Issue 16, 2010
From the journal:

Journal of Materials Chemistry

Interlayer modification of a layered H-octosilicate (H-RUB-18) with methanol: formation of a highly ordered organosilicate nanohybrid†

Shosuke Kiba,acd   Tetsuro Itagaki,b   Teruyuki Nakatoc  and  Kazuyuki Kuroda*abd  

* Corresponding authors

a Department of Nano-Science and Nano-Engineering, Faculty of Science & Engineering, Waseda University, 3-4-1 Ohkubo, Shinjuku-ku, Tokyo, Japan
E-mail: kuroda@waseda.jp

b Department of Applied Chemistry, Faculty of Science & Engineering, Waseda University, 3-4-1 Ohkubo, Shinjuku-ku, Tokyo, Japan

c Graduate School of Bio-Applications and System Engineering, Tokyo University of Agriculture and Technology, 2-24-16 Naka-cho, Koganei-shi, Tokyo, Japan

d Kagami Memorial Research Institute for Materials Science and Technology, Waseda University, 2-8-26 Nishiwaseda, Shinjuku-ku, Japan

Abstract

Highly ordered silicate–organic nanohybrids were prepared by the modification of interlayer silanol groups of a layered polysilicic acid (H-octosilicate, H-RUB-18) with methanol. The grafting reaction was performed in a Teflon-lined stainless steel autoclave at 120 °C for various reaction periods. The grafting of methoxy groups onto the interlayer surface was evidenced by the downfield chemical shifts of the methyl groups in the solid state 13C NMR spectra and the exothermic DTA peaks with substantial weight losses due to combustion of methyl groups. The degree of modification with the methoxy groups was variable in the range between 0.42 and 0.95, depending on the reaction time. The retention of the layered silicate structure was proved by XRD and 29Si HD/MAS NMR. The structure was also analyzed by molecular mechanics force field calculation and Rietveld analysis, indicating the expansion of the silicate plane composed of the 54 cage with six-membered rings in the structure. This small structural distortion, caused by repulsion between the grafted methoxy groups, resulted in transformation of the crystal system from tetragonal to monoclinic. Hydrogen molecules were sorbed into the grafted products.

Graphical abstract: Interlayer modification of a layered H-octosilicate (H-RUB-18) with methanol: formation of a highly ordered organosilicate nanohybrid

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Article information

DOI
https://doi.org/10.1039/B915818A
Article type
Paper
Submitted
03 Aug 2009
Accepted
08 Feb 2010
First published
08 Mar 2010

J. Mater. Chem., 2010,20, 3202-3210

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Interlayer modification of a layered H-octosilicate (H-RUB-18) with methanol: formation of a highly ordered organosilicate nanohybrid

S. Kiba, T. Itagaki, T. Nakato and K. Kuroda, J. Mater. Chem., 2010, 20, 3202 DOI: 10.1039/B915818A

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