In　this　study,　a　bimetallic　composite　catalyst　(Co-Fe@C)　was　fabricated　with　calcination　at　high　temperature　(800　degrees　C)　by　using　Co-MIL-101　(Fe)　as　the　precursor.　The　characterization　results　showed　that　the　resulted　Co-Fe@C　composite　mainly　consisted　of　carbon,　FeCo　alloys,　Fe3O4,　Co3O4　and　FeO,　and　owned　evident　magnetism.　In　addition,　the　Co-Fe@C　was　employed　to　activate　the　peroxydisulfate　(PDS)　to　degrade　a　representative　organic　pollutant　(p-arsanilic　acid,　p-ASA)　and　the　main　factors　were　optimized,　which　involved　0.2　g　L-1　of　catalyst　dosage,　1.0　g　L-1　of　PDS　dosage　and　5.0　of　initial　pH.　Under　the　optimal　condition,　Co-Fe@C/PDS　system　could　completely　degrade　p-ASA　(20　mg　L-1)　in　5　min.　In　the　Co-Fe@C/PDS　system,　SO4-center　dot,　Fe(IV)　and　center　dot　OH　were　the　main　species　during　p-ASA　degradation.　Under　the　attack　of　these　species,　p-ASA　was　first　decomposed　into　phenols　and　then　transformed　into　the　organics　acids　and　finally　mineralized　into　CO2　and　H2O　through　a　series　of　reactions　like　hydroxylation,　dearsenification,　deamination　and　benzene　ring　opening.　Importantly,　most　of　the　released　inorganic　arsenic　species　(93.40%)　could　be　efficiently　adsorbed　by　the　catalyst.