Reduced　graphene　oxide　supported　Fe/Ni　nanocomposites　were　prepared　for　the　rapid　and　effective　adsorption　and　dechlorination　of　2,4-dichlorophenol　(2,4-DCP)　by　using　liquid　phase　reduction　method.　The　morphological　characterization　showed　that　the　spherical　Fe/Ni　bimetallic　nanoparticles　with　the　size　of　80~150nm　were　successfully　inserted　into　the　graphene　sheets　and　mainly　distributed　at　the　edges　and　folds　of　the　graphene　sheets.　The　agglomeration　of　Fe/Ni　nanoparticles　decreased　significantly.　XRD　patterns　and　FTIR　analysis　showed　nZVI　nanoparticles　were　successfully　embedded　into　graphene　through　Fe-O　bond,　Fe/Ni　bimetallic　nanoparticles　had　poor　crystallinity　and　amorphous　iron　oxide　which　covered　the　outer　layer　of　nanoparticles.　The　effects　of　different　preparation　conditions　such　as　carbon　iron　ratio,　nickel　loading　and　reduction　degree　of　graphene　oxide　on　the　removal　of　2,4-DCP　were　discussed.　The　optimum　preparation　conditions　of　the　Fe/Ni@rGO　composites　are　as　follows:　the　mass　ratio　of　graphene　to　Fe　is　1:2,　the　Ni　loading　is　5%,　and　the　molar　ratio　of　NaBH4to　Fe2+　is　5:1.　The　adsorption　and　dechlorination　perfermance　of　2,4-DCP　by　nZVI,　Fe/Ni,　Fe@rGO　composites　and　Fe/Ni@rGO　composites　were　compared　and　analyzed.　The　results　showed　that　the　removal　efficiency　of　2,4-DCP　by　five　materials　followed　the　sequence:　Fe/Ni@rGOcomposites＞Fe/Ni＞rGO＞Fe@rGOcomposites＞nZVI.　However,　the　cycle　test　and　storage　stability　test　showed:　compared　with　Fe/Ni　bimetallic,　Fe/Ni@rGO　composites　had　stable　reactivity　activity　and　high　reruse　value.　The　results　demonstrated　the　removal　mechanism　of　2,4-DCP　by　Fe/Ni@rGO　composites　was　the　synergistic　effect　of　adsorption　and　dechlorination.　©　2023　Chinese　Society　for　Environmental　Sciences.　All　rights　reserved.