一种含磷-氮-溴膨胀型阻燃剂的合成  

Synthesis of A Phosphorus-Nitrogen-Bromine Containing Intumescent Flame Retardant

作　　者：肖碧鹏[1] 章颖[1] 樊继亮[1] 朱宗民[1] 朱杰[1] 黄齐茂[1] 潘志权[1] 

机构地区：[1]武汉工程大学绿色化工过程省部共建教育部重点实验室国家磷资源开发利用工程技术研究中心,湖北武汉430073

出　　处：《化学与生物工程》2013年第6期56-58,86,共4页Chemistry & Bioengineering

摘　　要：以苯酚、溴素、双氧水、三氯氧磷、三聚氰胺等为原料,经三步合成含磷-氮-溴膨胀型阻燃剂双-(2,4,6-三溴苯基)磷酸二酯二三聚氰胺盐。第一步以乙醇为溶剂,苯酚、溴素与双氧水的摩尔比为1∶1.55∶1.78时,中间体Ⅰ三溴苯酚的收率达到98.2%;第二步以苯为溶剂、吡啶为缚酸剂,中间体Ⅰ与三氯氧磷的摩尔比为2.3∶1时,中间体Ⅱ的收率达到89.1%;第三步以DMSO为溶剂,反应温度为130℃,目标产物Ⅲ的收率达到95.8%。采用红外光谱和质谱对中间体及目标产物进行了结构表征。Phosphorus-nitrogen-bromine containing intumescent flame retardant bis（2,4,6-tribromophenyl） phosphoric diraelamine salt was synthesized from phenol,bromine,hydrogen peroxide, phosphorous oxychloride and melamine through the three-step method. The suitable synthetic conditions were obtained as follows：in the step one,the molar ratio 1：1.55 ：1.78 of phenol,bromine and hydrogen peroxide was used with ethanol as solvent,the yield of intermediate I reached 98. 2%, in the step two, the molar ratio of intermediate Ⅰ to phos- phorous oxychloride was 2.3：1 using phenol as solvent,pyridine as HC1 acceptor,the yield of intermediate Ⅱ reached 89.1% ,in the step three,DMSO was selected as solvent,the reaction temperature was 130℃ ,and the yield of target product Ⅲ reached 95.8%. The structures of the intermediates and the target product were con- firmed by FTIR and MS.

关 键 词：膨胀型阻燃剂 合成 双-(2 4 6-三溴苯基)磷酸二酯二三聚氰胺盐 

分 类 号：TQ314.248[化学工程—高聚物工业]