Journal of Petrochemical Universities ›› 2010, Vol. 23 ›› Issue (3): 58-61.DOI: 10.3696/j.issn.1006-396X.2010.03.014

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The Organic Electrochemical Synthesis of Nickelocene

  

  1. School of Petrochemical Engineering,Liaoning Shihua University,Fushun Liaoning 113001,P.R.China
  • Received:2010-04-19 Revised:2010-05-13 Published:2010-09-25 Online:2010-09-25

有机电化学法合成二茂镍的研究

李琪 乔庆东*   

  1. 辽宁石油化工大学石油化工学院, 辽宁抚顺113001
  • 作者简介:李琪(1969 -), 女, 辽宁抚顺市, 副教授, 在读硕士
  • 基金资助:
    辽宁省自然科学基金项目(20082187);辽宁省教育厅科技攻关项目(2008379)

Abstract: The purification of cyclopentadiene and the electrosynthesis of nickelocene were studied. Nickelocene was electrochemical synthesized by using purified cyclopentadiene as the raw material, and metal nickel used as both anode and cathode, sodium bromide as the conducting salt, N,N-dimethylformamide (DMF) as the organic solvent, and nitrogen as the protection gas of the solution. In the dicyclopentadiene purification experiment, the best depolymerization and best circumfluence temperature of cyclopentadiene are 170 ℃ and 120 ℃ respectively. The purification process above must be continuously carried on. The purities of dicyclopentadiene and cyclopentadiene determined by gas chromatography are 95.4% and 97.3%. In the electrochemical synthesis experiment, the electrode potential changes are first determined using calomel electrode as the reference electrode; meanwhile the polarizing curves are also measured in order to confirm the best current density, i.e. 3.93 mA/cm2. Secondly the best reaction time determined is 210 min through the observation of the solution color changes, the electrode potential changes, the ultraviolet and the infrared spectrogram of the solution. Finally the current efficiency is 82.87% by calculating the mass decrement of nickel board during the experiment. 

Key words: Nickelocene , Dicyclopentadiene , Cyclopentadiene , Polarizating curve

摘要: 对环戊二烯的提纯和二茂镍的电化学合成过程进行研究,以提纯后的环戊二烯为原料,金属镍为阳极和阴极,溴化钠作导电盐,N,N二甲基甲酰胺(DMF)作有机溶剂,采用氮气保护,恒流源电解,合成了二茂镍。结果表明,双环戊二烯的最佳解聚温度170 ℃,环戊二烯提纯时的最佳回流温度120 ℃,且提纯过程必须连续,用气相色谱法检测双环戊二烯和环戊二烯的纯度分别为95.4%和97.3%。在电合成实验中,首先以甘汞电极为参比电极跟踪电解合成过程的电极电位变化,并作极化曲线图,确定最佳电流密度3.93 mA/cm2。其次,通过观察溶液的颜色变化、电极电位的变化和反应溶液的紫外可见、红外谱图变化确定实验最佳反应时间为210 min。最后,通过镍板的减少量计算电流效率为82.87%。

关键词: 二茂镍 , 双环戊二烯 , 环戊二烯 , 极化曲线

Cite this article

LI Qi, QIAO Qing-dong. The Organic Electrochemical Synthesis of Nickelocene[J]. Journal of Petrochemical Universities, 2010, 23(3): 58-61.

李琪, 乔庆东. 有机电化学法合成二茂镍的研究[J]. 石油化工高等学校学报, 2010, 23(3): 58-61.