Abstarct:   Industrial effluents are more important due to high consumption and variety of pollutants. The used caustic wastewater is very toxic and has an unpleasant smell due to its high alkalinity, sulfide concentration and high salinity; therefore, it is necessary to remove these pollutants from the wastewater before the final discharge to the environment. Recently, advanced electrochemical oxidation processes, including the Electrofenton process, have been developed to remove resistant organic pollutants. These processes are very efficient and are suggested as an attractive method for treating industrial effluents with high TDS and TSS. In this study, in order to treat the caustic wastewater used by the electrofenton process, the surface of the graphite electrode was modified in three different ways. First, the surface of the graphite cathode electrode was coated with the porous nanoparticle of mextal-organic frxamework MIL-88A(Fe). Then, in order to improve the efficiency of wastewater treatment, a coating of the combination of MIL-88A(Fe) nanoparticles and CuFe-LDH double laxyer hydroxide was applied on the surface of the graphite electrode with two paste and hydrothermal methods. In order to investigate the structural features of the coated graphite electrode and ensure the correctness of its surface modification, various characterization analyzes such as SEM, EDX, FTIR, XRD, BET, AFM, EIS and zetapotential were performed. Comparing the performance of the fabricated electrodes showed that the COD removal efficiency for G/MIL-88A(Fe), G/MIL-88A(Fe)/CuFe-LDH-P and G/MIL-88A(Fe)/CuFe-LDH electrodes -H was obtained as 55.4%, 73% and 90%, respectively. In the following, the effect of various parameters, including electrolyte concentration, hydrogen peroxide concentration, wastewater pH, applied current intensity, the presence of various inhibitors on the wastewater treatment efficiency was investigated using the best electrode (G/MIL-88A(Fe)/CuFe-LDH-H) and the optimal values were determined as 0.05 mol/L, 100 µL, pH=7, and 120 mA during the reaction time of 90 minutes. The reproducibility and stability of the modified electrode showed that the reduction of COD removal efficiency is less than 10% at the end of the fifth cycle, and the amount of iron and copper mextals released from the nanocomposite coating structure is minor. This indicates the high reusability of the modified electrode and its favorable stability in the operational conditions of wastewater treatment. Shahrood University of Technology