The PbO2/Co3O4 composite electrodes were synthesized using the composite co-deposition method, which involved the incorporation of Co3O4 nanoparticles into a PbO2 coating. These composite electrodes were employed as anodes for phenol electrooxidation in wastewater treatment. The results demonstrate that the PbO2/Co3O4 composite electrode exhibits a three-dimensional porous structure, leading to a significant increase in the electrochemically active surface area. Electrochemical measurements indicate that the composite electrode achieves a minimum oxygen evolution potential of 526.5 mV. Moreover, the electrode facilitates the indirect degradation of phenol, even at low voltage (0.45 V). The unique structure, improved conductivity, and enhanced surface area of the electrode contribute to its exceptional performance in phenol degradation. Additionally, this approach offers the potential for synergistic integration with other treatment methods, providing a sustainable and energy-efficient solution for removing persistent organic compounds from wastewater.