Nanoscale　zero-valent　iron　(nZVI)　is　more　valuable　in　environmental　restoration　than　other　materials.　Chemical　treatment　of　fly　ash　(CFA)　was　employed　as　a　support　material　to　disperse　iron　nickel　bimetal　nanoparticles　(CFA-nZVI/Ni)　to　remove　2,4-dichlorophenol　(2,4-DCP).　Batch　experiments　showed　that　2,4-DCP　was　completely　removed　by　CFA-nZVI/Ni,　and　an　optimal　loading　ratio　was　8:1.　The　degradation　of　2,4-DCP　by　CFA-nZVI/Ni　was　a　chemical　control　reaction　with　an　activation　energy　of　95.6　kJ　mol(-1)　and　followed　pseudo-first-order　kinetics.　The　addition　of　Cl-　increased　the　removal　rate　of　2,4-DCP　by　4%,　while　the　addition　of　CO32-　and　SO42-　decreased　the　removal　rate　of　2,4-DCP　by　32%　and　72.3%,　respectively.　The　removal　process　of　2,4-DCP　by　CFA-nZVI/Ni　included　adsorption　and　reduction.　The　2-CP　(7.1　mg/L)　and　4-CP　(11.6　mg/L)　could　be　converted　to　phenol　using　the　CFA-nZVI/Ni　system.　Cl　on　the　para-position　of　2,4-DCP　was　simpler　to　remove　than　on　the　ortho-position.　The　following　steps　were　taken　in　the　electrophilic　substitution　reaction　between　substituted　phenols　and　hydrogen　radicals:　2,4-DCP　＞　2-CP　＞　4-CP　＞　phenol.　This　research　provides　a　novel　concept　to　effectively　remove　2,4-DCP　and　mechanism　analysis.