氟代碳酸乙烯酯的合成

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);在反应温度65℃,硫酰氯滴加时间72 min,反应时间90 min,n(EC)∶n(SO2Cl2)=1∶1.3,n(AIBN)∶n(EC)=1∶200的条件下,CEC的收率达85.81%。以氟化钾(KF)为氟化剂在溶剂中对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);在反应温度75℃,反应时间1.5～2 h,n(CEC)∶n(KF)=1∶1.3,V(CEC)∶V(乙腈)=1∶1的条件下,FEC的收率达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。

Synthesis of Fluoroethylene Carbonate

Chloroethylene carbonate(CEC) was prepared by chlorination of ethylene carbonate(EC) with sulfuryl chloride as chlorinating agent and azobisisobutyronitrile(AIBN) as an initiator.CEC reacted with potassium fluoride(KF) which functioned as a fluorinating agent in a solution to give fluoroethylene carbonate(FEC).The optimum technological conditions for preparing CEC were as follows:the reaction taking place at 65 ℃;sulfuryl chloride was added into the reaction solution in drops in 72 min and reacted for 90 min;the molar ratio of ethylene carbonate(EC) and sulfuryl chloride was 1∶1.3;the amount of substance ratio of AIBN to EC was n(AIBN)∶n(EC)=1∶200.The yield of CEC could reach 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 1.5~2 h,and the molar ratio of CEC to KF was 1∶1.3,the molar ratio of CEC and acetonitrile was 1∶1.Under these reaction conditions,the yield of FEC could reach 71.86%.The product was characterized by means of IR and GC-MS.