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Accelerated 5-hydroxymethylfurfural synthesis: Microwave-driven carbohydrate dehydration with mixed metal spinel catalysts

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  • Tomer, Richa
  • Hermans, Sophie
  • Biswas, Prakash

Abstract

In this study, a series of spinel mixed metal oxide catalysts, namely ZnAl2O4, 1M-SO4/ZnAl2O4-TiO2, 1.5M-SO4/ZnAl2O4-TiO2, and 2M-SO4/ZnAl2O4-TiO2 were synthesized using the sol-gel method followed by sulfate impregnation. The characterization results confirmed the spinel structure of ZnAl2O4 and anatase phase of TiO2. Ternary metal oxides Ti-Zn-Al exhibit enhanced Lewis (L) acidity, while Brӧnsted (B) acidic sites were incorporated due to ammonium sulfate treatment and calcination. Total acidity and B/L ratio increased after the impregnation of sulfate groups; however, a higher sulfate loading (>1M) did not enhance acidity but instead caused agglomeration on the catalyst surface. The selective glucose dehydration to 5-hydroxymethylfurfural was performed in a microwave reactor, and the reaction parameters were optimized for a higher 5-HMF yield. Experimental results demonstrated very high glucose conversion (∼90 %) with ∼58 % of 5-HMF at 150 °C in 25 min in the presence of 1M-SO4/ZnAl2O4-TiO2 catalyst in a biphasic NaCl-H2O/THF medium. The B/L ratio and the solvent used played an important role in the yield of 5-HMF. After several cycles, the regenerated 1M-SO4/ZnAl2O4-TiO2 catalyst demonstrated its consistent activity and 5-HMF yield. This study provides detailed insights into mixed metal spinel catalysts for biomass valorization and reveals a fast, efficient microwave-assisted route for sustainable 5-HMF production.

Suggested Citation

  • Tomer, Richa & Hermans, Sophie & Biswas, Prakash, 2025. "Accelerated 5-hydroxymethylfurfural synthesis: Microwave-driven carbohydrate dehydration with mixed metal spinel catalysts," Renewable Energy, Elsevier, vol. 250(C).
    • Handle: RePEc:eee:renene:v:250:y:2025:i:c:s0960148125009309
    DOI: 10.1016/j.renene.2025.123268
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    References listed on IDEAS

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    1. Niakan, Mahsa & Masteri-Farahani, Majid & Seidi, Farzad, 2022. "Efficient glucose-to-HMF conversion in deep eutectic solvents over sulfonated dendrimer modified activated carbon," Renewable Energy, Elsevier, vol. 200(C), pages 1134-1140.
    2. Niakan, Mahsa & Masteri-Farahani, Majid & Seidi, Farzad, 2023. "Sulfonated ionic liquid immobilized SBA-16 as an active solid acid catalyst for the synthesis of biofuel precursor 5-hydroxymethylfurfural from fructose," Renewable Energy, Elsevier, vol. 212(C), pages 50-56.
    3. Shi, Xian & Xing, Xinyi & Liu, Wanni & Ruan, Mengya & Guan, Ying & Lyu, Gaojin & Gao, Hui & Xu, Siquan, 2024. "Cellulose conversion to 5-hydroxymethylfurfural via a simple and efficient phosphate-doped hafnium oxide catalyst," Renewable Energy, Elsevier, vol. 226(C).
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