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Ultrafine silver (Ag) nanoparticles (NPs) were successfully loaded on a robust aluminum (Al) metal–organic framework (MOF), NOTT-300­(Al), by means of a double-solvent method (DSM), and the construction of Ag@NOTT-300­(Al) composites led to a highly efficient catalytic reduction of nitrophenols in these hybrid systems. Of note, the catalytic activity of Ag@NOTT-300­(Al) was used as a heterogeneous catalyst for the reduction of 4-nitrophenol (4-NP) with a reaction rate constant (k) of 2.67 min–1 and activation energy (E a) of ca. 29.7 kJ mol–1. Kinetics and thermodynamics of catalytic 4-NP reduction in this current system complied with the Langmuir–Hinshelwood mechanism. Moreover, the combined use of ultrafine Ag0 NPs and porous NOTT-300­(Al) supports favored reactants diffusion while accelerating the reduction of 4-NP.

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