新型反应型阻燃剂中间体DOPO的合成工艺改进

Improvement on the Synthetic Method of Novel Reactive Flame Retardant Intermediate DOPO

以三氯化磷和邻苯基苯酚在ZnCl2催化下合成新型阻燃剂中间体9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)。该文首先合成DOPO-2′-羟基联苯基-2-次磷酸(HPPA)混合物,然后在甲苯介质中将混合物脱水转化为高纯度DOPO。考察了催化剂种类、催化剂用量、物料配比、反应温度、反应时间等对收率的影响,并用正交实验进行了条件优化,优化条件为:物料配比n(OPP)n(PCl3)=1 1.7,反应温度220℃;反应时间3 h;ZnCl2的质量分数为0.1%。在该优化条件下DOPO收率96.2%。

9,10 - dihydro - 9 - oxa - 10 - phosphaphenanthrene - 10 - oxide （ DOPO）, a novel flame retardant intermediate, is synthesized from phosphorous trichloride and o - phenylphenol in present of ZnCl2. In this paper DOPO was prepared as a mixture of DOPO and 2＇ - hydroxydiphenyl - 2 - phosphinic acid （HPPA）. Thus the mixture was dehydrated in toluene solution to give a high purity of DOPO. Factors that influenced the product yield such as mol ratio of OPP： PCl3, the reaction temperature, the reaction time and the catalyst amount were discussed. The optimum reaction conditions were determined by orthogonal experiments as follows： mol ratio of OPP：PCl3 is 1：1.7;the reaction temperature is 220℃; the reaction time is 3 h; the catalyst amount is 0.1% （mass fraction）. In the optimal condition, the yield of DOPO is 96.2%.