Tahmasbi Marzieh, Koukabi Nadiya, Seidi Farzad
Department of Chemistry, Semnan University, Semnan 35351-19111, Iran.
Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources and International Innovation Center for Forest Chemicals and Materials, Nanjing Forestry University, Nanjing 210037, China.
Nanoscale. 2022 May 19;14(19):7189-7202. doi: 10.1039/d2nr00303a.
In synthetic organic chemistry, the formation of carbon-carbon bonds is a significant and substantial reaction. As a result, developing a highly active magnetic heterogeneous catalyst with excellent performance is a very appealing technique for constructing C-C bonds in organic chemistry. The present study describes the fabrication of a novel and readily recoverable nickel-based metal-organic framework (MOF) for C-C bond formation through the Sonogashira coupling reaction. The efficient magnetic core-shell structure (FeO@TEA@MOF) with a 3D dendritic fibrous morphology was successfully synthesized using a hydrothermal approach by immobilizing Ni-based MOF onto the FeO@TEA core-shell structure. The fabrication of FeO@TEA@MOF was confirmed by various analyses; Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray analysis (EDS), and elemental mapping confirmed the stepwise fabrication of catalyst. X-ray diffraction analysis (XRD) showed the crystalline nature of the catalyst. Field-emission scanning electron microscopy (FE-SEM) displayed the 3D dendritic fibrous morphology. Thermogravimetric analysis (TGA) and vibrating sample magnetometer analysis (VSM) showed the excellent thermal stability and magnetic properties of FeO@TEA@MOF. The Brunauer-Emmett-Teller analysis (BET) found that the fabricated catalyst with a surface area of 36.2 m g, pore volume of 0.18 cm g, and mean pore diameter of 20.38 nm belongs to mesoporous structures. In addition, the information from the inductively coupled plasma-optical emission spectroscopy (ICP-OES) about fresh and reused catalysts showed that the metal leaching amount is slight and about 1.98%. Other advantages of the FeO@TEA@MOF catalyst can be mentioned as easily reusable for four runs and high performance (above 98%) in synthesizing diphenylacetylene from phenylacetylene, aryl halide, and cesium carbonate (as the base) under solvent-free and microwave conditions.
在合成有机化学中，碳 - 碳键的形成是一种重要且关键的反应。因此，开发一种具有优异性能的高活性磁性非均相催化剂，是有机化学中构建碳 - 碳键的一种极具吸引力的技术。本研究描述了一种新型且易于回收的镍基金属有机框架（MOF）的制备，该框架用于通过Sonogashira偶联反应形成碳 - 碳键。通过水热法将镍基金属有机框架固定在FeO@TEA核壳结构上，成功合成了具有三维树枝状纤维形态的高效磁核壳结构（FeO@TEA@MOF）。通过各种分析证实了FeO@TEA@MOF的制备；傅里叶变换红外光谱（FT - IR）、X射线光电子能谱（XPS）、能量色散X射线分析（EDS）和元素映射证实了催化剂的逐步制备。X射线衍射分析（XRD）显示了催化剂的晶体性质。场发射扫描电子显微镜（FE - SEM）展示了三维树枝状纤维形态。热重分析（TGA）和振动样品磁强计分析（VSM）显示了FeO@TEA@MOF优异的热稳定性和磁性。Brunauer - Emmett - Teller分析（BET）发现，制备的催化剂表面积为36.2 m²/g，孔体积为0.18 cm³/g，平均孔径为20.38 nm，属于介孔结构。此外，电感耦合等离子体发射光谱（ICP - OES）关于新鲜和重复使用催化剂的信息表明，金属浸出量轻微，约为1.98%。FeO@TEA@MOF催化剂的其他优点包括可轻松重复使用四次，以及在无溶剂和微波条件下，由苯乙炔、芳基卤化物和碳酸铯（作为碱）合成二苯乙炔时具有高性能（高于98%）。
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