Enhanced catalytic conversion of cellobiose/cellulose to 5-hydroxymethylfurfural using dual catalysts: Sulfonated activated carbon and Lewis acid catalyst

Tomer, Richa;Tonelli, Alessia;Morena, Anthony;Fusaro, Luca;Hermans, Sophie;et.al.
(2025) Biomass & Bioenergy — Vol. 203, p. 108320 (2025)

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An activated carbon (SX+) was functionalized with sulfonic groups via the diazonium coupling method to impart Brӧnsted (B) acidity to catalyze cellobiose and cellulose upgrading into 5-HMF. X-ray photoelectron spectroscopy (XPS) confirmed SO3H groups grafting, which significantly enhanced the total acidity to 1.33 mmol/g cat., as confirmed by Boehm titration. The B nature of acidity was verified by 31P ssNMR. The catalytic activity of SO3H/ SX+ alone and with AlCl3 as Lewis (L) acid was evaluated by optimizing reaction conditions such as temperature, solvent, and B/L ratio. A ~47 % 5-HMF yield was obtained with 100 % cellobiose conversion at 150 ◦C, 4 h with SO3H/Al ratio of 1:10 in Milli-Q water (MQ)/tetrahydrofuran (THF) solvent. When AlCl3 was replaced with heterogeneous Lewis acidic catalysts (γ-Al2O3, AlOOH, and TiO2), TiO2 combined with SO3H/SX+ showed similar catalytic activity, achieving ~50 % yield of 5-HMF with 100 % cellobiose conversion, attributed to its high total acidity (2.4 × 10􀀀 2 mol/g cat.). 5-HMF was isolated from the reaction mixture using liquid-liquid extraction, resulting in ~98 % pure 5-HMF. Moreover, SO3H/SX+ efficiently cleaved the glycosidic bonds of microcrystalline cellulose by giving a ~24 % 5-HMF yield when combined with Lewis acid TiO2. This study presents a novel dual catalytic system, utilizing an optimized B/L acidity ratio to achieve efficient cellulose conversion into 5-HMF.
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Tomer, R., Tonelli, A., Morena, A., Fusaro, L., Meynen, V., Aprile, C., & Hermans, S. (2025). Enhanced catalytic conversion of cellobiose/cellulose to 5-hydroxymethylfurfural using dual catalysts: Sulfonated activated carbon and Lewis acid catalyst. Biomass & Bioenergy, 203, 108320. https://doi.org/10.1016/j.biombioe.2025.108320 (Original work published 2025)