This study deals with the elimination of methyl orange (MO) from an aqueous solution by utilizing the 3D electroFenton process in a batch reactor with an anode of porous graphite and a cathode of copper foam in the presence of granular activated carbon (GAC) as a third pole, besides, employing response surface methodology (RSM) in combination with Box-Behnk Design (BBD) for studying the effects of operational conditions, such as current density (3–8 mA/cm2), electrolysis time (10–20 min), and the amount of GAC (1–3 g) on the removal efficiency beside to their interaction. The model was veiled since the value of R2 was high (>0.98) and the current density had the greatest influence on the response. The best removal efficiency (MO Re%) at pH = 3 was 95.62% with an average energy consumption of 6.22 kWh/kg MO, which was achieved under maximal conditions of current density = 5.12 mA/cm2, mass of GAC = 3 g, and time = 20 min with small amounts of Fe2+ (0.124 mM), and Na2SO4 (0.02 M). Moreover, the present work investigated the effectiveness of 3D electro-Fenton assisted by ultrasound known as Sono-ElectroFenton (SEF), by following a new strategy based on applying the minimum circumstances of EF and comparing its results with that of SEF under the same conditions. MO Re% for EFmin was 49.24% while SEF was 50.51%, which is considered an exiguous improvement. However, using copper foam as a working electrode in the 3D EF system for the degradation of MO was an excellent choice. Furthermore, the suggested approach is characterized by simplicity, speed, and efficiency with a high percentage of pollutant removal, in addition to being eco-friendly.
