Micro-nano structure was constructed on the polyester fiber’s surface through in-situ polymerization by trialkoxysilane containing dicyano and zinc oxide, endowing the fabric with SO2 adsorption performance. The treating conditions, including the selection of solvent, water content in the solvent, and catalysts were investigated extensively. Therefore, three distinct first-order rough structures were fabricated, namely, triethylamine catalyzing coating (TEA@PET), triethylenediamine catalyzing coating (DTEA@PET), and tetraethylenepentamine catalyzing coating (TEPA@PET). Then, based on the primary structure DTEA@PET, the nano-zinc oxide was employed for secondary treatment, and the micro-nano structure (ZnO/CN@PET) with zinc oxide particles attached to the surface of silicone microspheres was fabricated. Combined with the surface’s chemical composition assessment and morphology investigation, it was demonstrated that the micro-nano surface consisted of inorganic nano-zinc oxide on the organopolysiloxane micron particles’ surface. When the roughness of DTEA@PET was 199 nm, ZnO/CN@PET increased to 229 nm. The SO2 adsorption capacity of DTEA@PET was 28.2 mL/g, while that of ZnO/CN@PET reached 38.6 mL/g, proving that the composite ZnO nanoparticles on micron roughened surface could offer remarkable SO2 adsorption capacity.
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