Demko-Sharpless合成稀土四唑化合物的结构及性质  

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

作　　者：应婷婷 韩定冲 谭育慧[1] 李玉孔 黄珺[1] 唐云志[1] 杜鹏康 庄加昌 YING Tingting;HAN Dingchong;TAN Yuhui;LI Yukong;HUANG Jun;TANG Yunzhi;DU Pengkang;ZHUANG Jiachang(Faculty of Materials Metallurgy and Chemistry,Jiangxi University of Science and Technology,Ganzhou 341000,China)

机构地区：[1]江西理工大学材料冶金化学学部,赣州341000

出　　处：《人工晶体学报》2021年第8期1464-1470,共7页Journal of Synthetic Crystals

基　　金：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(H_(2)O)_(8)·3(p-TPD)·2(p-HTPD)·7H 2 O],(Ln=La(1),Gd(2),Er(3),p-TPD=4-四唑吡啶),[Ln(H_(2)O)_(8)·3(m-TPD)·6H_(2)O]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(H_(2)O)_(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。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(H_(2)O)_(8)·3(p-TPD)·2(p-HTPD)·7H 2 O],(Ln=La(1),Gd(2),Er(3),p-TPD=4-tetrazolpyridine),[Ln(H_(2)O)_(8)·3(m-TPD)·6H_(2)O],(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(H_(2)O)_(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 throughπ-πstacking 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.

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 

分 类 号：O641.4[理学—物理化学]