New multidoped TiO2 nanomaterials with potential photochemical response were synthesized through an uncomplicated sol–gel process, and their structures and properties were evaluated using X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-visible diffuse reflectance spectroscopy (DRS) and specific surface area (N2 adsorption-desorption). The results showed that the crystallite size of doped TiO2 nanomaterials was smaller than undoped TiO2 P25 and the surface area of these nanomaterials was found to average 800 m2/g for C,N,S-0.3Fe-TiO2. Their optical properties shifted from UV into visible light region and induced visible light absorption between 394 − 918 nm. The photochemical response of these TiO2 doped nanomaterials was followed using methyl orange (MO) dye under visible light irradiation. In fact, doped TiO2 nanomaterials with nitrogen, carbon, iron and/or sulfur exhibited a photochemical response 2 to 3 folds greater than TiO2 P25, and the photocatalytic efficiency depends on the doses and nature of dopants. In addition, the synergetic of S,N,C, and iron has shown significant effects on the crystalline structure, optical properties, pore volume and surface area.