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<p>This study aims to develop an environmentally friendly synthesis protocol for 1,3-dioxolane (DOX5) and 1,3-dioxane (DOX6). The reaction was performed using microwave-assisted, solvent-free acetalization of benzaldehyde with glycerol, facilitated by an acid-activated clay catalyst. The heterogeneous catalyst was produced by treating natural raw clay (RC) with a 3-M aqueous HCl solution for 2&#xa0;h, resulting in the acid-activated clay (AC<sub>2</sub>). The physicochemical properties of the catalyst were analyzed through X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), BET surface area analysis, and X-ray fluorescence (XRF). The AC<sub>2</sub> catalyst demonstrated excellent performance, achieving 90% glycerol conversion, a 96% total yield of both products (DIOX), and 65% selectivity towards 1,3-dioxolane (DOX5) under 270&#xa0;W irradiation power for 20 min. To further enhance glycerol conversion and product selectivity, various reaction parameters were adjusted. Notably, the addition of benzaldehyde and acetophenone derivatives significantly increased DOX5 selectivity, reaching up to 93%. A reaction mechanism was proposed to clarify the formation of these products through the catalytic process. This study highlights the potential of acid-activated clays as efficient catalysts for green chemical synthesis.</p> Graphical abstract <p></p>

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Microwave-assisted valorization of glycerol for efficient production of 1,3-dioxolanes and 1,3-dioxanes catalyzed by acid-activated clay

  • 期刊论文

  • 发表日期：

    2025年10月9日

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  • Rassil Hayder,
  • Jalel Labidi,
  • Néji Besbes,
  • Madiha Kamoun Mhiri

摘要

This study aims to develop an environmentally friendly synthesis protocol for 1,3-dioxolane (DOX5) and 1,3-dioxane (DOX6). The reaction was performed using microwave-assisted, solvent-free acetalization of benzaldehyde with glycerol, facilitated by an acid-activated clay catalyst. The heterogeneous catalyst was produced by treating natural raw clay (RC) with a 3-M aqueous HCl solution for 2 h, resulting in the acid-activated clay (AC2). The physicochemical properties of the catalyst were analyzed through X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), BET surface area analysis, and X-ray fluorescence (XRF). The AC2 catalyst demonstrated excellent performance, achieving 90% glycerol conversion, a 96% total yield of both products (DIOX), and 65% selectivity towards 1,3-dioxolane (DOX5) under 270 W irradiation power for 20 min. To further enhance glycerol conversion and product selectivity, various reaction parameters were adjusted. Notably, the addition of benzaldehyde and acetophenone derivatives significantly increased DOX5 selectivity, reaching up to 93%. A reaction mechanism was proposed to clarify the formation of these products through the catalytic process. This study highlights the potential of acid-activated clays as efficient catalysts for green chemical synthesis.

Graphical abstract