通过壳聚糖、香草醛和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)反应制备一种壳聚糖基含DOPO阻燃剂CS-L。采用红外光谱、紫外-可见光谱、X射线光电子能谱和热失重表征CS-L结构,并通过垂直燃烧、锥形量热和动态热机械分析研究CS-L对环氧树脂阻燃性能和玻璃化转变温度(Tg)的影响。结果表明:制备的CS-L为预期结构。CS-L能抑制环氧树脂的滴落、燃烧以及烟的产生,由于其在气相和凝聚相中发挥阻燃作用。在燃烧过程中,15% CS-L使环氧树脂的热释放速率峰值、平均热释放速率、总热释放、平均质量损失率、总烟释放、总烟产量、平均比消光面积分别降低了243.2kW/m2、58.8kW/m2、18.4MJ/m2、0.022g/s、698m2/m2、6.17m2、120.6m2/kg,使其残留量提高8.76%。CS-L对环氧树脂的Tg影响较小,含20% CS-L环氧树脂的Tg高达157.0℃。
A chitosan-based flame retardant with DOPO,named as CS-L,was prepared from chitosan,vanillin and DOPO (9,10-dihydro-9-oxa-10-phosphaphenantrtene-10-oxide).Its structure was characterized by FT-IR,UV-Vis,XPS and thermogravimetry.The effect of CS-L on the flame retardant property and glass transition temperature (Tg) of epoxy resin was studied.The results showed that the prepared CS-L had the expected structure.CS-L was able to inhibit dripping,burning and smoke generation of epoxy resin(EP) because it played the flame-retardant role in gas phase and condensed phase.The loading of 15wt% CS-L made the peak heat release rate,mean heat release rate,total heat release,mean mass loss rate,total smoke release,total smoke production and mean specific extinction area of EP reduced by 243.2kW/m2,58.8kW/m2,18.4MJ/m2,0.022g/s,698m2/m2,6.17m2,120.6m2/kg,respectively,and increased its residual amount by 8.76wt%.CS-L had little effect on the Tg of EP,and the Tg of EP with 20wt% CS-L was up to 157.0℃.
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基金资助
岭南师范学院燕岭优秀青年教师培养计划(YL20200213);广东省自然科学基金资助项目(2021A1515011398)
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