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 3aminopropanol 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 (similar to 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. (c) 2025 The Chemical Industry and Engineering Society of China, and Chemical Industry Press Co., Ltd. All rights are reserved, including those for text and data mining, AI training, and similar technologies.