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Green synthesis of a palladium-polyaniline nanocomposite for green Suzuki-Miyaura coupling reactions

机译:铃木-Miyaura偶联反应的钯-聚苯胺纳米复合材料的绿色合成

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摘要

A palladium-polyaniline (Pd-PANI) nanocomposite was successfully synthesized using a one-pot green synthetic procedure in water by the reaction between aniline hydrochloride and potassium hexachloropalladate. Strong interaction between PANI and Pd was clearly evident in the UV-visible and Fourier transform infrared (FTIR) spectrum of the nanocomposite. Powder X-ray diffraction (XRD) patterns revealed the presence of Pd(0) in the nanocomposite with a fcc crystal structure. Field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) imaging showed that the Pd-PANI nanocomposite has spherical morphology with an average particle size of 175 +/- 42 nm. High resolution TEM imaging and energy dispersive X-ray (EDX) spectroscopy studies revealed that very small nanoparticles of Pd (3.1 +/- 0.9 nm) were found dispersed throughout the PANI matrix. X-ray photoelectron spectroscopy (XPS) revealed the presence of Pd(0) in the nanocomposite. The catalytic behavior of the Pd-PANI nanocomposite was studied for Suzuki-Miyaura coupling reactions in the presence of different bases in both organic and aqueous media. The results revealed that the Suzuki-Miyaura reaction proceeds much faster in water than in toluene. The excellent catalytic activity of the nanocomposite resulted in 86 and 91% yield in water and toluene respectively, when potassium carbonate was used as the base.
机译:通过一锅绿色合成程序在水中通过苯胺盐酸盐与六氯钯酸钾的反应成功地合成了钯-聚苯胺(Pd-PANI)纳米复合材料。在纳米复合材料的紫外可见光和傅立叶变换红外(FTIR)光谱中,PANI和Pd之间的强相互作用显而易见。粉末X射线衍射(XRD)模式揭示了具有fcc晶体结构的纳米复合材料中Pd(0)的存在。场发射扫描电子显微镜(FE-SEM)和透射电子显微镜(TEM)成像显示,Pd-PANI纳米复合材料具有球形形态,平均粒径为175 +/- 42 nm。高分辨率TEM成像和能量色散X射线(EDX)光谱研究表明,发现非常小的Pd纳米颗粒(3.1 +/- 0.9 nm)分散在整个PANI基质中。 X射线光电子能谱(XPS)揭示了纳米复合材料中Pd(0)的存在。研究了Pd-PANI纳米复合材料在有机和水性介质中在不同碱存在下的Suzuki-Miyaura偶联反应的催化行为。结果表明,铃木-宫浦反应在水中的反应比在甲苯中的反应快得多。当使用碳酸钾作为碱时,纳米复合材料的出色的催化活性分别导致在水和甲苯中的产率分别为86%和91%。

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