一种新型苯磺酸-咪唑配合物的结构及催化性能研究

摘要/Abstract

摘要： 本文以NiSO₄·6H₂O、咪唑(Im)和苯磺酸钠(C₆H₅SO₃Na)为原料,利用溶剂热法合成了一种新型镍的苯磺酸-咪唑配合物Ni(Im)₆(C₆H₅SO₃)₂。通过单晶X射线衍射、电感耦合等离子体发射光谱、红外光谱、粉末X射线衍射和热重分析技术对其结构、组成、纯度及热稳定性进行了表征,确定了分子结构;通过氮气吸附/脱附测试确定了其比表面积和孔隙结构。结果表明,该配合物属于单斜晶系P2₁/c空间群,为三维空间立体结构,具有较高的相纯度和热稳定性,其晶胞参数a=8.377 3(4) Å,b=10.151 8(5) Å,c=20.526 3(10) Å,α=90°,β=90.292 0(10)°,γ=90°,V=1 745.63(15) Å³,Z=2,M_r=781.52,F(000)=812,μ=0.737 mm^-1,D_c=1.487 g·cm^-3,最终结构残差因子R₁=0.042 1,wR₂=0.110 3。并以Knoevenagel反应为探针,考察了配合物的催化性能,实验结果证明,室温无溶剂条件下,该配合物可在较短时间完成催化反应,且具有较高的催化活性。

关键词: 咪唑, 苯磺酸金属配合物, 晶体结构, Knoevenagel反应, 催化性能

Abstract: A novel benzenesulfonate-imidazole complex of nickel Ni(Im)₆(C₆H₅SO₃)₂ was synthesized by solvothermal method with nickel sulfate, sodium benzenesulfonate and imidazole as main raw materials. The structure, composition and thermal stability of complex were characterized by single X-ray crystal diffraction, inductively coupled plasma optical emission spectrometer, infrared spectroscopy, powder X-ray diffraction and thermogravimetric analysis. The molecular structure was determined. The specific surface area and the pore structure were determined by N₂ adsorption-desorption test. The result shows that the complex belongs to monoclinic system, P2₁/c space group, exhibiting a 3D spatial structure. It exhibits high phase purity and thermal stability. The cell parameters of complex are a=8.377 3(4) Å, b=10.151 8(5) Å, c=20.526 3(10) Å, α=90°, β=90.292 0(10)°, γ=90°, V=1 745.63(15) Å³, Z=2, M_r=781.52, F(000)=812, μ=0.737 mm^-1, D_c=1.487 g·cm^-3, R₁=0.042 1, wR₂=0.110 3. Then, the Knoevenagel reaction was used as a probe to test the catalytic performance of complex. The experimental results show that under room temperature and solvent-free conditions, the complex could complete catalytic reactions in a relatively short time and exhibit high catalytic activity.

Key words: imidazole, benzenesulfonate metal complex, crystal structure, Knoevenagel reaction, catalytic property

中图分类号:

O614.81⁺3

祁金阳, 王敏, 杨瑞杰, 张迎春, 宋志国. 一种新型苯磺酸-咪唑配合物的结构及催化性能研究[J]. 人工晶体学报, 2024, 53(2): 300-306.

QI Jinyang, WANG Min, YANG Ruijie, ZHANG Yingchun, SONG Zhiguo. Study on the Structure and Catalytic Property of a Novel Benzenesulfonate-Imidazole Complex[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2024, 53(2): 300-306.

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