新型无卤硅-氮成炭剂的合成及其热稳定性

以三聚氯氰和γ-氨丙基三乙氧基硅烷为原料，经取代反应制得2-氯-4，6-二(3-三乙氧基硅烷-1-丙氨基)-1，3，5-三嗪(3)； 3与二乙烯三胺(4)反应合成了一种新型的无卤高含硅量的成炭剂(5)，其结构和性能经¹H NMR， FT-IR和TGA表征。考察了物料比、缚酸剂、反应时间、反应溶剂和反应温度对5收率的影响。实验结果表明:最佳反应条件为：甲苯为溶剂，三乙胺为缚酸剂， n(3): n(4)= 3.3 : 1，于100 ℃反应11 h，收率62.7%; 5的初始分解温度为197 ℃， 700 ℃时残炭为36.7%。

Synthesis and Thermal Stability of A Novel Halogen-free Si-N Charring Agent

2-Chloro-4,6-di(3-triethoxysiloxy-1-aminoproply)-1,3,5-triazine(3) was prepared by substitution reaction of cyanuric chloride with γ-aminopropyl triethoxysilane. A novel halogen-free and high silicon content of charring agent(5) was synthesized by reaction of 3 with diethylenetriamine(4). The structure and thermal properties were characterized by ¹H NMR, FT-IR and TGA. Effects of molar ratio of raw materials, acid-blinding agent, reaction time, reaction solvent and reaction temperature on the yield of 5 were investigated. The optimum reaction conditions were as followed: toluene was solvent, triethylamine was acid-binding agent, and n(3) : n(4) was 3.3:1, at 100 ℃ for 11 h, the yield was 62.7%. The initial decomposition temperature of 5 was 197 ℃, and the char yield was about 36.7% at 700 ℃.