Developing　highly　efficient,　stable,　recyclable,　and　application　value　heterogeneous　catalysts　in　advanced　oxidation　processes　has　essential　application　value　in　the　degradation　of　refractory　pollutants.　In　this　paper,　the　CoNi　alloy　anchored　onto　N-doped　porous　carbon　(CoNi-600@NC)　catalyst　was　prepared　using　bimetallic　doped　metal-organic　frameworks　as　precursors.　The　magnetic　CoNi-600@NC　can　activate　peroxymonosulfate　(PMS)　to　degrade　sulfamethoxazole　(SMX).　Therefore,　SMX　can　be　removed　100%　within　25　min.　CoNi-600@NC/PMS　has　a　broad　pH　(3–9)　application　range,　good　applicability,　and　repeatability.　Radical　quenching,　quantitative　and　electrochemical　experiments　proved　that　the　degradation　of　SMX　was　dominated　by　free　radical　(Superoxide　anions)　and　non-free　radical　pathways　(surface-bound　radicals).　Mechanistic　analysis　showed　that　the　interaction　between　Co-Nx/pyridine　N-sites　and　graphitized　carbon　with　PMS　induced　the　formation　of　surface-bound　active　species.　Moreover,　CoNi　nanoparticles　promoted　the　redox　cycle　of　metals.　The　synergistic　catalytic　mechanisms　between　the　CoNi　alloy　and　the　abundant　functional　groups　gave　CoNi-600@NC　excellent　catalytic　properties　and　applicability.　Using　density　functional　theory　predicted　the　reaction　sites　of　SMX　and　proposed　four　degradation　pathways.　The　toxicity　of　intermediates　was　comprehensively　evaluated.　In　addition,　a　CoNi-600@NC　continuous　flow　reactor　was　constructed　with　a　daily　treatment　capacity　of　45　L　and　100%　SMX　removal.　This　study　expands　the　application　of　persulfate　advanced　oxidation　technology　by　synthesizing　recyclable　magnetic　catalysts　and　provides　new　synergistic　degradation　mechanisms　for　removing　refractory　organics.　©　2022　Elsevier　Ltd