Department of Chemistry, Faculty of Science and Letters, Aksaray University, 68100 Aksaray, Turkey.
Department of Chemistry, Faculty of Science, University of Qom, 3716146611, Qom, Iran.
Carbohydr Polym. 2019 Oct 15;222:115029. doi: 10.1016/j.carbpol.2019.115029. Epub 2019 Jun 26.
This study reports (i) preparation and characterization of palladium nanoparticles (Pd NPs) stabilized on magnetically separable chitosan/agar microcapsules (Pd NPs@FeO/CS-AG microcapsules) and (ii) investigation of catalytic behaviors of the prepared nanoparticles in Suzuki-Miyaura C-C cross-coupling reactions and reduction of p-nitrophenol (p-NP). Fourier transforms infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), elemental mapping, inductively coupled plasma-optical emission spectrometry (ICP-OES) and thermogravimetry/derivative thermogravimetry (TG/DTG) techniques were used for analyzing the Pd NPs@FeO/CS-AG microcapsules. Characterization studies showed that Pd NPs@FeO/CS-AG microcapsules were successfully synthesized and the size of the particles was in the range of 28-39 nm. Pd NPs@FeO/CS-AG microcapsules displayed highly effective catalytic performance in the conversion of various aryl halides into the corresponding biaryl derivatives by Suzuki-Miyaura reaction under solvent-free conditions in 5 min. Pd NPs@FeO/CS-AG microcapsules were also successfully employed in p-NP reduction to p-aminophenol (p-AP) in water at room temperature in 180 s. Moreover, reproducibility studies showed that Pd NPs@FeO/CS-AG microcapsules were highly efficient and could be used many times in both catalytic reactions due to their magnetically separable nature. According to the results of this work, Pd NPs@FeO/CS-AG microcapsules are highly efficient, economical, practical and environmentally superb catalysts for Suzuki-Miyaura reaction and p-NP reduction.
本研究报告了(i)钯纳米粒子(Pd NPs)稳定在可磁化壳聚糖/琼脂微胶囊(Pd NPs@FeO/CS-AG 微胶囊)上的制备和表征,以及(ii)所制备的纳米粒子在铃木-宫浦 C-C 交叉偶联反应和对硝基苯酚(p-NP)还原中的催化行为的研究。傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、X 射线衍射(XRD)、元素映射、电感耦合等离子体-光学发射光谱(ICP-OES)和热重/导数热重(TG/DTG)技术用于分析 Pd NPs@FeO/CS-AG 微胶囊。表征研究表明,成功合成了 Pd NPs@FeO/CS-AG 微胶囊,颗粒尺寸在 28-39nm 范围内。Pd NPs@FeO/CS-AG 微胶囊在无溶剂条件下,通过铃木-宫浦反应,在 5min 内将各种芳基卤化物转化为相应的联芳基衍生物,显示出高效的催化性能。Pd NPs@FeO/CS-AG 微胶囊还成功地用于在室温下将 p-NP 还原为对氨基酚(p-AP),在水中 180s 内即可完成。此外,重现性研究表明,由于其可磁化的性质,Pd NPs@FeO/CS-AG 微胶囊在这两种催化反应中都非常高效且可多次使用。根据这项工作的结果,Pd NPs@FeO/CS-AG 微胶囊是铃木-宫浦反应和 p-NP 还原的高效、经济、实用和环境友好的催化剂。