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磁性膨润土负载钯纳米粒子和交联聚乙烯基吡啶作为高效纳米催化剂用于Suzuki 偶联反应和 4-硝基苯酚还原反应。

Magnetic bentonite decorated with Pd nanoparticles and cross-linked polyvinyl pyridine as an efficient nanocatalyst for Suzuki coupling and 4-Nitrophenol reduction reactions.

机构信息

Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, 76169, Iran.

Department of Carpet, University of Birjand, 17 Shahrivar Street, Birjand, Iran.

出版信息

Sci Rep. 2023 Feb 3;13(1):2001. doi: 10.1038/s41598-023-27800-3.

Abstract

This study reports the preparation of a novel type of support based on magnetically recyclable bentonite functionalized with divinylbenzene-polyvinyl pyridine (PVP-DVB) for Pd (II) nanocatalyst by a simple cost-effective method. Firstly, the conventional co-precipitation method synthesized FeO nanoparticles (NPs) onto bentonite sheets. Then the prepared magnetic support surface was functionalized by divinylbenzene-polyvinyl pyridine (PVP-DVB) to create a cross-linked polymer with a high coordination ability with palladium. Repeated nitrogen units in the PVP-DVB polymer chain increase the number of Pd bonds and thus lead to higher performance of the nanocatalyst. Finally, the palladium NPs were simultaneously synthesized and immobilized under mild conditions. The synthesized nanocatalyst was characterized by several methods such as scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, vibrating sample magnetometer, inductively coupled plasma mass spectrometry and thermogravimetric analysis. The efficiency of synthesized heterogeneous nanocatalyst was investigated in Suzuki-Miyaura cross-coupling reactions between a range of aryl halides (X = Cl, Br, I) with phenylboronic acid and in the reduction of 4-nitrophenol (4-NP). Moreover, the synthesized nanocatalyst could be easily recovered and reused several times with an efficiency greater than 90%.

摘要

本研究报告了一种新型的基于磁性可回收膨润土的支撑物的制备,该支撑物通过一种简单且具有成本效益的方法,用二乙烯基苯-聚乙烯基吡啶(PVP-DVB)进行了功能化,用于 Pd(II)纳米催化剂。首先,通过常规共沉淀法将 FeO 纳米粒子(NPs)合成到膨润土片上。然后,通过二乙烯基苯-聚乙烯基吡啶(PVP-DVB)对制备的磁性载体表面进行功能化,以创建与钯具有高配位能力的交联聚合物。PVP-DVB 聚合物链中的重复氮单元增加了钯键的数量,从而导致纳米催化剂具有更高的性能。最后,在温和条件下同时合成并固定钯 NPs。通过扫描电子显微镜、透射电子显微镜、X 射线光电子能谱、X 射线衍射、傅里叶变换红外光谱、振动样品磁强计、电感耦合等离子体质谱和热重分析等多种方法对合成的纳米催化剂进行了表征。研究了合成的多相纳米催化剂在一系列芳基卤化物(X=Cl、Br、I)与苯硼酸之间的 Suzuki-Miyaura 交叉偶联反应以及 4-硝基苯酚(4-NP)的还原中的效率。此外,合成的纳米催化剂可以很容易地回收和重复使用多次,效率大于 90%。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/31d2/9898528/c4b1ae6debb9/41598_2023_27800_Fig1_HTML.jpg

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