Xu Zhian, Xiao Liang, Fan Xuetao, Lin Dongtao, Ma Liting, Nie Guochao, Li Yiqun
Department of Chemistry, College of Chemistry and Materials Science, Jinan University, Guangzhou 511443, China.
Photoelectric Information Center, School of Physics and Telecom, Yulin Normal University, Yulin 537000, China.
Nanomaterials (Basel). 2022 May 11;12(10):1641. doi: 10.3390/nano12101641.
A novel and interesting method for the preparation of carboxymethylcellulose-polyaniline film-supported copper catalyst (Cu@CMC-PANI) has been developed via spray-assisted interfacial polymerization. Using copper sulfate as an initiator, spraying technology was introduced to form a unique interface that is perfectly beneficial to the polymerization of aniline monomers onto carboxymethylcellulose macromolecule chains. To further confirm the composition and structure of the as-prepared hybrid film, it was systematically characterized by inductively coupled plasma (ICP), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and thermogravimetric analysis (TGA) techniques. The Cu content in the fresh Cu@CMC-PANI film was determined to be 1.805 mmol/g, and spherical nanoparticles with an average size of ca. 10.04 nm could be observed in the hybrid film. The Cu@CMC-PANI hybrid film was exerted as a dip catalyst to catalyze the aldehyde-alkyne-amine (A) coupling reactions. High yields of the products (up to 97%) were obtained in this catalytic system, and the catalyst could be easily picked up from the reaction mixture by tweezers and reused for at least six consecutive runs, without any discernible losses in its activity in the model reaction. The dip catalyst of Cu@CMC-PANI, with easy fabrication, convenient deployment, superior catalytic activity, and great reusability, is expected to be very useful in organic synthesis.
通过喷雾辅助界面聚合开发了一种新颖有趣的制备羧甲基纤维素-聚苯胺膜负载铜催化剂（Cu@CMC-PANI）的方法。以硫酸铜为引发剂，引入喷雾技术形成独特界面，这对苯胺单体在羧甲基纤维素大分子链上的聚合极为有利。为进一步确认所制备杂化膜的组成和结构，采用电感耦合等离子体（ICP）、傅里叶变换红外光谱（FTIR）、X射线光电子能谱（XPS）、X射线衍射（XRD）、扫描电子显微镜（SEM）、能量色散X射线光谱（EDS）和热重分析（TGA）技术对其进行了系统表征。新鲜的Cu@CMC-PANI膜中的铜含量测定为1.805 mmol/g，在杂化膜中可观察到平均尺寸约为10.04 nm的球形纳米颗粒。将Cu@CMC-PANI杂化膜用作浸渍催化剂来催化醛-炔-胺（A）偶联反应。在该催化体系中获得了高产率的产物（高达97%），并且该催化剂可以用镊子轻松地从反应混合物中取出并重复使用至少六次，在模型反应中其活性没有任何明显损失。Cu@CMC-PANI浸渍催化剂制备简单、部署方便、催化活性优异且可重复使用性强，有望在有机合成中非常有用。
