Synthesis of silicalite-1 using a disiloxane-based structure-directing agent

Hirotaka Ishii, Keiji Itabashi, Tatsuya Okubo, Atsushi Shimojima*


研究成果: Article査読

4 被引用数 (Scopus)


A cationic organosiloxane compound where two tetrapropylammonium (TPA) cations are bridged by a tetramethyldisiloxane unit (MSi-TPA) has been used as a structure-directing agent (SDA) for the synthesis of a pure silica MFI-type zeolite, silicalite-1, with a unique microstructure and particle morphology. The hydrothermal treatment of the mixture of tetraethoxysilane as a silica source, MSi-TPAOH, and water yields solid products that are identified as silicalite-1 by X-ray diffraction and solid-state 29Si MAS NMR. Solid-state 29Si and 13C CP/MAS NMR and elemental analyses confirm that MSi-TPA is covalently incorporated in the MFI framework via cleavage of the disiloxane linkage. Compared with conventional silicalite-1 prepared with TPA cations, the amount of defect sites is higher, which can be attributed to the attachment of the organosilyl groups to the framework by Si-O-Si bonds. Scanning electron microscopic (SEM) observation shows spherical particle morphology that is quite different from the typical coffin-shaped crystals obtained with TPA. Importantly, MFI is not formed when triethoxysilyl- and diethoxysilyl-TPAs, instead of MSi-TPA, are used as SDAs under similar conditions, suggesting that the possible number of Si-O-Si linkages formed by SDAs greatly affects the crystallization process of MFI zeolite.

ジャーナルMicroporous and Mesoporous Materials
出版ステータスPublished - 2011 3月

ASJC Scopus subject areas

  • 化学 (全般)
  • 材料科学(全般)
  • 凝縮系物理学
  • 材料力学


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