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作 者:李琪[1] 乔庆东[1] 孙悦[1] 任铁强[1] 杨占旭[1]
机构地区:[1]辽宁石油化工大学石油化工学院,辽宁抚顺113001
出 处:《精细化工中间体》2012年第4期66-69,共4页Fine Chemical Intermediates
基 金:辽宁省教育厅科技攻关项目(L2011057)
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3.2~5.2V(vs.SCE),反应时间为5h,反应温度为40℃,强烈搅拌条件下电解合成效率较高.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.
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