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With oil spill accidents and oil industrial wastewater increasing, oil/water separation has attracted much attention in recent years. Herein, we report the fabrication of superhydrophilic and underwater superoleophobic thiol-ene/silica hybrid decorated fabrics for oil/water separation via vapor-liquid interfacial reaction. It is based on sol-gel reaction of tetraethyl orthosilicate (TEOS) to generate silica and thiol-ene reaction between poly(ethylene glycol) dimethacrylate (PEGDMA) and trimethylolpropane tris(3-mercaptopropionate) (TTMP) to form crosslinked hydrophilic polymer on polyester fabric under the catalysis of butylamine/ammonia vapor. The chemical structure of the surfaces on thiol-ene/silica hybrid decorated fabric was confirmed by FTIR and XPS, and obvious micro-nano morphology and roughness were observed with SEM and AFM. The water contact angle of the fabric attained 0° in 0.36 s, and the underwater oil contact angle reached up to 160°. Importantly, the fabric exhibited high separation efficiency at 99.5%, fast water flux above 71600 Lm −2 h −1 and excellent recyclability in oil/water separation. Our findings open a new strategy to fabricate organic-inorganic hybrid superhydrophobic and underwater superoleophobic materials for oil/water separation. [ABSTRACT FROM AUTHOR]