丙基二甲氧基硅酸环膦酸酯的合成与应用  

Synthesis and Application of Propyl Dimethoxy Silicic Acid Monocyclic Phosphate

作　　者：贺婧 李果 王彦林 He Jing,Li Guo,Wang Yanlin(School of Chemistry Bioligy and Material Engineering,Suzhou University of Science and Technology,Suzhou 215000,Chin)

机构地区：[1]苏州科技大学化学生物与材料工程学院

出　　处：《塑料科技》2018年第4期122-125,共4页Plastics Science and Technology

摘　　要：以（正）丙基三甲氧基硅烷和笼状亚膦酸酯-4-乙基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷为原料,合成了一种磷、硅双重阻燃元素协同阻燃剂——丙基二甲氧基硅酸环膦酸酯（PDSMP）。探讨了反应温度、反应时间及物质量比等对产率的影响。结果表明,该合成反应的最佳反应条件为：n（笼状磷酸酯）：n（丙基三甲氧基硅烷）=1：1.2,在160℃保温反应17 h。该条件下,产物的产率可达到89.2%。通过红外光谱（FTIR）、核磁共振氢谱（1H-NMR）、热重/差热分析（TG-DTA）及极限氧指数（LOI）测试等对产物的结构及性能进行了表征。测试结果表明,产物具有较好的热稳定性,分解温度为220℃。将其应用于191不饱和树脂时,表现出了很好的阻燃效果。A phosphorus, silicon element dual synergistic flame retardant, propyl dimethoxy silicic acid monocyclic phosphate （PDSMP）, was synthesized by caged phosphite-4-ethyl-2,6,7- trioxa-l-phosphorus oxabicyclo [2.2.2] octane and n-propyltrimethoxysilane. The effects of reaction temperature, reaction time and molar ratio on the yield were investigated. The optimal conditions were selected as follows： n（caged phosphite-4-ethyl-2,6,7-trioxa-l-phosphorus oxabicyclo [2.2.2] octane）：n（n-propyltrimethoxysilane）=1：1.2, kept the reaction going at 160 ℃ for 17 h. And the yield could reach to 89.2%. The structure and flame retardance of the product were characterized by means of FTIR, 1H-NMR, TG-DTA analysis and LOI test. Results showed that the decomposition temperature of the product was 220℃, and the product also had a good thermal stability and high flame-retardant efficiency when applied to 191 unsaturated polyester.

关 键 词：(正)丙基三甲氧基硅烷 笼状磷酸酯 有机硅磷阻燃剂 含硅阻燃剂 

分 类 号：TQ314.248[化学工程—高聚物工业]