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Green synthesis of solketal from glycerol using metal-modified ZSM-5 zeolite catalysts: process optimization

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Abstract

This study investigates the production of solketal (2,2-dimethyl-1,3-dioxolane-4-methanol) from glycerol via ketalization reaction using M-ZSM-5 catalysts (M = Fe, Co, Ni, Cu, and Zn). The wet impregnation method ensured precise metal loading and versatility in catalyst preparation. We present a novel approach by employing a suite of characterization techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET), Thermogravimetric analysis (TGA), and Field-emission scanning electron microscopy (FE-SEM), to elucidate the catalyst’s structure, bonding, surface area, thermal stability, and morphology, ultimately linking these properties to their performance. Solketal synthesis was optimized in a reactor, with parameters like temperature, glycerol:acetone molar ratio, catalyst amount, reaction time, and stirring speed. Optimal conditions were identified as 60 °C, 1:4, 0.2 g, 60 min, and 1200 rpm, respectively. Gas chromatography-mass spectrometry (GC–MS) analysis confirmed successful solketal formation. Among M-ZSM-5 catalysts tested, Cu-ZSM-5 emerged the most efficient, achieving an impressive 99% glycerol conversion and 96% solketal selectivity. Notably, Cu-ZSM-5 catalyst displayed exceptional reusability, regaining its initial activity through calcination, thus minimizing waste generation. This research unveils Cu-ZSM-5 as a highly efficient catalyst and promotes sustainability by utilizing a renewable glycerol feedstock to produce valuable solketal with applications in fuel additives, solvents, and pharmaceuticals. This work paves the way for developing environmentally friendly processes for waste valorization and producing valuable bio-based chemicals.

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All data generated is available within the published version of the manuscript.

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Acknowledgements

The author expresses gratitude to the Director of Maulana Azad National Institute of Technology, Bhopal, India, for facilitating the necessary resources and support essential for the successful completion of this research.

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Contributions

Jamna Prasad Gujar: conceptualization, investigation, methodology, data curation, writing the original draft; Bharat Modhera: supervision, methodology, writing—review and editing.

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Correspondence to Bharat Modhera.

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No human and/or animal studies were involved in this study.

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Informed consent was obtained from all participants involved in the study.

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The authors declare no competing interests.

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Responsible Editor: George Z. Kyzas

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Highlights

• Solketal synthesis over metal (M) impregnated with ZSM-5 catalyst was studied.

• Optimal reaction conditions were identified (60 °C, glycerol:acetone 1:4, 0.2-g catalyst, 60 min, 1200 rpm) with solketal formation confirmed by GC-MS.

• The Cu-ZSM-5 catalyst exhibited significant glycerol conversion (99%) and solketal selectivity (96%).

• Cu-ZSM-5 catalyst reusability is vital for economically possible solketal production, showing consistent performance across cycles.

• The ketalization reaction is sustainable and produces no harmful by-products.

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Gujar, J.P., Modhera, B. Green synthesis of solketal from glycerol using metal-modified ZSM-5 zeolite catalysts: process optimization. Environ Sci Pollut Res 31, 28353–28367 (2024). https://doi.org/10.1007/s11356-024-33031-4

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  • DOI: https://doi.org/10.1007/s11356-024-33031-4

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