The fabrication of novel and efficient transition metal-based catalysts for peroxymonosulfate (PMS) activation is of great significance for environmental remediation. Concerning energy consumption, the Co 3 O 4 @N-doped carbon (Co 3 O 4 @NC-350) was constructed via a half-pyrolysis strategy. The relatively low calcination temperature (350 °C) caused Co 3 O 4 @NC-350 to exhibit ultra-small Co 3 O 4 nanoparticles, rich functional groups, uniform morphology, and a large surface area. For PMS activation, Co 3 O 4 @NC-350 could degrade 97% of sulfamethoxazole (SMX) in 5 min with a high k value of 0.73364 min -1 , which was superior to the ZIF-9 precursor and other derived materials. Besides, Co 3 O 4 @NC-350 could be re-used over 5 times without obvious performance and structure change. The investigation of the influencing factors containing co-existing ions and organic matter demonstrated the Co 3 O 4 @NC-350/PMS system has satisfactory resistance. The quenching experiments and electron paramagnetic resonance (EPR) tests showed ˙OH, SO 4 ˙ - , ˙O 2 - and 1 O 2 participated in the degradation process. Moreover, the structure and toxicity of intermediates during the SMX decomposing process have been evaluated. Overall, this research provides new prospects for exploring efficient and recycled MOF-based catalysts for PMS activation.