Ni Nanoparticles Supported Montmorillonite Clay for Selective Catalytic Transfer Hydrodeoxygenation of Vanillin into 2‐Methoxy‐4‐methylphenol

Abstract The targeted catalytic transfer hydrodeoxygenation (CTHDO) of vanillin (VAN) to 2‐methoxy‐4‐methylphenol (MMP) holds promise as a noteworthy subject in the domain of bio‐oil utilization, offering potential as a future biofuel and finding versatile use in fragrances and pharmaceutical industry. In this study, stable, cost‐effective Ni nanoparticles supported on montmorillonite (MMT) clay was synthesized for eco‐friendly, alcohol‐mediated CTHDO of VAN to MMP. The Ni(10 %)/MMT catalyst achieved >99 % VAN conversion and 95.2 % MMP selectivity using isopropanol (IPA) as a solvent and hydrogen donor. Characterization encompassing PXRD, SEM, TEM, and XPS confirmed successful Ni integration onto MMT. NH 3 ‐TPD, pyridine‐IR, and H 2 ‐TPR analysis evaluated catalyst surface acidity and reducibility. The synergy between surface‐modulated acidity of MMT and Ni nanoparticles collectively facilitated IPA and VAN activation, driving CTHDO performance. The Ni(10 %)/MMT catalyst displayed sustained activity over five recycles. Its exceptional stability and performance underscore its potential as an eco‐friendly, sustainable, non‐noble transition metal‐based catalyst for the hydrogenating lignin bio‐oil model compounds, contributing to greener catalytic advancements.