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新型无卤硅-氮成炭剂的合成及其热稳定性
引用本文:王文涛,熊宽宽,赵斌,赵培华,刘亚青. 新型无卤硅-氮成炭剂的合成及其热稳定性[J]. 合成化学, 2016, 24(1): 26-29. DOI: 10.15952/j.cnki.cjsc.1005-1511.2016.01.15320
作者姓名:王文涛  熊宽宽  赵斌  赵培华  刘亚青
作者单位:中北大学 材料科学与工程学院 山西省高分子复合材料工程技术研究中心,山西 太原 030051
基金项目:山西省科技攻关项目(20120321016-02),山西省研究生教育创新项目(2015SY54)
摘    要: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%。

关 键 词:无卤硅-氮成炭剂  合成  热稳定性  
收稿时间:2015-09-15

Synthesis and Thermal Stability of A Novel Halogen-free Si-N Charring Agent
WANG Wen-tao,XIONG Kuan-kuan,ZHAO Bin,ZHAO Pei-hua,LIU Ya-qing. Synthesis and Thermal Stability of A Novel Halogen-free Si-N Charring Agent[J]. Chinese Journal of Synthetic Chemistry, 2016, 24(1): 26-29. DOI: 10.15952/j.cnki.cjsc.1005-1511.2016.01.15320
Authors:WANG Wen-tao  XIONG Kuan-kuan  ZHAO Bin  ZHAO Pei-hua  LIU Ya-qing
Affiliation:Research Center for Engineering Technology of Polymeric Composites of Shanxi Province, School of Materials Science and Engineering, North University of China, Taiyuan 030051, China
Abstract: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 ℃.
Keywords:halogen-free silicon-nitrogen charring agent  synthesis  thermal stability
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