Doxycycline hydrochloride (DOX) is a widely used broad-spectrum antibiotic that is challenging to degrade, leading to a series of environmental issues. In this study, a bimetallic oxide catalyst was synthesized through hydrothermal calcination followed by annealing. The catalytic carbon cloth anode was fabricated by bonding materials directly onto carbon cloth. Various characterization methods were employed to analyze the surface morphology, composition, and electrochemical properties of the electrodes. The materials exhibited rich surface morphology and exceptional electrochemical surface area. The catalyst primarily consisted of CeO2 and CeAlO3, demonstrating a 93.85% removal efficiency of DOX within 2 hours under optimized conditions. Even after seven consecutive degradation cycles, the DOX degradation rate remained at 82%, confirming the remarkable stability of the electrodes. The product distribution generated during the degradation of DOX was identified using LC-MS analysis, and a potential electrochemical degradation mechanism was proposed. Our results indicate that the bimetallic hybrid coordination significantly enhances the catalytic activity and electrochemical stability of the materials. This work offers a novel approach for preparing modified carbon cloth anodes with high catalytic activity and durability, laying a crucial foundation for the efficient degradation of the antibiotic DOX.