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人工晶体学报 ›› 2021, Vol. 50 ›› Issue (8): 1464-1470.

• 研究论文 • 上一篇    下一篇

Demko-Sharpless 合成稀土四唑化合物的结构及性质

应婷婷, 韩定冲, 谭育慧, 李玉孔, 黄珺, 唐云志, 杜鹏康, 庄加昌   

  1. 江西理工大学材料冶金化学学部,赣州 341000
  • 收稿日期:2021-06-08 出版日期:2021-08-15 发布日期:2021-09-14
  • 通讯作者: 谭育慧,博士,副教授。E-mail:tyxcn@163.com唐云志,博士,教授。E-mail:tangyunzhi75@163.com
  • 作者简介:应婷婷(1997—),女,江西省人,硕士研究生。E-mail:807425109@qq.com
  • 基金资助:
    国家自然科学基金(21761013,21671086,21461010,21471070)

Synthesis, Structures and Properties of Tetrazole Compounds by Demko-Sharpless Method

YING Tingting, HAN Dingchong, TAN Yuhui, LI Yukong, HUANG Jun, TANG Yunzhi, DU Pengkang, ZHUANG Jiachang   

  1. Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China
  • Received:2021-06-08 Online:2021-08-15 Published:2021-09-14

摘要: 使用 Demko-Sharpless法,用氰基吡啶(4-氰基吡啶和3-氰基吡啶)与稀土硝酸盐(Ln=La, Gd, Er)在水热条件下反应,安全有效地合成了四个稀土四唑离子型化合物:[Ln(H2O)8·3(p-TPD)·2(p-HTPD)·7H2O], (Ln=La(1), Gd(2), Er(3), p-TPD=4-四唑吡啶), [Ln(H2O)8·3(m-TPD)·6H2O]和(m-TPD=3-四唑吡啶, Ln=Er(4))。同时,对这四个稀土四唑离子型化合物进行单晶X射线衍射、红外光谱、热重、介电性能、X射线粉末衍射等测试,并且对其介电性质进行了研究。X射线单晶结构分析显示,所得到的四个稀土四唑化合物均为离子型,稀土金属离子与配体分别处于不同的两层,[Ln(H2O)8]3+结构单元与 p-TPD 以及水分子通过氢键作用形成阳离子层,同时p-TPD与p-HTPD通过π-π堆积与氢键作用形成阴离子层,阳离子层和阴离子层交替排列形成一个规则的网络结构。介电性能测试表明化合物1,2具有较好的介电性。

关键词: 四唑化合物, 稀土硝酸盐, 晶体结构, 热重分析, 介电性能

Abstract: The tetracyanopyridine (4-cyanopyridine and 3-cyanopyridine) was reacted with rare earth nitrates (Ln=La, Gd, Er) under hydrothermal conditions by the Demko-Sharpless method, and four rare earth tetrazolium ionic compound were synthesized safely and effectively, named [Ln(H2O)8·3(p-TPD)·2(p-HTPD)·7H2O], (Ln=La(1), Gd(2), Er(3), p-TPD=4-tetrazolpyridine), [Ln(H2O)8·3(m-TPD)·6H2O], (m-TPD=3-tetrazolpyridine, Ln=Er(4)). These four rare earth tetrazolium ionic compounds were characterized by the single crystal X-ray diffraction, infrared spectroscopy, thermogravimetry, dielectric properties, X-ray powder diffraction. The X-ray single crystal structure analysis shows that the four rare earth tetrazolium compounds were all ionic, and the rare earth metal ions and ligands were in two different layers. The [Ln(H2O)8]3+ structure unit and p-TPD and water molecules formed a cationic layer through hydrogen bonding, while p-TPD and p-HTPD formed an anion layer through π-π stacking and hydrogen bonding. The cation layer and anion layer alternately form a regular network structure. Moreover, the dielectric properties tests indicate that the compounds 1, 2 have good dielectric properties.

Key words: tetrazole compound, rare earth nitrate, crystal structure, TGA, dielectric property

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