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Demko-Sharpless 合成稀土四唑化合物的结构及性质
引用本文:应婷婷,韩定冲,谭育慧,李玉孔,黄珺,唐云志,杜鹏康,庄加昌.Demko-Sharpless 合成稀土四唑化合物的结构及性质[J].人工晶体学报,2021,50(8):1464-1470.
作者姓名:应婷婷  韩定冲  谭育慧  李玉孔  黄珺  唐云志  杜鹏康  庄加昌
作者单位:江西理工大学材料冶金化学学部,赣州 341000
基金项目:国家自然科学基金(21761013,21671086,21461010,21471070)
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  
收稿时间:2021-06-08

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.Synthesis,Structures and Properties of Tetrazole Compounds by Demko-Sharpless Method[J].Journal of Synthetic Crystals,2021,50(8):1464-1470.
Authors:YING Tingting  HAN Dingchong  TAN Yuhui  LI Yukong  HUANG Jun  TANG Yunzhi  DU Pengkang  ZHUANG Jiachang
Affiliation:Faculty of Materials Metallurgy and Chemistry, Jiangxi University of Science and Technology, Ganzhou 341000, China
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.
Keywords:tetrazole compound  rare earth nitrate  crystal structure  TGA  dielectric property  
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