Leakage of hazardous chemicals often causes significant casualties, enormous economic losses, and negative social benefits. Presently, fire rescue personnel lack efficient and eco-friendly disposal materials for hazardous chemical leakage accidents. In this study, chitosan (CS) aerogels with excellent flame-retardant performance were prepared via cross-linking by two phosphorus-containing vanillin-based compounds (DV and TV). The as-prepared chitosan aerogels were lightweight and porous. The introduction of DV and TV greatly enhanced the residual char yields of CS at 700 °C and the flame-retardant performance of chitosan aerogels. TCS-5.0 possessed the best flame-retardant performance, indicating that TV was more effective than DV in enhancing the flame-retardant performance of chitosan aerogels. The greatly improved flame-retardant properties could be attributed to TV effectively promoting the residual char formation of chitosan aerogels and reducing the formation of combustible gas phase products. To improve the hydrophobicity of chitosan aerogels, TCS-5.0 was treated with solution immersion to load siloxane molecules on its surface. The water contact angle of HTCS-5.0 was 136.1°. HTCS-5.0 had a high oil absorption multiplicity, absorbing up to 31 times its own weight of chloroform. HTCS-5.0 could continuously absorb organic solvents on the water surface with the assistance of a vacuum pump, indicating that HTCS-5.0 could be used for the clean-up of hazardous chemical leakage accidents.
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