Removal　of　hetero　ions　from　the　hydrogen　peroxide　solution　is　a　crucial　step　in　purifying　electronic-grade　H2O2.　Conventional　adsorption　materials　are　challenged　to　meet　the　need　for　the　simultaneous　adsorption　of　both　anions　and　cations　in　solvents.　UiO-66　(Zr)　modified　by　acetic　acid　and　amino　group　for　simultaneous　adsorption　of　phosphate　and　Pb2+　in　H2O2　purification　was　fabricated　in　this　work.　The　as-prepared　defective　UiO-66-NH2　(Zr)　demonstrated　a　significant　increase　in　specific　surface　area　and　porosity,　along　with　more　exposed　sites　for　phosphate　and　Pb2+　adsorption.　The　adsorption　capacity　of　De-UiO-66-NH2　for　phosphate　and　Pb2+　in　H2O2　solution　was　52.28　mg　g-1　and　35.4　mg　g-1,　which　is　1.19　times　and　1.88　times　that　of　unmodified　UiO-66　(Zr),　respectively.　The　trace　simultaneous　adsorption　with　both　100　ppb　phosphate　and　Pb2+　showed　removal　rates　of　94.0%　and　88.7%,　respectively,　confirming　the　practicality　of　MOF　materials　in　the　purification　of　electronic　chemicals.　This　work　highlights　the　potential　of　Zr-based　MOFs　as　anionic　and　cationic　simultaneous　adsorbents　for　highly　efficient　purification　of　electronic-grade　solvents.　©　2024　American　Chemical　Society