氟代碳酸乙烯酯的合成
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湖南省高校创新平台开放基金项目,编号,11k062


Synthesis of Fluoroethylene Carbonate
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    摘要:

    以偶氮二异丁腈(AIBN)为引发剂,硫酰氯(SO2Cl2)为氯化剂,对碳酸乙烯酯(EC)进行氯化,合成了氯代碳酸乙烯酯 (CEC)。当反应温度为65℃,硫酰氯滴加时间72min,反应时间90min,n(EC):n(SO2Cl2)=1:1.3,n(AIBN):n(EC)=1:200时CEC的收率达到85.81% 。用氟化钾(KF)在溶剂中对CEC进行氟化,得到锂离子电池电解液添加剂氟代碳酸乙烯酯(FEC)。当反应温度75℃,反应时间1.5~2h,n(CEC):n(KF)=1:1.3, V(CEC):V(乙腈)=1:1的条件下FEC的收率为71.86%。采用红外光谱及气质联用分析对产物进行了结构表征。

    Abstract:

    Chloroethylene carbonate (CEC) was prepared by chlorination of ethylene carbonate (EC) with sulfuryl chloride and azobisisobutyronitrile (AIBN) as an initiator. CEC reacted with Potassium fluoride (KF) as a fluorinating agent in a solution to give Fluoroethylene Carbonate (FEC). The optimum technological conditions for preparing CEC were as follows: the reaction taken place at 65℃; sulfuryl chloride was added into the reaction solution in drops in 72min and reacted for 1.5h, the molar ratio of ethylene carbonate(EC) and sulfuryl chloride was 1:1.3, the amount of substance ratio of AIBN and EC was n(AIBN):n(EC)=1:200. The yield could be reached to 85.81% under such reaction conditions. The optimum technological conditions for preparing FEC were as follows: acetonitrile was chosen as the solvent, the reaction temperature was 75℃, the reaction time was 1.5 to 2h, the molar ratio of CEC and KF was1:1.3. Under these reaction conditions, the yield can be reached to 71.86%. The product was characterized by IR and GC-MS.

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姚桂,段正康.氟代碳酸乙烯酯的合成[J].精细化工,2012,29(4):0

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  • 收稿日期:2011-10-25
  • 最后修改日期:2011-12-26
  • 录用日期:2012-01-10
  • 在线发布日期: 2012-03-20
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