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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。
The main raw material of wheat straw alkaloid lignin (WSAL) was modified by γ-aminopropyl triethoxysilane (KH550), and the N, Si lignin-based charring agent (CFA-WSAL) The synthesis process is optimized. At the same time, the structure and thermal stability of this lignin-based char were characterized by Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). The results showed that the target product CFA-WSAL was successfully obtained. The initial degradation temperature (T_ (5%)) in air was 269.9 ℃, which was significantly higher than that of WSAL (204.7 ℃). Under the premise of fixed lignin and solvent dosage of 200 mg and 5 ml respectively, the optimal preparation process of CFA-WSAL was as follows: the volume ratio of ethanol to deionized water was 0.5: 4.5, the reaction temperature was 80 ℃, the reaction time was 2 h, KH550 dosage of 0.488 g. In addition, the carbon residue ratios of CFA-WSAL at 500 ℃ and 800 ℃ were 31.5% and 21.3% respectively, which were significantly higher than 2.0% and 1.9% of WSAL. This shows that the charring agent has good thermal stability and charring ability, and has potential application in the field of intumescent flame retardant polymer materials.