The catalytic activities of the iron catalysts over activated carbon supports prepared by different activation methods in the heterogeneous Fenton-like oxidation of Procion Red MX-5B were investigated. The activated carbons were prepared from walnut shells by applying physical and three chemical activation methods, including HNO3, ZnCl2, and KOH activations to obtain various catalyst supports. KOH-activated carbon catalyst was assessed to be the most efficient one. Under the optimum reaction conditions, 47.5% COD removal, 51.6% degradation, and 91.6% decolorization efficiencies were achieved in the presence of this catalyst. In the kinetic study, the activation energy was evaluated as 47.36 kJ/mol.