The　improper　disposal　of　waste　high　purity　acetonitrile　(HPA)　not　only　causes　environmental　degradation　but　also　poses　significant　risks　to　human　health.　One　of　the　major　challenges　in　the　recycling　and　reuse　of　waste　HPA　is　the　removal　of　trace　metal　ions.　In　this　study,　we　successfully　fabricated　a　chitin/ZIF-67　composite　hydrogel　(CZ-n)　by　one　pot　in　situ　synthesis　method　for　the　purification　and　recovery　of　waste　HPA　for　the　first　time.　ZIF67　was　embedded　into　chitin　through　hydrogen　bonding　and　coordination　and　provided　more　active　adsorption　sites,　which　resulted　in　CZ-3　with　higher　adsorption　capacity　than　CZ-0.　The　maximum　adsorption　capacities　of　CZ-3　for　Zn2+　and　Ag+,　as　determined　by　fitting　the　Langmuir　model,　were　85.46　mg　&　sdot;g-1　and　91.26　mg　&　sdot;g-1,　respectively.　CZ-3　was　able　to　effectively　decrease　the　metal　ion　(Zn2+　and　Ag+)　concentration　to　below　10　ppb　within　24　h　through　a　monolayer　adsorption　process　using　chelation.　Furthermore,　the　adsorption　capacity　remained　satisfactory　even　in　the　presence　of　an　equivalent　concentration　of　NaCl,　and　CZ-3　exhibited　remarkable　reusability,　with　a　removal　rate　exceeding　80　%　after　five　cycles.　Additionally,　it　also　displayed　notable　biodegradability,　with　complete　degradation　observed　within　60　days.　These　results　indicated　that　CZ-3　could　be　a　potential　absorbent　in　the　purification　and　recovery　of　waste　HPA.