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Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units

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Abstract

A mesostructured silica-based material was synthesized by self-assembly of a novel amphiphilic molecule consisting of a well-defined siloxane head with a double five-ring (D5R) structure and a hydrophobic alkyl tail. A precursor functionalized with ethoxy groups, C22H45Si10O15(OEt)9 (1), was hydrolyzed under an acidic condition with the retention of the D5R units, leading to the formation of two-dimensional (2D) hexagonal phase by evaporation-induced self-assembly of amphiphilic hydrolyzed molecules. Solid-state 29Si MAS NMR analysis of the resulting hybrid solid confirmed that the D5R units were cross-linked to form siloxane networks. Calcination of this hybrid solid gave mesoporous silica with high BET surface area (740 m2 g−1). These results expand the design possibility of silica-based materials at both molecular- and meso-scales, leading to the bottom up synthesis of hierarchically ordered materials.

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Acknowledgments

The authors are grateful to Prof. D. Mochizuki (Tokyo Institute of Technology), Dr. Y. Hagiwara, and Mr. R. Goto (Waseda University) for experimental help. This work was supported in part by the Elements Science and Technology Project of the Ministry of Education, Culture, Sports, Science and Technology (MEXT) of Japan, and a Waseda University Grant for Special Research Projects (No. 2009B-172). This work was performed under the Global COE program “Practical Chemical Wisdom”. The A3 Foresight Program “Synthesis and Structural Resolution of Novel Mesoporous Materials” supported by the Japan Society for the Promotion of Science (JSPS) is greatly appreciated.

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Authors and Affiliations

  1. Department of Chemical System Engineering, The University of Tokyo, Hongo-7, Bunkyo-ku, Tokyo, 113-8656, Japan

    Atsushi Shimojima

  2. Department of Applied Chemistry, Waseda University, Ohkubo-3, Shinjuku-ku, Tokyo, 169-8555, Japan

    Hideki Kuge & Kazuyuki Kuroda

  3. Kagami Memorial Laboratory for Materials Science and Technology, Waseda University, Nishiwaseda-2, Shinjuku-ku, Tokyo, 169-0051, Japan

    Kazuyuki Kuroda

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  1. Atsushi Shimojima
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  2. Hideki Kuge
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  3. Kazuyuki Kuroda
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Correspondence to Atsushi Shimojima or Kazuyuki Kuroda.

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Shimojima, A., Kuge, H. & Kuroda, K. Synthesis of mesostructured silica from monoalkyl-substituted double five-ring units. J Sol-Gel Sci Technol 57, 263–268 (2011). https://doi.org/10.1007/s10971-010-2224-7

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  • DOI: https://doi.org/10.1007/s10971-010-2224-7

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