Nayamadi Mahmoodabadi Malihe, Akhlaghinia Batool, Ein Afshar Sima, Safarzadeh Mostafa
Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad Mashhad 9177948974 Iran
RSC Adv. 2024 Jan 2;14(1):492-516. doi: 10.1039/d3ra07151k.
In the present study, Ni immobilized on FeO@WO functionalized by aminated epichlorohydrin using -methylisothiourea (FeO@WO-E-SMTU-Ni) as a novel magnetically separable nanostructured catalyst was successfully synthesized and characterized using FT-IR, XRD, TEM, FE-SEM, EDX, EDX mapping, VSM, TGA, H-TPR, ICP-OES and CHNS techniques. Characterization results revealed the spherical morphology and superparamagnetic behaviour of the as-synthesized catalyst with mean diameters of 19-31 nm as well as uniform distributions of the desired elements (Fe, O, W, C, N, S and Ni). The antibacterial activity of FeO@WO-E-SMTU-Ni was evaluated against a set of Gram positive and Gram negative bacteria, and the catalyst showed considerable activity against the strain. The aforementioned nanostructured catalyst exhibited perfect catalytic efficiency in the Heck-Mizoroki and Suzuki-Miyaura reactions under mild conditions without using toxic solvents (EtOH as a green solvent and WEB as a benign base). Desired coupled products were obtained from the reaction of different Ar-X (X = I, Br, Cl) with alkyl acrylates and arylboronic acids. A high nickel content with negligible metal leaching during the course of reactions led to the high catalytic performance and stability of FeO@WO-E-SMTU-Ni under optimized reaction conditions. The magnetically separation and ease of recovery and reusability of up to six cycles without a discernible decrease in catalytic activity or metal leaching are the most important features of the catalytic system from both industrial and environmental viewpoints.
在本研究中,成功合成了一种新型的磁性可分离纳米结构催化剂,即通过使用甲基异硫脲将镍固定在经胺化环氧氯丙烷功能化的FeO@WO上(FeO@WO-E-SMTU-Ni),并使用傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)、透射电子显微镜(TEM)、场发射扫描电子显微镜(FE-SEM)、能谱仪(EDX)、能谱映射(EDX mapping)、振动样品磁强计(VSM)、热重分析(TGA)、氢程序升温还原(H-TPR)、电感耦合等离子体发射光谱(ICP-OES)和元素分析仪(CHNS)技术对其进行了表征。表征结果显示,所合成的催化剂具有球形形态和超顺磁性行为,平均直径为19 - 31 nm,并且所需元素(铁、氧、钨、碳、氮、硫和镍)分布均匀。评估了FeO@WO-E-SMTU-Ni对一组革兰氏阳性菌和革兰氏阴性菌的抗菌活性,该催化剂对测试菌株显示出相当的活性。上述纳米结构催化剂在温和条件下,无需使用有毒溶剂(乙醇作为绿色溶剂,碳酸钾作为良性碱),在Heck-Mizoroki反应和Suzuki-Miyaura反应中表现出完美的催化效率。通过不同的芳基卤化物(X = I、Br、Cl)与丙烯酸烷基酯和芳基硼酸反应得到了所需的偶联产物。在反应过程中高镍含量且金属浸出可忽略不计,使得FeO@WO-E-SMTU-Ni在优化的反应条件下具有高催化性能和稳定性。从工业和环境角度来看,磁性分离以及易于回收和重复使用多达六个循环而催化活性或金属浸出没有明显下降是该催化体系最重要的特征。