Ultrasound-Enhanced Solvo-Hydrothermal Synthesisof Metal-Free Carbon Catalysts for Eco-FriendlyVisible-Light-Driven Oxidation
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0000-0003-1453-2481 Date
2026-08-24
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Wiley
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Abstract
This study examines the optimization of an ultrasound-assisted solvo-hydrothermal route for the synthesis of metal-free carbonmaterials and evaluates the role of sonication in the selective oxidation of the lignin-derived monomer coniferyl alcohol, animportant precursor to high-value aromatic compounds. Sonication parameters applied during the preparation of the chito-san/lignin (C/L) system, including frequency, power, and irradiation time, were systematically varied to assess their influenceon product yield, selectivity, and the structural and morphological properties of the resulting carbon materials. The as-preparedmaterials were characterized by X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FTIR), andscanning electron microscopy (SEM). Photocatalytic performance was investigated through the visible-light-driven selective oxi-dation of coniferyl alcohol (Con OH) to ferulic acid in acetonitrile. Among the materials examined, the sample synthesized undersonication at 22 kHz for 2 h exhibited the highest photocatalytic activity, affording 22% conversion of coniferyl alcohol and 35%selectivity toward ferulic acid after 4 h of irradiation, together with the formation of 68 μmol of H2O 2 . The improved performanceis attributed to the beneficial effect of ultrasound during the solvo-hydrothermal process, where acoustic cavitation is proposed toenhance mass transfer and promote pathways favorable to selective oxidation. In addition, the ultrasound-assisted method out-performed conventional preparation approaches by reducing processing time and improving product quality. Overall, this workdemonstrates that ultrasound is an effective tool for optimizing solvo-hydrothermal synthesis and provides a sustainable strategyfor the preparation of metal-free carbon photocatalysts for the selective valorization of renewable feedstocks into fuels and othervalue-added products.
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Ahmed Malek Djaballah, Behdokht Hashemi Hosseini, Juan Carlos Colmenares, Ultrasound-Enhanced Solvo-Hydrothermal Synthesis of Metal-Free Carbon Catalysts for Eco-Friendly Visible-Light-Driven Oxidation, Chemistry - Methods 2026, 6, e70154. https://doi.org/10.1002/cmtd.70154