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Preparation anchored Pd nanoparticles on glyoxal modified metal- organic framework for Sonogashira coupling reactions
Journal of Organometallic Chemistry ( IF 2.1 ) Pub Date : 2019-12-05 00:00:00 , DOI: 10.1016/j.jorganchem.2019.121069
Heshmatollah Alinezhad , Mansoureh Cheraghian , Shahram Ghasemi

UIO-66-NH2-Gl@Pd nanocatalyst was successfully synthesized during post-synthetic modification (PSM) method and its application was investigated in the Sonogashira coupling reactions. Initially, UIO-66-NH2 was synthesized and identified. This metal organic framework (MOF) was modified with glyoxal, then, palladium nanoparticles (NPs) were supported on the modified framework through PSM. This nanocatalyst was identified via Fourier-transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance (1HNMR) spectroscopy, N2 gas adsorption-desorption, thermogravimetric analyses (TGA), energy dispersive X-ray mapping spectroscopy (EDX-MAP), field emission scanning electron microscopy (FE-SEM), and X-ray diffraction (XRD). 1HNMR analysis showed that around 30% of the amine functional groups of nanoporous UIO-66-NH2 were modified with glyoxal. The formation of Pd NPs supported on MOF was confirmed by transmission electron microscopy (TEM) and EDX-MAP. As well, according to the inductive couple plasma atomic emission spectroscopy (ICP), around 2.98 w% of Pd NPs was present in the modified MOF. Eventually, the nanocatalyst provided the excellent catalytic activity in the Sonogashira coupling reaction. Also, the nanocatalyst has the capability to be easily recycled up to 4 times, while its catalytic activity was maintained during the activity.



中文翻译:

在乙二醛修饰的金属-有机骨架上制备锚定的Pd纳米粒子用于Sonogashira偶联反应

在合成后修饰(PSM)方法中成功合成了UIO-66-NH 2 -Gl @ Pd纳米催化剂,并研究了其在Sonogashira偶联反应中的应用。最初,合成并鉴定了UIO-66-NH 2。用乙二醛对金属有机骨架(MOF)进行修饰,然后通过PSM将钯纳米粒子(NPs)负载在修饰的骨架上。该纳米催化剂通过傅立叶变换红外光谱(FT-IR),质子核磁共振(1 HNMR)光谱,N 2气体吸附-解吸,热重分析(TGA),能量色散X射线谱图(EDX-MAP)进行鉴定),场发射扫描电子显微镜(FE-SEM)和X射线衍射(XRD)。1 HNMR分析表明,约30%的纳米多孔UIO-66-NH 2的胺官能团被乙二醛改性。通过透射电子显微镜(TEM)和EDX- MAP证实了MOF上负载的Pd NP的形成。同样,根据感应耦合等离子体原子发射光谱法(ICP),修饰的MOF中存在约2.98 w%的Pd NP。最终,纳米催化剂在Sonogashira偶联反应中提供了优异的催化活性。同样,纳米催化剂具有易于回收多达4次的能力,同时在活性期间保持了其催化活性。

更新日期:2019-12-05
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