含磷阻燃剂DOPO的合成及在环氧树脂中的应用-有机化学专业论文.docxVIP

I I 摘 要 9,10 一二氢-9-氧杂-10-磷杂菲一 10-氧化物(DOPO)是新型反应型阻燃剂 中间体，由它合成的阻燃剂有优良的热稳定性和阻燃性，可用于电子、合成纤维、 半导体封装材料的阻燃。 本论文以三氯化磷与邻苯基苯酚为原料合成了含 9,10 一二氢-9 一氧杂-10- 磷杂菲-10 一氧化物和 2′－羟基联苯基－2－次磷酸的混合物，后在甲苯体系中 转化为 DOPO。考察了催化剂种类、物料配比、催化剂用量、反应温度、反应时 间等因素对收率的影响，并用正交实验优化了工艺条件。最佳反应条件为：无水 三氯化铝为催化剂，反应时间 8h，反应温度 200℃，n（PCl3）﹥n（OPP）=1.3， 并在 DOPO 上引入叔丁基，改进了 DOPO 在高分子材料中的相溶性。 以 DOPO 及其衍生物和邻甲苯酚环氧树脂反应，制成反应型环氧树脂。对 其进行阻燃性能测试。采用氧指数(L0I)及垂直燃烧法从阻燃性能、热性能及阻 燃耐久性等方面对含磷本质环氧树脂、添加型环氧树脂进行说明。研究表明， DOPO 反应型环氧树脂具有阻燃效率高，阻燃性能持久的优势，在 DOPO 含量 达到 10%时，残碳率最高，阻燃性最好，氧指数达到 29.4。 关键词：阻燃剂中间体;DOPO;环氧树脂;叔丁基氯;阻燃性能测试 II II Abstract 9 ， 10 － dihydro-9-oxa-10-phosphaphenanthren-10-oxide(DOPO) is a novel reactively flame-retardant intermediate. Flame-retardants which are synthesized by DOPO have excellent thermal-stabilities and flame-retardancy, can be used to the flame retardancy of electronical facilities, synthetic fiber and semi-conductor encapsulation material. This work synthesized a mixture contain 9 ， 10 － dihydro-9-oxa-10- phos- phaphenanthren-10-oxide through phosphorus trichloride and o-phenyl phenol, then transformed to DOPO in toluene system. Investigate the factors that infect the productive rate such as catalyzer species, material ratio, the dosage of catalyzer, reaction temperature and time, the best conditions is :catalyzer is aluminum trichloride ,reaction time 8h,reaction temperature 200 ℃ ,the ratio of n(PCl3):n(OPP)=1.3,and optimized the process through orthogonal experiment. Tert-Butyl group was brought into DOPO, improved the solubility in polymer materials. DOPO and its derivatives react with o-cresol formaldehyde novolac epoxy resin, produce the reactive epoxy resin. Test the performance of flame-retardancy. The LOI(Limited Oxygen Index) value and UL-94 experiment can explain the difference of Flame retardent o-cresol formaldehyde novolac epoxy resin and Flame resistant o-cresol formaldehyde novolac epoxy resin in flame retardancy、flame wearing time and ca