“一锅”法合成高纯度反应型含磷阻燃剂DOPO

Synthesis of High-purity Reactive Flame Retardent DOPO by One-pot Method

采用“一锅”法合成了高纯度反应型阻燃剂9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)。用DSC、FTIR、气相色谱-质谱联用以及TGA分别对产物的熔点、结构、纯度和热稳定性进行了表征。结果显示:优化工艺后得到的DOPO熔点为106℃左右,纯度可达到92%～96.95%,收率75.4%,产物热分解温度为213℃。对DOPO的合成工艺进行了探讨,考察了催化剂的加入量、PCl3/OPP物质的量比、反应温度、反应时间等对产物收率的影响,较佳反应条件为:PCl3/OPP物质的量比1.5∶1,反应温度160℃,反应时间5￣6h。

By＂in one-pot＂ technique, highpurity reactive flame retardant 9,10-dihydm-9-oxa-10-phos-phaphenanthrene -10-oxide （DOPO） was synthesized. The melting point, structure, purity and thermal degradation behavior of the product were investigated by DSC,FTIR, GC-MS and TGA .The results indicated that after optimum of synthesis technique, the melting point of the product is about 106 ℃, the purity is 92%- 96.95%, the yield is 75.4%, the decomposition temperature of the product is 213 ℃. Synthesis technical process of DOPO such as the effects of the catalysts amount, the mole ratio of PCI3 and OPP, reaction temperature, reaction time on the yield of the product were also discussed. The optimum reaction condition are： PCI3/OPP（mass）： 1.5：1, reaction temperature： 160℃, reaction time：5-6 h.