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机构地区:[1]浙江省化工研究院有限公司,浙江杭州310023
出 处:《浙江化工》2011年第11期18-20,17,共4页Zhejiang Chemical Industry
摘 要:以邻苯基苯酚(OPP)与三氯化磷(PCl3)为原料,以无水ZnCl2为催化剂,采用酯化、酰基化、水解反应连续进行的方法制得中间体HPPA,HPPA再经分子内脱水成环反应制得DOPO。通过核磁共振氢谱对其结构进行了表征。讨论了投料比、反应温度、水解方式等因素对DOPO产率的影响。结果表明,当PCl3与OPP摩尔比为1.2,反应温度为180℃,在甲苯中水解,DOPO的产率达90.1%。A novel phosphorous-containing flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene10-oxide(DOPO)was synthesized by using o-phenyl phenol and phosphorous trichloride as starting materials and zinc chloride as catalyst through esterification, acylation, hydrolysis and intramolecular dehydration. The structure of DOPO was characterized by ^1H-NMR spectroscopies. Factors that influenced the product yield such as charge ratio, reaction temperature and hydrolysis method were discussed. The results show that the yield of DOPO is 90.1% when the reaction conditions were determined as follows:mol ratio of OPP:PCIν3 is 1.2,the reaction temPerature is 180 °C and hydrolysis in toluene solution.
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