含硅三笼状磷酸酯阻燃剂的合成及结构表征

Synthesis and structure characterization of silicon-containing caged phosphate flame retardant

以乙烯基三氯硅烷和1-氧代-4-羟甲基-2,6,7-三氧杂-1-磷杂双环[2,2,2]辛烷(PEPA)为原料,合成含硅三笼状磷酸酯阻燃剂,即三(1-氧代-2,6,7-三氧杂-1-磷杂双环[2,2,2]辛烷-4-亚甲氧基)乙烯基硅烷(EPSi),通过核磁共振光谱、红外光谱、热失重分析等手段对其进行结构表征和热性能分析。结果表明:合成的产物为目标产物EPSi;EPSi在空气和氮气中热分解5%的温度分别为309℃和349℃,700℃残余质量率分别为36.9%和54.5%,具有良好的热稳定性和成炭率。

A novel silicon-containing caged phosphate flame retardant, tri （ 1 -oxo-2,6,7-trioxa- 1 -phosphabicyclo [ 2,2,2 ] octaneethenylsilane （EPSi）, was synthesized by using vinyltrichlorosilane and 1-oxo-4-hydroxymethyl-2,6,7-trioxa-l-phosphabicyclo[ 2,2,2 ] octane （PEPA） as raw material. The structure characterization and thermal property analysis were conducted by nuclearmagnetic resonance spectroscopy, infrared spectroscopy and thermogravimetric analysis. The results showed that the synthesizedproduct was the target product EPSi; and the decomposition temperatures of EPSi at 5% weight loss were 309 ℃ and 349 ℃,and the mass residue was 36.9% and 54.5% at 700 ℃ under air and nitrogen atmosphere, respectively, which proved that theflame retardant possessed favorable thermal stability and char yield.