The bio-electro-fenton (BEF) system is a novel technology that can be utilized to degrade both emerging and persistent pollutants while producing clean, green, and sustainable energy. Various catalysts that have a high active surface area are employed in these systems to enhance the oxygen reduction reaction (ORR) efficiency. In this study, the Nickel/Cobalt metal-organic framework (Ni/Co BTC-MOF) as heterogeneous catalyst was synthesized and deposited by the cathodic electrochemical deposition method on the carbon felt (CF) and graphite plate (GP) electrodes. The results of FT-IR, Field Emission Scanning Electron Microscopy (FE-SEM), X-ray Diffraction (XRD), and Energy Dispersive X-ray spectroscopy (EDS) analysis proved that the synthesis of Ni/Co-BTC MOF successfully carried out. The performance and positive effect of the modified electrodes in ORR were investigated and compared in electrical energy generation. Finally, bio-electro-degradation of bisphenol-S (BPS) as one of the endocrine-disrupting compounds (EDCs) was studied by the optimal modified electrode. According to the results of electrochemical experiments, the highest maximum power density is equal to 133.6 mW/m