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

Shosuke Kiba, Tetsuro Itagaki, Teruyuki Nakato, Kazuyuki Kuroda

Research output: Contribution to journalArticle

14 Citations (Scopus)

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.

Original languageEnglish
Pages (from-to)3202-3210
Number of pages9
JournalJournal of Materials Chemistry
Volume20
Issue number16
DOIs
Publication statusPublished - 2010 Apr 9

ASJC Scopus subject areas

  • Chemistry(all)
  • Materials Chemistry

Fingerprint Dive into the research topics of 'Interlayer modification of a layered H-octosilicate (H-RUB-18) with methanol: Formation of a highly ordered organosilicate nanohybrid'. Together they form a unique fingerprint.

  • Cite this