas S-TiO2, Co-TiO2, and undoped TiO2 reduced it to 89%, 56%, and 39%, respectively. A pH optimization study showed that the optimum pH of RBB decolorization by S-Co-TiO2 was 3.0, the optimum mass was 0.6 g L−1, and reuse studies show that S-Co-TiO2 8% has the potential to be used repeatedly to remove colored pollutants. The results obtained indicate that the modification of S, Co co-doped titania synthesized using a single precursor has been successfully carried out and showed excellent characteristics and activity compared to undoped or doped TiO2.