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Amphiphilic organosilane-directed synthesis of crystalline zeolite with tunable mesoporosity

Nature Materials volume 5, pages 718–723 (2006)Cite this article

Abstract

Zeolites are a family of crystalline aluminosilicate materials widely used as shape-selective catalysts, ion exchange materials, and adsorbents for organic compounds1,2. In the present work, zeolites were synthesized by adding a rationally designed amphiphilic organosilane surfactant to conventional alkaline zeolite synthesis mixtures. The zeolite products were characterized by a complementary combination of X-ray diffraction (XRD), nitrogen sorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The analyses show that the present method is suitable as a direct synthesis route to highly mesoporous zeolites. The mesopore diameters could be uniformly tailored, similar to ordered mesoporous silica with amorphous frameworks3. The mesoporous zeolite exhibited a narrow, small-angle XRD peak, which is characteristic of the short-range correlation between mesopores, similar to disordered wormhole-like mesoporous materials4,5. The XRD patterns and electron micrographs of the samples taken during crystallization clearly showed the evolution of the mesoporous structure concomitantly to the crystallization of zeolite frameworks. The synthesis of the crystalline aluminosilicate materials with tunable mesoporosity and strong acidity has potentially important technological implications for catalytic reactions of large molecules, whereas conventional mesoporous materials lack hydrothermal stability and acidity.

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Figure 1: Electron microscopic investigation on the formation of mesoporous MFI zeolite.
Figure 2: Powder XRD patterns for the products precipitated after various reaction times, during hydrothermal synthesis of mesoporous MFI zeolite at 150 ∘C.
Figure 3: Pore structure analysis of the products precipitated after various reaction times during hydrothermal synthesis of mesoporous MFI zeolite at 150 ∘C.
Figure 4: Mesoporous MFI zeolites with tunable mesopore diameters.
Figure 5: Mesoporous LTA zeolite synthesized using [(CH3O)3SiC3H6N(CH3)2C16H33]Cl.

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Acknowledgements

This work was supported by the Ministry of Science and Technology through the Creative Research Initiative Program, and by the School of Molecular Science through the Brain Korea 21Project. Synchrotron radiation XRD was supported by Pohang Light Source. The authors are grateful to S. Bai, and I. Lee for helpful discussions on electron microscopy.

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  1. National Creative Research Initiative Center for Functional Nanomaterials and Department of Chemistry, Korea Advanced Institute of Science and Technology, Daejeon, 305-701, Korea

    Minkee Choi, Hae Sung Cho, Rajendra Srivastava, Chithravel Venkatesan, Dae-Heung Choi & Ryong Ryoo

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Correspondence to Ryong Ryoo.

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Choi, M., Cho, H., Srivastava, R. et al. Amphiphilic organosilane-directed synthesis of crystalline zeolite with tunable mesoporosity. Nature Mater 5, 718–723 (2006). https://doi.org/10.1038/nmat1705

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