To reduce the various hazards of SMX to aquatic ecosystems, in this study, magnetically separable LaCoO3@Fe3O4 catalysts for the degradation of sulfamethoxazole (SMX) in water by activated peroxymonosulfate (PMS) were successfully prepared by using cobalt oxalate recovered from spent batteries using sol–gel, hydrothermal, and high-temperature calcination methods. The main factors influencing the reaction and the effect of coexisting ions on the degradation efficiency of SMX were investigated. The results showed that under optimal conditions ([SMX] = 30 mg, [LaCoO3@Fe3O4] = 10 mg/L, [PMS] = 30 mg/L, pH (initial) = 7.02), the LaCoO3@Fe3O4/PMS system degraded SMX up to 93 % in 15 min. The degradation of SMX in the LaCoO3@Fe3O4/PMS system was shown to be achieved by a combination of radical (SO4•-/•OH/•O2–) and non-radical (1O2) pathways by quenching experiments and electron paramagnetic resonance spectroscopy (EPR) analysis. Then, three possible degradation pathways were proposed using LC-MS, and Ecological Constitutive Relationship (ECOSAR) analysis showed that the toxicity of the intermediate products was all lower than that of SMX, indicating that the system is feasible for SMX degradation. This study provides a new idea for activating PMS for the degradation of antibiotics in water by preparing catalysts using precious metals from recycled batteries.