Amidst the rapid development of the textile industry, wastewater problems also arise. High-performance materials for reactive black 5 (RB5) dye treatment by adsorption and photocatalysis were evolved using Titanium dioxide (TiO2) nanoparticles on carbon media. Herein, the synthesis of spherical carbon via the water–in–oil emulsion method alongside a sol–gel process and the production of TiO2 nanoparticles using the precipitation procedure of Titanium isopropoxide and carbonization at 700–900 °C for 2 h are a novel approach in this work. The characterization of these materials indicates that different temperatures result in distinct properties, for instance, raised pores on the surface of the media and changes in the crystal structure of TiO2. The results show that the as-synthesized material carbonized at 900 °C had distinguished dye adsorption, up to 430 ppm in 1 h, due to their high surface area and pore volume. On the contrary, the calcined 700 °C condition had the prominent photocatalytic efficiency on account of the heterojunction band gap between anatase and rutile crystal structure. A mixed phase minimizes the charge recombination, subsequently increasing the photocatalytic capability.