新型无卤硅-氮成炭剂的合成及其热稳定性

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

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%。

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 by1 H 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 ℃.