应用化学

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纳米PbO/Ti电极催化还原偏硼酸锂制备硼氢化锂

朱传高*,王凤武   

  1. (淮南师范学院化学系 淮南 232001)
  • 收稿日期:2011-11-21 修回日期:2011-12-22 出版日期:2012-10-10 发布日期:2012-10-10
  • 通讯作者: 朱传高,副教授; Tel/Fax:0554-6863586; E-mail:zhucg88@126.com; 研究方向:纳米材料合成及电化学研究
  • 基金资助:
    国家自然科学基金资助项目(21176099);安徽省教育厅自然科学基金重点项目(KJ2010A309)

Preparation of LiBH4 by Electrocatalytic Reduction of LiBO2 at a Nano-PbO/Ti Electrode

ZHU Chuangao*, WANG Fengwu   

  1. (Department of Chemistry,Huainan Normal College,Huainan 232001,China)
  • Received:2011-11-21 Revised:2011-12-22 Published:2012-10-10 Online:2012-10-10

摘要: 在乙二醇甲醚溶液中电解铅片,制备了铅醇盐配合物,然后将溶液直接水解、凝胶,再通过提拉法涂抹在钛丝表面,450 ℃煅烧2 h制备纳米PbO/Ti电极。 将PbO/Ti电极在0.2~1.0 mol/L LiOH+0.1~0.5 mol/L LiBO2溶液测试催化还原性能,研究了影响电解还原LiBO2制备硼氢化锂(LiBH4)的主要因素,如LiBO2和LiOH浓度等。 通过X射线粉末衍射和扫描电子显微镜对PbO/Ti电极和LiBH4进行了表征。 实验表明,纳米PbO/Ti电极表面颗粒分散较好,修饰电极催化性能稳定,放电电流较大,产率和电流效率分别达15.6%和25.3%。

关键词: 纳米PbO/Ti电极, 电催化还原, 硼氢化锂, 电流效率

Abstract: Lead alkoxide complexes were prepared by electrochemical dissolution of pure lead in the glycol solution. The PbO sols were achieved by the direct sol-gel process of electrolyte solution. The PbO sols coated on pure titanium substrate were calcined at 450 ℃ for 2 h in a muffle furnace, the nano-PbO/Ti electrode was obtained. The electrocatalytic reduction activity of the nano-PbO/Ti electrode was investigated by cyclic voltammetry(CV) in solution containing 0.2~1.0 mol/L LiOH and 0.1~0.5 mol/L LiBO2. The main factors of electrocatalytic reduction of LiBO2 to LiBH4, such as LiBO2 and LiOH concentrations, were studied. The mono-disperse structure and the diameter of nano-PbO/Ti electrode were observed by XRD and SEM, respectively. The results show that the nano PbO is uniformly dispersed on the electrode surface. The electrocatalytic reduction performance of nano-PbO/Ti electrode is stable. A yield of 15.6% and current efficiency of 25.3% were obtained respectively.

Key words: nano-PbO/Ti electrode, electro-catalytic reduction, LiBH4, current efficiency

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