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The activation of PMS to produce active species is an attractive technique for antibiotic degradation but is restricted to the low reaction kinetics and high costs. In this work, a cobalt-based catalyst was prepared by in situ electrodeposition to enhance the electrically activated PMS process for the degradation of antibiotics. Almost 100% of pefloxacin (PFX) was removed within 10 min by employing Co(OH)₂ as the catalyst in the electrically activated peroxymonosulfate (PMS) process, and the reaction kinetic constant reached 0.52 min⁻¹. The redox processes of Co²⁺ and Co³⁺ in Co(OH)₂ catalysts were considered to be the main pathways for PMS activation, in which ¹O₂ was the main active species. Furthermore, this strategy could also achieve excellent degradation efficiency for other organic pollutants. This study provides an effective and low-cost strategy with no secondary pollution for pollutant degradation.