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In a batch reactor, the EF advanced oxidation decolorization of aqueous solutions of methyl orange MO, a commercial azo reactive textile dye, was investigated in the presence of two different electrodes. The evaluation included various operational variables such as the IC current intensity (60 mA, 80 mA, and 100 mA), initial concentration of pollutant MO (20 mg/L, 40 mg/L, and 60 mg/L), initial pH of solution (3, 5, and 7), temperature of solution (20 °C, 30 °C, and 50 °C), and initial concentration of catalyst [Fe2+] (0.1 mM, 0.2 mM, and 0.3 mM) on the discoloration rate. A Box-Behnken Design of Experiment (BBD) was used to optimize the parameters that directly affect the Electro-Fenton (EF) process. Under the optimal experimental conditions such as [Fe2+] = 0.232 mM, pH = 3, IC = 80 mA, [MO] = 60 mg/L, and T = 30 ± 0.1 °C, the maximum discoloration rate achieved was 94.9%. The discoloration of the aqueous MO solution during the treatment time was confirmed by analysis of the UV-visible spectrum. After a review of the literature on organic pollutant degradation, the EF system provided here is shown to be one of the best in terms of discoloration rate when compared to other AOPs.