The　intensification　of　industrial　production　has　led　to　a　sharp　increase　in　the　discharge　of　toxic　organic　chemicals　and　wastewater　from　printing　and　dyeing　industry.　In　this　study,　flower-like　ZnO　modified　TiO2@Ti3C2Tx　composites　(ZnO/TiO2@Ti3C2Tx)　were　prepared　by　in-situ　oxidation　solvothermal　method　from　zinc　nitrate　hexahydrate　and　tetramethylammonium　hydroxide　intercalated　Ti3C2Tx.　During　the　solvothermal　processes,　sodium　hydroxide　acted　as　an　etchant　to　further　exfoliated　the　accordion-like　Ti3C2Tx　into　single　or　few-layer;　and　at　the　same　time,　TiO2　was　formed　in-situ　on　the　surface　of　Ti3C2Tx　with　simultaneous　deposition　of　flower-like　ZnO.　The　layer　structural　Ti3C2Tx　facilitates　the　loading　and　dispersion　of　ZnO　and　TiO2　on　its　surface.　After　the　in-situ　oxidation　by　solvothermal　method,　TiO2　was　evenly　distributed　on　the　surface　of　Ti3C2Tx,　adjusting　the　functional　groups　on　the　surface　of　the　ZnO/TiO2@Ti3C2Tx　composite,　and　improving　its　adsorption　performance.　ZnO/TiO2@Ti3C2Tx　can　be　used　as　an　efficient　adsorbent　for　malachite　green　with　a　high　maximum　adsorption　capacity　of　1232.7　mg　g−1,　which　is　higher　than　that　of　TiO2@Ti3C2Tx　(628.57　mg　g−1).　Moreover,　a　superhydrophilic　and　underwater　superoleophobic　ZnO/TiO2@Ti3C2Tx@PU　sponge　was　prepared　by　loading　ZnO/TiO2@Ti3C2Tx　onto　polyurethane　(PU)　sponge.　The　introduction　of　ZnO　enhances　the　surface　roughness　of　the　ZnO/TiO2@Ti3C2Tx@PU　sponge,　which　can　effectively　separate　six　oil-water　mixtures,　and　has　a　high　separation　flux　of　171784　L　m−2　h−1　and　separation　efficiency　of　99.6%　for　cyclohexane-water　mixture.　©　2024　Elsevier　Ltd