摘要
以靛红为原料,采用线性扫描伏安法探讨了电解液组成对电还原过程的影响.实验结果表明:当阴极电解液由硫酸(1.5mol/L)、甲醇(5.0mol/L)和靛红组成,阳极电解液由硫酸(1.0mol/L)溶液组成时,以Cu为工作电极,对靛红电还原起到良好的效果.在此基础上,分别以Cu和Pb为工作电极,进行电解实验,研究了温度、电势和时间等对产物产率和电流效率的影响.优先考虑产率,当工作电极为Cu、电极电势-0.9V(vs.SCE)、电解时间为4h和温度为40℃时,3-羟基-2-吲哚酮的产率为91.1%,电流效率为9.4%;当工作电极为Pb、电极电势-1.1V(vs.SCE)、电解时间为4h和温度为50℃时,产率为89.5%,电流效率为26.1%.这为3-羟基-2-吲哚酮的绿色合成提供了可行的技术参考.
The effect of electrolyte composition on the electrochemical reduction process was discussed by linear sweep voltammetry with isatin as raw material.The experimental results show that when the catholyte was composed of 1.5 mol/L sulfuric acid,5.0 mol/L methanol and isatin,the anolyte was composed of 1.0 mol/L sulfuric acid,the electrochemical reduction of isatin performed and exhibited well results with Cu as working electrode.On the basis of the above results,the effects of temperature,potential and time on product yield and current efficiency were studied by using Cu and Pb as the working electrode respectively.Considering the productivity chiefly,when Cu cathode was used as working electrode,and the reduction time,temperature and potential were 4 h,40℃and-0.9 V(vs.SCE),respectively,the yield for electrochemical synthesis of 3-hydroxy-2-indolinone is 91.1%,and its current efficiency is 9.4%;when Pb cathode was used as working electrode,the reduction time,temperature and potential were 4 h,50℃and-1.1 V(vs SCE),respectively,the yield for electrochemical synthesis of 3-hydroxy-2-indolinone is 89.5%,and its current efficiency is 26.1%.The above results indicate a reliable technical advice for green synthesis of 3-hydroxy-2-indolinone.
作者
李国华
朱家俊
李媛
应元霸
吕德义
LI Guohua;ZHU Jiajun;LI Yuan;YING Yuanba;Lü Deyi(College of Chemical Engineering,Zhejiang University of Technology,Hangzhou 310014,China;State Key Laboratory Breeding Base of Green Chemistry-Synthese Technology,Zhejiang University of Technology,Hangzhou 310014,China)
出处
《浙江工业大学学报》
CAS
北大核心
2018年第3期242-247,281,共7页
Journal of Zhejiang University of Technology
基金
国家自然科学基金资助项目(21173193
213001154)
宁波市自然科学基金资助项目(2014A610089)
关键词
靛红
电还原
3-羟基-2-吲哚酮
绿色合成
Isatin
electrochemical reduction
3-hydroxy-2-indolinone
green synthesis
