物理化学学报 >> 2016, Vol. 32 >> Issue (9): 2232-2240.doi: 10.3866/PKU.WHXB201605263

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3, 4-二乙氧基苯甲酸与2, 2'-联吡啶三元稀土配合物的合成、晶体结构及热化学性质

靳成伟1,2,王叶1,2,宿素玲3,张建军1,2,*()   

  1. 1 河北师范大学分析测试中心,石家庄050024
    2 河北师范大学化学与材料科学院,石家庄050024
    3 河北省锅炉压力容器监督检验院,石家庄050061
  • 收稿日期:2016-04-15 发布日期:2016-09-08
  • 通讯作者: 张建军 E-mail:jjzhang6@126.com
  • 基金资助:
    国家自然科学基金(21473049);河北省自然科学基金(B2016205207)

Synthesis, Crystal Structures and Thermochemical Properties of Ternary Rare Earth Complexes Based on 3, 4-Diethoxybenzoic Acid and 2, 2'-Bipyridine

Cheng-Wei JIN1,2,Ye WANG1,2,Su-Ling XU3,Jian-Jun ZHANG1,2,*()   

  1. 1 Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024, P. R. China
    2 College of Chemistry & Material Science, Hebei Normal University, Shijiazhuang 050024, P. R. China
    3 Hebei Super Vision & Inspection Institute of Boiler & Pressure Vessel, Shijiazhuang 050061, P. R. China
  • Received:2016-04-15 Published:2016-09-08
  • Contact: Jian-Jun ZHANG E-mail:jjzhang6@126.com
  • Supported by:
    National Natural Science Foundation of China(21473049);Natural Science Foundation of Hebei Province, China(B2016205207)

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摘要：

本文合成了两种三元稀土配合物[Ln（3, 4-DEOBA）3DIPY]2DIPY（Ln=Er（1），Gd（2）；3, 4-DEOBA：3, 4-二乙氧基苯甲酸根；DIPY：2, 2'-联吡啶），通过元素分析，红外光谱和单晶X-射线衍射对配合物进行表征和分析。实验表明两种配合物是同种晶型的双核分子，相邻结构单元通过π-π作用形成一维链状和二维层状的超分子结构。同时还利用同步热分析与傅里叶变换红外联用（TG-FTIR）技术对配合物的热分解机理进行分析。通过差示扫描量热（DSC）技术，测得两种配合物的摩尔热容，将所得配合物的摩尔热容与折合温度进行多项式拟合，并根据热力学方程，计算得到了两种配合物的舒平摩尔热容和热力学函数值。

关键词: 3, 4-二乙氧基苯甲酸, 2, 2'-联吡啶, 稀土配合物, 热分解机理, 摩尔热容, 热化学性质

Abstract:

Two novel ternary rare earth complexes [Ln(3, 4-DEOBA)3DIPY]2DIPY (Ln=Er (1), Gd (2); 3, 4-DEOBA=3, 4-diethoxybenzoate; DIPY=2, 2'-bipyridine) were synthesized and characterized by elemental analysis, infrared spectroscopy and X-ray single crystal diffraction. The experiments show that the two complexes are isomorphous with dinuclear structures, and adjacent structure units are stitched together through π-π interactions to form 1D chains and 2D-layered supramolecular structures. Simultaneous thermal analysis and Fourier transform infrared detection (TG-FTIR) was used to study the process of the thermal decomposition of the complexes. The molar heat capacity of the two complexes was obtained by differential scanning calorimetry (DSC). The smoothed values of the average molar heat capacity and thermodynamic functions of the complexes were calculated by the fitted polynomial and thermodynamic equations.

Key words: 3, 4-Diethoxybenzoic acid, 2, 2'-Bipyridine, Rare earth complex, Thermal decomposition mechanism, Molar heat capacity, Thermochemical property