化工学报 ›› 2017, Vol. 68 ›› Issue (4): 1660-1666.DOI: 10.11949/j.issn.0438-1157.20161359

• 材料化学工程与纳米技术 • 上一篇    下一篇

对丙烯基茴香醚的直接电氧化活化

武倩倩, 叶春梅, 廖艳梅, 张安伦, 朱英红, 马淳安   

  1. 浙江工业大学化工学院, 绿色化学合成技术国家重点实验室培育基地, 浙江 杭州 310032
  • 收稿日期:2016-09-28 修回日期:2016-12-23 出版日期:2017-04-05 发布日期:2017-04-05
  • 通讯作者: 朱英红
  • 基金资助:

    国家重点基础研究发展计划项目前期研究专项(2012CB722604)。

Direct electro-oxidation of p-propenyl anisole

WU Qianqian, YE Chunmei, LIAO Yanmei, ZHANG Anlun, ZHU Yinghong, MA Chun'an   

  1. State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology, College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310032, Zhejiang, China
  • Received:2016-09-28 Revised:2016-12-23 Online:2017-04-05 Published:2017-04-05
  • Supported by:

    supported by the National Basic Research Program of China (2012CB722604).

摘要:

采用循环伏安法(CV(、恒电位电解法和计时电流法研究了对丙烯基茴香醚(p-PA)在乙腈-水混合溶液中的直接电氧化行为,考察了水的含量、扫描速度、温度、反应底物浓度、电解电位、电极等因素对p-PA中C═C电氧化活化的影响。实验结果表明,p-PA在乙腈-水混合溶液中的电氧化过程是不可逆的,且该过程受扩散步骤控制,扩散系数D=2.53×10-6cm2·s-1。通过GC-MS检测,p-PA直接电氧化的主要产物为对甲氧基苯甲醛(p-MBA)。在一室型无隔膜电解槽中,以石墨棒为工作电极,25℃下,乙腈-水混合溶液中水的含量为20%时,反应底物几乎全部转化,p-MBA的产率可达93%。

关键词: 对丙烯基茴香醚, 直接电氧化, C═C电氧化活化, 对甲氧基苯甲醛, 无隔膜电解槽

Abstract:

Direct electro-oxidation of p-propenyl anisole(p-PA) in acetonitrile aqueous solutions was studied by cyclic voltammetry (CV), controlled potential electrolysis and chronoamperometry. The effect of water content, scan rate, temperature, reactant concentration, electrolysis potential and electrode on activation of C═C bond were studied. The results showed that electro-oxidation of p-PA in acetonitrile aqueous solutions was an irreversible process, which was mainly diffusion-controlled with the diffusion coefficient (D) of 2.53×10-6 cm2·s-1. The major direct electro-oxidation product of p-PA was p-methoxybenzaldehyde (p-MBA). At 20% water content, the yield of p-MBA could be improved to 93% and almost complete conversion of reactant on graphite rod electrode at 25℃ in an undivided electrolytic cell.

Key words: p-propenyl anisole, direct electro-oxidation, C=C bond oxidative activation, p-methoxy-benzaldehyde, undivided electrolytic cell

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