| 第 45 卷第 3 期 |  | Vol. 45 No. 3 | | 2015 年 6 月 | Jun 2015 |
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所属栏目：医药及中间体
磷酸三乙酯合成新工艺研究 |
| 李培国，杨善志，陈 杰
（浙江新安化工集团股份有限公司，浙江 建德 311600） |
| 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0.07 MPa，反应时间60 min；酯化二阶段温度25℃，反应时间为120 min，体系真空度为0.098 MPa。新工艺磷酸三乙酯收率85%，产品酸酯低于1 mgKOH／L，副产氯化氢气体易于去除。 |
| 关键词：磷酸三乙酯；两步法酯化；经济环保 |
| 中图分类号：TQ225.24+1 文献标识码：A 文章编号：1009-9212（2015）03-0030-03 |
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| A Novel method for the Synthesis of Triethyl Phosphate |
| LI Pei-guo, YANG Shan-zhi, CHEN Jie
( Zhejiang Wynca Chemical Industry Group Co., Ltd., Jiande 310000, China) |
| Abstract：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 conditions for the second step esterification reaction are temperature of 25℃, reaction time of 120 min, 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. |
| Key words：triethyl phosphate; two-step esterification; economic and environmental friendly |
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作者简介：李培国（1975-），男，高级工程师，科研管理和新材料、新化学品开发工作（E-mail：li_pg@wynca.com）
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收稿日期： 2015-04-0
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