4.5 Article

Interlayer Silylation of Layered Octosilicate with Organoalkoxysilanes: Effects of Tetrabutylammonium Fluoride as a Catalyst and the Functional Groups of Silanes

Journal

EUROPEAN JOURNAL OF INORGANIC CHEMISTRY
Volume 2021, Issue 19, Pages 1836-1845

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/ejic.202100050

Keywords

Layered compounds; Mesoporous materials; Organotriethoxysilane; Silylation; Tetrabutylammonium fluoride (TBAF)

Funding

  1. ANR [ANR-15-JTIC-0003-01]
  2. ANR (Agence Nationale de la Recherche)
  3. JST (Japan Science and Technology Agency) [ANR-15-JTIC-0003-01]
  4. JSPS
  5. DFG
  6. MEXT [18J22738]
  7. Agence Nationale de la Recherche (ANR) [ANR-15-JTIC-0003] Funding Source: Agence Nationale de la Recherche (ANR)
  8. Grants-in-Aid for Scientific Research [18J22738] Funding Source: KAKEN

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In this study, interlayer silylation of Na-Oct with various organoalkoxysilanes was conducted using C(16)TMA-Oct as an intermediate, with or without TBAF. The addition of TBAF increased the degree of silylation, possibly due to nucleophilic attack by F- ions. MPTES exhibited higher reactivity in silylation reactions, indicating better accessibility to the interlayer polar region of C(16)TMA-Oct.
Interlayer silylation of layered sodium octosilicate (Na-Oct) with various organoalkoxysilanes was conducted using hexadecyltrimethylammonium ion-exchanged layered octosilicate (C(16)TMA-Oct) as an intermediate in the presence or absence of tetrabutylammonium fluoride (TBAF). The degree of silylation was increased by adding TBAF. It is suggested that F- ions perform a nucleophilic attack on the alkoxysilanes, which promotes the silylation reaction. C(16)TMA-Oct was silylated with octyltriethoxysilane (C8TES) or 3-mercaptopropyltriethoxysilane (MPTES) to compare the reactivity of the two organoalkoxysilanes in the presence or absence of TBAF. A higher degree of silylation of C(16)TMA-Oct was observed with MPTES, suggesting the higher accessibility of this silylating agent into the interlayer polar region of C(16)TMA-Oct. Overall TBAF appears as a relevant catalyst for the covalent interlayer surface modification of layered silicates with organic functional groups.

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