CN102964364B - 一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法 - Google Patents

一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法 Download PDF

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CN102964364B
CN102964364B CN201210509662.2A CN201210509662A CN102964364B CN 102964364 B CN102964364 B CN 102964364B CN 201210509662 A CN201210509662 A CN 201210509662A CN 102964364 B CN102964364 B CN 102964364B
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transition metal
imidazoles
metal copper
base
acid complex
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CN102964364A (zh
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邹建平
蔺万峰
夏梦棋
鲁苗苗
张龙帅
段满玉
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Nanchang Hangkong University
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Abstract

一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法，其特征是化学式为CuC20H14N4O4，三方晶系，空间群为R-3，单胞参数为a = 23.47～23.57 ，b = 23.47～23.57 ，c = 10.06～10.16 ，a= 90°，= 90°， = 120°，Z = 9。本发明的优点是：1、该配合物具有较好的气体吸附性质，其氢气气体吸附值是4.3m2/g；2、与大多数配合物的热分解温度低不同，所合成的化合物的热稳定性较好，其热分解温度为300℃；3、合成方法简单，易操作、原料来源充足、生产成本低廉、化合物合成的产率较高，纯度也很高以及重复性好，使得其适合扩大化生产的要求。

Description

一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法
技术领域
本发明涉及一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法。
背景技术
4-(咪唑-1基)苯甲酸，英文名4-（1h-imidazol-1-yl）benzoic acid，作为一种含羧酸根、两点配位有机配体，被广泛地应用于合成具有光谱学、磁学、吸附分离、药物学和生物无机学研究价值的新型配合物材料的合成与研究，它具有两种配位方式，它能与过渡金属或稀土金属离子形成稳定的配合物。这些配合物在诸如立体化学、配位化学、生物无机化学、磁性、吸附分离、光谱学研究以及反应机理、咪基羧酸配体的反应研究等科学领域均有重要意义。因此深入地研究金属4-(咪唑-1基)苯甲酸配合物的结构和性质，不仅能在配位化学领域为我们提供更多更新颖的结构模型，更能在光学元件开发、仿生技术、生物无机和药物研制等多个方面发挥作用。
发明内容
本发明的目的在于提供一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法，其合成方法简单，易操作、原料来源充足、生产成本低廉、化合物合成的产率较高，纯度也很高以及重复性好，使得其适合扩大化生产的要求。
本发明是这样来实现的，其特征是目标化合物为具有孔洞的过渡金属铜4-(咪唑-1基)苯甲酸配合物，其化学式为CuC20H14N4O4，三方晶系，空间群为R-3，单胞参数为a = 23.47～23.57 ，b = 23.47～23.57 ，c = 10.06～10.16 ，a= 90°，= 90°， = 120°，Z = 9。
金属铜4-(咪唑-1基)苯甲酸配合物的制备方法为：将4-(咪唑-1基)苯甲酸和乙酸铜按照2:1的摩尔比例分别进行称量，其中4-(咪唑-1基)苯甲酸的用量为10毫克；添加10毫升N,N-二甲基甲酰胺在盛有4-(咪唑-1基)苯甲酸的烧杯中，然后搅拌至完全溶解；最后依次缓慢滴加乙酸铜的水溶液，最终pH 值控制在6~7，过滤后静置，一周后得到蓝色块状晶体为过渡金属铜4-(咪唑-1基)苯甲酸配合物。产率为75-80％。
本发明所述的过渡金属铜4-(咪唑-1基)苯甲酸配合物具有较高的比表面积和良好的热稳定性，因此可望作为新型的吸附材料。
本发明具体反应式为：
2C10H8N2O2 (4-(咪唑-1基)苯甲酸) ＋ Cu(CH3COO3)2 H2O→ CuC20H14N4O4 ＋ 2 CH3COOH ＋ H2O
本发明的优点是：1、该配合物具有较好的气体吸附分离性质，其氢气气体吸附值是4.3m2/g； 2、与大多数配合物的热分解温度低不同，所合成的化合物的热稳定性较好，其热分解温度为300℃；3、合成方法简单，易操作、原料来源充足、生产成本低廉、化合物合成的产率较高，纯度也很高以及重复性好，使得其适合扩大化生产的要求。
附图说明
图1为本发明化合物分子的结构图（图中对称码，A: x-y+1,x+1,-z; B: -x+y-1,-x,z; C: -x,-y+1,-z；D: -y,x-y+1,z）。
图2为本发明化合物的热重图。
图3为本发明化合物的粉末衍射图
图4为本发明化合物的紫外漫反射图。
具体实施方式
本发明的化合物CuC20H14N4O4的合成：
CuC20H14N4O4是采用常规溶液挥发法得到的，具体反应式为：
2C10H8N2O2 (4-(咪唑-1基)苯甲酸) ＋ Cu(CH3COO3)2 H2O → CuC20H14N4O4 ＋ 2 CH3COOH ＋ H2O
具体操作步骤为：将4-(咪唑-1基)苯甲酸和乙酸铜按照2: 1的摩尔比例分别进行称量，其中4-(咪唑-1基)苯甲酸的用量为10毫克；添加10毫升N,N-二甲基甲酰胺在盛有4-(咪唑-1基)苯甲酸的烧杯中，然后搅拌至完全溶解；最后依次缓慢滴加乙酸铜的水溶液，最终pH 值控制在6~7，过滤后静置，大约一周后得到蓝色块状晶体为过渡金属铜4-(咪唑-1基)苯甲酸配合物。产率为77％。经单晶衍射仪测试表明该晶体为目标化合物。
如图1、图２、图３、图4所示，本发明的晶体结构参数为：a = 23.5250，b = 23.5250，c = 10.1087 ，a= 90 °,= 90 °= 120°，Z = 9。经过紫外漫反射光谱测试表明，该化合物的能带值为4.18 eV，其氢气气体吸附值是4.3m2/g，其孔体积为1.385cm3/g；另外，化合物的热稳定性测试表明其热分解温度为300 ℃。因此可以作为潜在的吸附材料。

Claims (1)

1.一种过渡金属铜4-(咪唑-1基)苯甲酸配合物作为氢气吸附材料的用途，所述配合物化学式为CuC20H14N4O4，三方晶系，空间群为R-3，单胞参数为a = 23.5250Å，b = 23.5250Å，c = 10.1087Å，a= 90°，β = 90°，γ = 120°，Z = 9，其特征在于，所述配合物的能带值为4.18eV，氢气气体吸附值是4.3m2/g，其孔体积为1.385cm3/g，热分解温度为300℃。
CN201210509662.2A 2012-12-04 2012-12-04 一种过渡金属铜4-(咪唑-1基)苯甲酸配合物及其制备方法 Expired - Fee Related CN102964364B (zh)

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