Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 was prepared by solvothermal synthesis using cadmium nitrate tetrahydrate, sodium p-toluenesulfonate and imidazole as raw materials. It was characterized by X-ray single crystal diffraction, infrared spectroscopy, thermogravimetric analysis and X-ray powder diffraction. The crystal structure was determined by X-ray single crystal diffraction. The crystal structure analysis shows that Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 belongs to the Pca21 space group of the single crystal oblique system, and its cell parameters are a=2.861 3(5)nm, b=0.580 49(10)nm, c=1.544 3(3)nm, α=90°, β=90°, γ=90°, V=2.565 0(8)nm3, Z=4. The composition and structure of the complex were verified by infrared spectroscopy, the stability of the complex was proved by thermogravimetric analysis, and the purity of the complex was demonstrated by X-ray powder diffraction. The catalytic performance of Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 was investigated with Knoevenagel reaction as an example. The experimental results showed that the complex greatly shortened the reaction time and increased the product yield of Knoevenagel reaction, and showed good catalytic activity after repeated use for three times.- DOI:10.3969/j.issn.1000-1565.2024.06.008配合物Cd(Im)2(p-CH3C6H4SO3)2(H2O)2的合成、结构及催化性能杨瑞杰,祁金阳,张迎春,史燚威,王敏(渤海大学 化学与材料工程学院,辽宁 锦州 121013)摘 要:以四水合硝酸镉、对甲基苯磺酸钠和咪唑为原料,利用溶剂热合成法制备了Cd(Im)2(p-CH3C6H4SO3)2(H2O)2.通过X线单晶衍射法、红外光谱法、热重分析法、X线粉末衍射法对其进行表征.X线单晶衍射法测定其晶体结构,结果表明:Cd(Im)2(p-CH3C6H4SO3)2(H2O)2属于单斜晶系的Pca21空间群,其晶胞参数为a=2.861 3(5)nm,b=0.580 49(10)nm,c=1.544 3(3)nm,α=90°,β=90°,γ=90°,V=2.565 0(8)nm3,Z=4.红外光谱法验证了其组成结构,热重分析法证明其稳定性较好,X线粉末衍射法说明该配合物的纯度较高.以Knoevenagel反应为例,考察了Cd(Im)2(p-CH3C6H4SO3)2(H2O)2的催化性能,实验结果表明,该配合物在催化Knoevenagel反应时,很大程度上缩短了反应时间,提高了产物产率,重复使用3次仍有较好的催化活性.关键词:苯磺酸镉配合物;晶体结构;Knoevenagel反应;催化性能中图分类号:O614.24 文献标志码:A 文章编号:1000-1565(2024)06-0625-08Synthesis, structure and catalytic properties of complexCd(Im)2(p-CH3C6H4SO3)2(H2O)2YANG Ruijie, QI Jinyang, ZHANG Yingchun, SHI Yiwei, WANG Min(College of Chemistry and Materials Engineering, Bohai University, Jinzhou 121013, China)Abstract: Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 was prepared by solvothermal synthesis using cadmium nitrate tetrahydrate, sodium p-toluenesulfonate and imidazole as raw materials. It was characterized by X-ray single crystal diffraction, infrared spectroscopy, thermogravimetric analysis and X-ray powder diffraction. The crystal structure was determined by X-ray single crystal diffraction. The crystal structure analysis shows that Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 belongs to the Pca21 space group of the single crystal oblique system, and its cell parameters are a=2.861 3(5)nm, b=0.580 49(10)nm, c=1.544 3(3)nm, α=90°, β=90°, γ=90°, V=2.565 0(8)nm3, Z=4. The composition and structure of the complex were verified by infrared spectroscopy, the stability of the complex was proved by thermogravimetric analysis, and the purity of the complex was demonstrated by X-ray powder diffraction. The catalytic performance of Cd(Im)2(p-CH3C6H4SO3)2(H2O)2 was investigated with Knoevenagel reaction as an example. The experimental results showed that the complex greatly shortened the reaction time and increased the product yield of Knoevenagel reaction, and showed good catalytic activity after repeated use for three times.- 收稿日期:2024-01-08;修回日期:2024-04-08 基金项目:教育部产学合作协同育人项目2024年第一批次资助项目(230805940290824) 第一作者:杨瑞杰(1998— ),女,渤海大学在读硕士研究生,主要从事绿色催化方向研究.E-mail:yangruijie1998@163.com 通信作者:王敏(1977—),女,渤海大学教授,博士,主要从事绿色催化化学的研究.E-mail:wangmin@qymail.bhu.edu.cn 第6期杨瑞杰等:配合物Cd(Im)2(p-CH3C6H4SO3)2(H2O)2的合成、结构及催化性能河北大学学报(自然科学版) 第44卷
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