摘要
由亚磷酸和正丁醇合成了亚磷酸二丁酯并对其合成工艺进行了探究,对反应原料配比、反应温度、反应时间及催化剂的种类等因素进行考察,并对分析方法进行了初步研究。用滴定的方法对产物组成进行了分析,结果表明最佳合成亚磷酸二丁酯工艺条件为:反应温度125-135℃,正丁醇与亚磷酸摩尔配比为3.6,不加任何催化剂的情况下反应3小时,亚磷酸二丁酯的产率可达68%。采用薄层色谱法,当展开剂选用10:1的正丁醇:苯时可以成功将产品分离。
The method of the synthesized of dibutyl phosphate from phosphorous acid and butanol was studied. Effects of reaction conditions,such as the ratio of raw materials, reaction temperature, reaction time, catalyst,and reaction time were investigated. The methods of analysis were defined. The composition of product was analyzed by titration method. The result showed: the best temperature was 125-135℃ ,the mole ratio of n-butanol / phosphorous acid was 3.6, the best reaction time without catalyst was 3h, the yield of dibutyl phosphate was 68%. The product can be separated by the n-butanol/benzene 10:1 in TLC.
出处
《科技视界》
2011年第23期72-74,共3页
Science & Technology Vision
基金
青岛大学创新型教学实验室研究项目(项目编号QDS09004)
青岛大学创新型教学实验室研究项目(项目编号200904)