摘要
以三氯氧磷和无水乙醇为原料，通过两步法酯化反应合成了磷酸三乙酯。考察了反应温度、真空度、反应时间和物料配比等因素对粗酯收率和酸度的影响。酯化反应优化工艺条件为：n（乙醇）：n（三氯氧磷）：4．5：1．0，酯化一阶段温度5-10℃，真空度0．07MPa，反应时间60min；酯化二阶段温度25℃，反应时间为120min，体系真空度为0．098MPa。新工艺磷酸三乙酯收率85％，产品酸酯低于1mgKOH／L，副产氯化氢气体易于去除。
Triethyl phosphate was synthesized by the two-step esterification using phosphorus oxychloride and ethanol as raw materials. The effects of reaction conditions including temperature, vacuum pressure, reaction time and ratio of materials on the yield and acidity of the obtained ester were evaluated. The experimental results indicated that the optimum technological conditions were as followings： 1. The molar ratio of ethanol to phosphorus oxychloride is 4.5：1; 2. The experimental conditions for first step of esterification reaction are temperature of 5-10℃, vacuum pressure of 0.07 MPa, and reaction time of 60 min; 3. The experimental eonditions for the second step esteriflcation reaction are temperature of 25℃, reaction time of 120 rain, and vacuum pressure of 0.098 MPa. A typical reaction yield is 85% with an acidity of the product lower than 1mg KOH/L. Furthermore, the hydrogen chloride gas produced in the reaction process can be easily eliminated.
出处
《精细化工中间体》
CAS
2015年第3期30-32,78,共4页
Fine Chemical Intermediates
关键词
磷酸三乙酯
两步法酯化
经济环保
triethyl phosphate
two-step esterification
economic and environmental friendly
