A mixed-valence Pd^0/IIO nanocomposite microsphere (Pd^0/IIONPs@CMC–Al) was prepared by Al³⁺ ion crosslinked carboxymethylcellulose (CMC) procedure using PdO nanoparticles (NPs) and sodium carboxymethylcellulose in an Al(NO₃)₃ solution. As evidenced by X-ray photoelectron spectroscopy (XPS), the Pd⁰ was generated in situ on the surface of PdO NPs through the reduction of CMC in the formation of composite microspheres. The identity of the as-prepared Pd^0/IIONPs@CMC–Al microsphere was fully verified using various techniques such as Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray analysis (EDX), elemental mappings, and thermogravimetric analysis (TGA). The composite microsphere was found to be effective in the aminocarbonylations of various iodobenzenes with different benzyl amines, resulting in moderate to good yields of the desirable products using phenyl formate as a simple and efficient CO surrogate. The microsphere can be easily recovered through simple filtration and can be recycled for up to five consecutive runs without losing its activity. The advantages include the ease of handling the catalyst, no additional reducing agent required, simple workup procedure, tolerance for a wide range of functional groups, and effective catalyst recyclability, all of which enhances its practical applicability.

Graphical Abstract

中文翻译：

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Al3+ 交联羧甲基纤维素微球中混合价 Pd0/IIO 纳米颗粒的轻松成型用于催化氨基羰基化

混合价 Pd ^0/II O 纳米复合微球 (Pd ^0/II ONPs@CMC–Al) 采用 Al (NO _{3溶液中的 PdO 纳米粒子 (NPs) 和羧甲基纤维素钠，通过 Al} ³⁺离子交联羧甲基纤维素 (CMC) 制备。）₃解。X射线光电子能谱(XPS)证明，Pd ⁰是通过复合微球形成过程中CMC的还原而在PdO NPs表面原位生成的。使用傅里叶变换红外光谱（FTIR）、X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电子显微镜等多种技术充分验证了所制备的Pd ^0/II ONPs@CMC-Al微球的身份。显微镜 (TEM)、X 射线光电子能谱 (XPS)、能量色散 X 射线分析 (EDX)、元素图和热重分析 (TGA)。研究发现，复合微球在各种碘苯与不同苄胺的氨基羰基化反应中有效，使用甲酸苯酯作为简单有效的 CO 替代物，可产生中等到良好的所需产物。微球可以通过简单的过滤轻松回收，并且可以连续循环使用最多五次而不会失去其活性。其优点包括易于处理催化剂、不需要额外的还原剂、简单的后处理程序、对多种官能团的耐受性以及有效的催化剂可回收性，所有这些都增强了其实际适用性。

图形概要