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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。
The synthesis of phosphorus-nitrogen-bromine intumescent flame retardant bis- (2,4,6-tribromophenyl) phosphonate was carried out with phenol, bromine, hydrogen peroxide, phosphorus oxychloride and melamine as raw materials Two melamine salt. The first step to ethanol as solvent, phenol, bromine and hydrogen peroxide molar ratio of 1: 1.55: 1.78, the intermediate Ⅰ tribromophenol yield reached 98.2%; the second step benzene as a solvent, pyridine as acid Agent, the molar ratio of intermediate I to phosphorus oxychloride is 2.3:1, the yield of intermediate II is 89.1%. The third step is to use DMSO as solvent and the reaction temperature is 130 ℃. The yield of target product III reaches 95.8%. The intermediates and target products were characterized by FTIR and mass spectrometry.