Facile synthesis of palladium nanoparticles immobilized on magnetic biodegradable microcapsules used as effective and recyclable catalyst in Suzuki-Miyaura reaction and p-nitrophenol reduction

Abstract

This study reports (i) preparation and characterization of palladium nanoparticles (Pd NPs) stabilized on magnetically separable chitosan/agar microcapsules (Pd NPs@Fe3O4/CS-AG microcapsules) and (ii) investigation of catalytic behaviors of the prepared nanoparticles in Suzuki-Miyaura C-C cross-coupling reactions and reduction of p-nitrophenol (p-NP). Fourier transforms infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), elemental mapping, inductively coupled plasma-optical emission spectrometry (ICP-OES) and thermogravimetry/derivative thermogravimetry (TG/DTG) techniques were used for analyzing the Pd NPs@Fe3O4/CS-AG microcapsules. Characterization studies showed that Pd NPs@Fe3O4/CS-AG microcapsules were successfully synthesized and the size of the particles was in the range of 28–39 nm. Pd NPs@Fe3O4/CS-AG microcapsules displayed highly effective catalytic performance in the conversion of various aryl halides into the corresponding biaryl derivatives by Suzuki-Miyaura reaction under solvent-free conditions in 5 min. Pd NPs@Fe3O4/CS-AG microcapsules were also successfully employed in p-NP reduction to p-aminophenol (p-AP) in water at room temperature in 180 s. Moreover, reproducibility studies showed that Pd NPs@Fe3O4/CS-AG microcapsules were highly efficient and could be used many times in both catalytic reactions due to their magnetically separable nature. According to the results of this work, Pd NPs@Fe3O4/CS-AG microcapsules are highly efficient, economical, practical and environmentally superb catalysts for Suzuki-Miyaura reaction and p-NP reduction. © 2019