Large　amounts　of　heavy-metal-containing　coal　fly　ash　can　cause　serious　environmental　hazards.　The　separation　and　extraction　of　titanium,　iron,　and　alumina　from　coal　fly　ash　can　provide　economic　and　environmental　benefits.　This　work　presents　an　electrolysis-hydrolysis　method　to　alter　the　precipitation　order　of　iron　and　alumina　by　changing　the　ion　charge　sequence　to　extract　iron　and　alumina　in　an　orderly　manner　while　recovering　the　waste　heat　to　polymerize　the　precipitated　titanium.　The　separation　and　extraction　of　titanium,　iron,　and　alumina　in　one　spot　can　shorten　the　process　and　make　full　use　of　the　electric　energy.　Under　optimal　conditions,　the　efficiencies　of　iron,　titanium,　and　alumina　were　97.6%,　93.1%　and　88.5%,　respectively.　The　iron　product　had　a　composition　of　95.8%　Fe2O3,　0.5%　Al2O3,　0.3%　CaO,　0.1%　SO3,　and　0.4%　TiO2.　The　alumina　product　had　a　composition　of　88.7%　Al2O3,　0.1%　Fe2O3,　0.2%　CaO,　9.1%　SO3　and　0.2%　TiO2.　The　titanium　product　had　a　composition　of　63.78%　TiO2,　3.11%　Al2O3,　8.15%　Fe2O3,　0.28%　CaO,　4.12%　SiO2,　and　9.6%　SO3.　Moreover,　in　the　entire　electrolysis　process,　no　expensive　membranes　or　chemical　additives　were　required,　avoiding　the　limitations　of　membranes　and　high　costs.　Fe,　Al(OH)3,　Ti(OH)4,　O2,　and　H2　were　generated　during　the　electrolysis-hydrolysis　process;　therefore,　no　harmful　substances　were　produced.　Thus,　this　study　proposes　an　alternative　electrolysis-hydrolysis　process　for　the　simultaneous　separation　and　extraction　of　titanium,　alumina,　and　iron　from　coal　fly　ash　leachate　in　one　spot.　©　2022　Elsevier　B.V.