苯基亚膦酸二甲酯的合成  

Synthesis of Dimethyl Phenyl Phosphonite

作　　者：赵辉爽[1] 

机构地区：[1]常州工程职业技术学院,江苏常州213164

出　　处：《化工文摘》2009年第2期43-44,47,共3页

摘　　要：文章以苯、三氯化磷、甲醇为主要原料,经两步反应合成了苯基亚膦酸二甲酯,并通过正交实验找到了最优的合成条件。第一步反应:苯和三氯化磷在三氯化铝催化剂作用下生成苯基二氯化膦,n(C6H6):n(AlCl3):n(PCl3)=1:3:1.3,回流时间为9h,三氯氧磷为处理剂,收率为95.5%。在第二步反应中苯基二氯化膦在三乙胺存在下与甲醇作用生成目的物,反应温度为20～30℃,最优的物料配比为n(phPCl2):n(CH3OH):n[N(C2H5)3]=1:2.2:2.7,在最优反应条件下收率为88.4%。Dimethyl phenyl phosphonite was synthesized by benzene, phosphorus trichloride and methyl alcohol as main raw materials through two-step reaction. The first step, phenyl dichloro phosphine was prepared by the reaction of benzene and phosphorous trichloride catalysted by aluminum trichloride, the best condition was found through orthogonal test which was n（C6H6）：n（AlCl3）：n（PCl3）=1：3：1.3, refluxing time was 9 hours, and the product treated by oxyphosphorus trichloride, the yield of the first stage was 95.5%. The second step, dimethyl phenytphosphonite was prepared by reaction of the phenyl-dichlorophosphine and methyl alcohol at 20-30℃ in the presence of triethylaniline, the best material ratio was n（phPCl2）：n（CH3OH）：n[N（C2H5）3]=1 ： 2.2 ： 2.7, at such contions we get the highest yield that is 88.4%.

关 键 词：苯基二氯化膦 苯基亚膦酸二甲酯 光引发剂 

分 类 号：TQ265.1[化学工程—有机化工] TB333[一般工业技术—材料科学与工程]