4,4'-联苯基双二氯化膦是制备耐高温抗氧剂四(2,4-二叔丁基苯基-4,4'-联苯基)双膦酸酯的主要原料。本文以联苯和三氯化磷为原料,在无水三氯化铝催化作用下,经减压蒸馏、解络和抽滤等工艺,得到4,4'-联苯基双二氯化膦溶液。实验表明：使用氯仿作为溶剂且联苯、三氯化磷和无水三氯化铝的摩尔比为1：4：2.7时,4,4'-联苯基双二氯化膦的收率达到最高值73.6%。另外,4,4'-联苯基双二氯化膦热稳定性不足,因此以其水解产物4,4'-联苯基二亚磷酸来表征。
4,4’-biphenyl-bis-dichlorophosphine is the main material of preparing the heat-resistant antioxidant tetrakis-(2,4-di-butylphenyl)-4,4’-biphenylene diphosphonite. The 4,4’-biphenyl-bis-dichlorophosphine solvent was synthesized using biphenyl and phosphorus trichloride as raw materials,and anhydrous aluminum trichloride as catalyst,by means of vacuum distillation、decomplexation and air pump filtration. The experiment showed that the yield of 4,4’-biphenyl-bis-dichlorophosphine could reach 73.6% when using chloroform as solvent and n( biphen-yl):n( phosphorus trichloride):n( anhydrous aluminum trichloride) was 1:4:2.7. In addition,due to the heat in-stability of 4,4’-biphenyl-bis-dichlorophosphine,it was characterized by its hydrolysate 4,4’-biphenyl-bis- diphos-phorous acid.
参考文献
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| [2] | 谢文杰,王鉴,曾群,曲云龙,杨年兴.二氯化苯基膦的合成进展[J].精细化工中间体,2005(06):19-21,31. |
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