The　heterogeneous　electro-Fenton　process　is　an　effective　technology　to　remove　organic　pollutants.　However,　developing　efficient　heterogeneous　electro-Fenton　catalysts　remains　challenging.　In　this　paper,　an　iron-cerium　layered　double　hydroxide　(Fe-Ce-LDH)　was　successfully　loaded　via　a　solvothermal　method　onto　the　defect　sites　of　the　molecular　sieve　13X　to　form　a　novel　heterogeneous　catalyst　(Fe-Ce-LDH/13X).　The　catalytic　performance　of　Fe-Ce-LDH/13X　was　evaluated　in　the　heterogeneous　electro-Fenton　(EF)　degradation　of　diuron.　Compared　with　a　traditional　powder　catalyst,　this　catalyst　was　easier　to　recycle　and　exhibited　good　stability.　The　layered　structure　of　the　catalyst　provided　more　active　sites.　Doping　with　Ce　greatly　improved　the　catalytic　performance　of　the　catalyst,　which　was　caused　by　the　synergistic　effect　of　Ce　and　Fe.　At　a　molar　Fe　to　Ce　ratio　of　7:3,　diuron　could　be　completely　degraded　within　60　min.　According　to　the　catalytic　mechanism,　the　hydroxyl　radical　center　dot　OH　is　the　main　reactive　species.　Possible　degradation　pathways　in　the　heterogeneous　EF　process　were　proposed　based　on　the　intermediates　identified　in　the　degradation　of　diuron.　Toxicity　analysis　indicated　that　the　heterogeneous　EF　process　could　not　only　degrade　diuron　but　also　reduce　toxicity.　This　work　presents　a　novel　preparation　method　of　a　composite　catalyst　with　excellent　catalytic　performance　in　an　EF　system,　which　supports　the　development　of　efficient　heterogeneous　EF　catalysts.