Ultrasonic-assisted rapid liquid-phase exfoliation of MFI-type zeolite nanoparticle aggregates

doi:10.1016/j.cjche.2025.02.029

Abstract

Abstract: The preparation of dispersible MFI-type zeolite nanoparticles with open micropores is challenging. Herein, a rapid and effective ultrasound-assisted liquid-phase exfoliation method along with a freezedrying process for redispersion of calcined silicalite-1 (S-1) zeolite nanoparticle aggregates using 3- aminopropanol as an exfoliating agent is demonstrated. The exfoliation of S-1 zeolite nanoparticles is characterized by X-ray diffraction, scanning electron microscopy and DLS particle size analysis. The effects of drying methods of as-synthesized zeolite nanoparticle suspension, zeolite contents in frozen nanoparticle suspension, exfoliating agent concentrations, and zeolite doses in ultrasonic suspension on exfoliation efficiency are systematically investigated. It is found that the S-1 zeolite nanoparticle (~70 nm) achieves a yield up to 95% through a 30 min ultrasonic exfoliation in a 3-aminopropanol solution along with a freeze-drying process. The proposed exfoliation mechanism involves two primary stages: guest molecule insertion followed by water expansion, both substantially enhanced by tip sonication. This work offers a comprehensive understanding of the exfoliation process, provides valuable insights into the dispersion of sintered zeolite nanoparticles.

Key words: Nanoparticles, Zeolite, Liquid phase exfoliation, Ultrasonic-assisted, Vacuum freeze drying, Sintering

摘要： The preparation of dispersible MFI-type zeolite nanoparticles with open micropores is challenging. Herein, a rapid and effective ultrasound-assisted liquid-phase exfoliation method along with a freezedrying process for redispersion of calcined silicalite-1 (S-1) zeolite nanoparticle aggregates using 3- aminopropanol as an exfoliating agent is demonstrated. The exfoliation of S-1 zeolite nanoparticles is characterized by X-ray diffraction, scanning electron microscopy and DLS particle size analysis. The effects of drying methods of as-synthesized zeolite nanoparticle suspension, zeolite contents in frozen nanoparticle suspension, exfoliating agent concentrations, and zeolite doses in ultrasonic suspension on exfoliation efficiency are systematically investigated. It is found that the S-1 zeolite nanoparticle (~70 nm) achieves a yield up to 95% through a 30 min ultrasonic exfoliation in a 3-aminopropanol solution along with a freeze-drying process. The proposed exfoliation mechanism involves two primary stages: guest molecule insertion followed by water expansion, both substantially enhanced by tip sonication. This work offers a comprehensive understanding of the exfoliation process, provides valuable insights into the dispersion of sintered zeolite nanoparticles.

关键词: Nanoparticles, Zeolite, Liquid phase exfoliation, Ultrasonic-assisted, Vacuum freeze drying, Sintering

Xinyi Gao, Qiancheng Zheng, Zhengbao Wang. Ultrasonic-assisted rapid liquid-phase exfoliation of MFI-type zeolite nanoparticle aggregates[J]. Chinese Journal of Chemical Engineering, 2025, 83(7): 38-50.

Xinyi Gao, Qiancheng Zheng, Zhengbao Wang. Ultrasonic-assisted rapid liquid-phase exfoliation of MFI-type zeolite nanoparticle aggregates[J]. 中国化学工程学报, 2025, 83(7): 38-50.

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