第 42 卷第 4 期Vol. 42 No. 4
2012 年 8 月Aug 2012

所属栏目:功能材料

二茂铁的电合成及反应条件研究
李 琪,乔庆东*,孙 悦,任铁强,杨占旭 (辽宁石油化工大学 石油化工学院,辽宁 抚顺 113001)
摘 要:以高纯度的环戊二烯(CPD)为原料,以金属铁为阳极,卤化盐作为导电盐,有机溶剂作为介质,在采用氮气保护的情况下电解合成二茂铁。对电解合成二茂铁的反应条件进行了优化研究,结果表明:电解液比例为二甲基亚砜(mL)∶环戊二烯(mL)∶溴化钠(moL)=10∶1∶0.008。实验分别以铁板和镍板作为工作电极和对电极,极板间距为1~1.5 cm,电解电压为3.2~5.2 V(vs.SCE),反应时间为5 h,反应温度为40℃,强烈搅拌条件下电解合成效率较高。
关键词:二茂铁;环戊二烯;电解合成
中图分类号:TQ 268.4  文献标识码:A  文章编号:1009-9212(2012)04-0066-04
Studies on Electrosynthesis of Ferrocene
LI Qi,QIAO Qing-dong*,SUN Yue,REN Tie-qiang,YANG Zhan-xu (School of Petrochemical Engineering,Liaoning Shihua University,Fushun 113001,Liaoning,China)
Abstract:Ferrocene was electrochemically synthesized under nitrogen atmosphere by using high purity of cyclopentadiene as the raw material,iron as the anode,halide salt as the conductive salt,and organic solvent as the medium. The reaction conditions were studied and optimized. The compositions of the electrolyte included 10 mL of dimethyl sulfoxide,1 mL of cyclopentadiene and 0.008 mol of sodium bromide. Iron plate and nickel plate were served as the working electrode and the counter electrode respectively,and the distance of the two electrodes was 1~1.5 cm. The working electrode potential was at the range of 3.2~5.2 V(vs.SCE). The reaction time was 5 hours and the reaction temperature was 40℃. Under the above conditions as well as strong stirring,the efficiency of the electrolytic synthesis was the best.
Key words:ferrocene;cyclopentadiene;electrochemical synthesis
基金项目:辽宁省教育厅科技攻关项目(L2011057)。
作者简介:李 琪(1969-),女,辽宁抚顺人,副教授。主要研究方向:精细化工。(E-mail:liqifs@126.com)
联 系 人:乔庆东。(E-mail:qiaoqingdong@163.com)
收稿日期:2012-09-20