一种新型苯磺酸-咪唑配合物的结构及催化性能研究  

Study on the Structure and Catalytic Property of a Novel Benzenesulfonate-Imidazole Complex

作　　者：祁金阳 王敏[1] 杨瑞杰 张迎春 宋志国[1] QI Jinyang;WANG Min;YANG Ruijie;ZHANG Yingchun;SONG Zhiguo(College of Chemistry&Chemical Engineering,Bohai University,Jinzhou 121013,China)

机构地区：[1]渤海大学化学与材料工程学院,锦州121013

出　　处：《人工晶体学报》2024年第2期300-306,共7页Journal of Synthetic Crystals

基　　金：渤海大学硕士研究生创新基金(YJC2022-030)。

摘　　要：本文以NiSO_(4)·6H_(2)O、咪唑(Im)和苯磺酸钠(C_(6)H_(5)SO_(3)Na)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)(C_(6)H_(5)SO_(3))_(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P 2_(1)/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=8.3773(4),b=10.1518(5),c=20.5263(10),α=90°,β=90.2920(10)°,γ=90°,V=1745.63(15)3,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R_(1)=0.0421,wR_(2)=0.1103。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。A novel benzenesulfonate-imidazole complex of nickel Ni(Im)_(6)(C_(6)H_(5)SO_(3))_(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 N_(2) adsorption-desorption test.The result shows that the complex belongs to monoclinic system,P2_(1)/c space group,exhibiting a 3D spatial structure.It exhibits high phase purity and thermal stability.The cell parameters of complex are a=8.3773(4),b=10.1518(5),c=20.5263(10),α=90°,β=90.2920(10)°,γ=90°,V=1745.63(15)3,Z=2,M r=781.52,F(000)=812,μ=0.737 mm^(-1),D c=1.487 g·cm^(-3),R_(1)=0.0421,wR_(2)=0.1103.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.

关 键 词：咪唑 苯磺酸金属配合物 晶体结构 KNOEVENAGEL反应 催化性能 

分 类 号：O614.813[理学—无机化学]