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Mesoporous poly-melamine-formaldehyde stabilized palladium nanoparticle (Pd@mPMF) catalyzed mono and double carbonylation of aryl halides with amines

机译:介孔聚三聚氰胺-甲醛稳定的钯纳米粒子(Pd @ mPMF)催化芳基卤化物与胺的单羰基和双羰基化

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摘要

A new mesoporous poly-melamine-formaldehyde material supported Pd nano catalyst (mPMF-Pd-0) has been synthesized and characterized by thermogravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), high-resolution transmission electron microscopy (HRTEM), UV-vis diffuse reflection spectroscopy (DRS), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and a N-2 adsorption study. The mPMF-Pd-0 material showed very good catalytic activity in the field of mono and double amino carbonylation of aryl bromides/iodides. Moreover, the catalyst is easily recoverable and can be reused six times without appreciable loss of catalytic activity in the above reactions. So, the highly dispersed and strongly bound palladium(0) sites in the mPMF-Pd-0 could be responsible for the observed high activities. Due to strong binding with the functional groups of the polymer, no evidence of leached Pd from the catalyst during the course of reaction occurred, suggesting true heterogeneity in the catalytic process.
机译:合成了一种新型的介孔聚三聚氰胺-甲醛材料负载的钯纳米催化剂(mPMF-Pd-0),并通过热重分析(TGA),粉末X射线衍射(XRD),扫描电子显微镜(SEM),能量色散进行了表征X射线光谱(EDS),高分辨率透射电子显微镜(HRTEM),紫外可见漫反射光谱(DRS),拉曼光谱,X射线光电子光谱(XPS)和N-2吸附研究。 mPMF-Pd-0材料在芳基溴化物/碘化物的单氨基和双氨基羰基化领域表现出非常好的催化活性。此外,该催化剂易于回收并且可以重复使用六次而在上述反应中没有明显的催化活性损失。因此,mPMF-Pd-0中高度分散且牢固结合的钯(0)位点可能是观察到的高活性的原因。由于与聚合物官能团的牢固结合,在反应过程中未发现有钯从催化剂中浸出的迹象,表明催化过程中存在真正的异质性。

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