Contaminated water is considered one of the major problems facing societies in recent years, leading to the increasing need for new purification systems, which has consequently become a leading area of research among scientists. Photocatalysts and Advanced Oxidation Processes (AOPs) are recognized as effective techniques for water purification and pollutant removal. These methods are particularly applicable in reducing both organic and inorganic contaminants in wastewater. The development of new technologies and nanostructures can enhance the efficiency of these processes and make them more suitable for broader use in water treatment. In the present study, a TiO₂/CoFe₂O₄ nanocomposite was synthesized using the sol-gel method. X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and UV-visible diffuse reflectance spectroscopy (UV-vis DRS) were employed to analyze the synthesized composite. The photocatalytic activity of the produced composite was studied through the degradation of methyl orange. The X-ray diffraction analysis indicated that titania was in the anatase phase while cobalt ferrite exhibited a cubic spinel structure. The average particle size of the nanoparticles was approximately 100 nm. The synthesized composite demonstrated effective degradation performance without the addition of oxidants. The photocatalytic degradation of titania increased followed by the addition of cobalt ferrite. The band gap energy of the samples decreased from 2.3 eV to 2.91 eV following the inclusion of CoFe₂O₄. The kinetic rate constants for the degradation of methyl orange for pure titania and composite samples were 0.0082 and 0.0143, respectively. Scavenger tests were conducted to investigate the photocatalytic degradation mechanism, which showed that superoxide and hydroxyl radicals were the most active species in the photocatalytic degradation process.