一种含N、Si木质素基成炭剂的合成及其表征  

Synthesis and Characterization of A Lignin-based Charring Agent Containing Nitrogen and Silicon

作　　者：路焕青 宋艳[1] 王中平[1] 刘代垚 明姚江 周晶晶[1] 

机构地区：[1]常州大学材料科学与工程学院,江苏常州213164

出　　处：《塑料科技》2016年第7期90-94,共5页Plastics Science and Technology

基　　金：江苏省大学生创新创业训练计划立项项目(201510292028Z)

摘　　要：以麦草碱木质素(WSAL)为主要原料,利用γ-氨丙基三乙氧基硅烷(KH550)对其进行改性,制得了含N、Si木质素基成炭剂(CFA-WSAL),并对其合成工艺进行了优化。同时,借助傅里叶变换红外光谱仪(FTIR)和热重分析仪(TGA)分别对该木质素基成炭剂的结构与热稳定性能进行了表征。结果表明:成功获得了目标产物CFA-WSAL,其在空气中的起始降解温度(T_(5%))为269.9℃,明显高于WSAL(204.7℃)。在固定木质素及溶剂用量分别为200 mg和5 ml的前提下,CFA-WSAL的最佳制备工艺为:乙醇和去离子水的体积比为0.5:4.5,反应温度为80℃,反应时间为2 h,KH550用量为0.488 g。此外,CFA-WSAL在500℃及800℃下的残炭率分别可达到31.5%和21.3%,明显高于WSAL的2.0%和1.9%。这表明该成炭剂具有良好的热稳定性及成炭能力,在膨胀型阻燃高分子材料领域具有潜在的应用前景。A lignin-based charring agent containing nitrogen and silicon（CFA-WSAL） was synthesized through the modification of wheat straw alkali lignin（WSAL） by γ-amino propyltriethoxysilane（KH550）, and the synthesis process was optimized. The structure and thermal stability of CFA-WSAL were then respectively characterized by Fourier infrared transform spectrometer（FTIR） and thermogravic analyzer（TGA）. The results showed that the target product CFA-WSAL was successfully prepared, and its initial degradation temperature（T_（5%）） was 269.9℃ under air atmosphere, obviously higher than that of WSAL（204.7℃）. Moreover, when the amounts of WSAL and solvent were fixed at 200 mg and 5 ml, the optimum reaction conditions were as followed： volume ratio of ethanol and deionized water 0.5：4.5, reaction temperature 80℃, reaction time 2 h, and dosage of KH550 0.488 g. Furthermore, the residuals of CFA-WSAL reached 31.5% and 21.3% when the temperatures were 500℃ and 800℃ respectively, significantly higher than those of WSAL（2.0% and 1.9%）, which suggested CFA-WSAL had a higher thermal stability and good charring ability. Therefore, the charring agent has a potential application in intumescent flame retardant polymer materials.

关 键 词：麦草碱木质素 Γ-氨丙基三乙氧基硅烷 改性 含N、Si成炭剂 

分 类 号：TQ314.248[化学工程—高聚物工业]