| 第 45 卷第 3 期 |  | Vol. 45 No. 3 | | 2015 年 6 月 | Jun 2015 |
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所屬欄目：醫藥及中間體
磷酸三乙酯合成新工藝研究 |
| 李培國，楊善志，陳 杰
（浙江新安化工集團股份有限公司，浙江 建德 311600） |
| 摘 要：以三氯氧磷和無(wú)水乙醇為原料，通過(guò)兩步法酯化反應合成了磷酸三乙酯�？疾炝朔磻獪囟�、真空度、反應時(shí)間和物料配比等因素對粗酯收率和酸度的影響。酯化反應優(yōu)化工藝條件為：n（乙醇）∶n（三氯氧磷）=4.5∶1.0，酯化一階段溫度5～10℃，真空度0.07 MPa，反應時(shí)間60 min；酯化二階段溫度25℃，反應時(shí)間為120 min，體系真空度為0.098 MPa。新工藝磷酸三乙酯收率85%，產(chǎn)品酸酯低于1 mgKOH／L，副產(chǎn)氯化氫氣體易于去除。 |
| 關(guān)鍵詞：磷酸三乙酯；兩步法酯化；經(jīng)濟環(huán)保 |
| 中圖分類(lèi)號：TQ225.24+1 文獻標識碼：A 文章編號：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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作者簡(jiǎn)介：李培國（1975-），男，高級工程師，科研管理和新材料、新化學(xué)品開(kāi)發(fā)工作（E-mail：li_pg@wynca.com）
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收稿日期： 2015-04-0
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