ABSTRACT Procion Red MX-5B (PRM) is harmful to both human health and the environment, and it is resistant to degradation through conventional wastewater treatment methods. In this study, solar-Fenton-like oxidation was used to treat it, employing Fe-doped corn cob ash and Fe-doped g-C₃N₄ (CN) photocatalysts. First, a characterization study (SEM, XRD, BET, PL, and XPS) was performed and its results proved that they were successfully synthesized and the most promising one was 20 wt. % Fe containing Fe/g-C3N4 ;(%20FeCN). Then, the influence of reaction parameters was studied and the optimal conditions were determined to be 0.2 g/L of %20FeCN, 10 mm of HPC, and pH = 3. At these reaction conditions, complete degradation of PRM was observed. Lastly, a kinetic study was performed and the reaction was found to follow the first-order kinetics, with an activation energy calculated to be 40.88 kJ/mol. This suggests that the 20% FeCN catalyst is highly effective and holds great promise for PRM degradation.