High Surface Area, Thermally Stable, Hydrophobic, Microporous, Rigid Gels Generated at Ambient from MeSi(OEt)3 /(EtO)3 SiCH2 CH2 Si(OEt)3 Mixtures by F- -Catalyzed Hydrolysis

Joseph C Furgal; Honami Yamane; Timothy R Odykirk; Eongyu Yi; Yoshiki Chujo; Richard M Laine

doi:10.1002/chem.201704941

High Surface Area, Thermally Stable, Hydrophobic, Microporous, Rigid Gels Generated at Ambient from MeSi(OEt)₃ /(EtO)₃ SiCH₂ CH₂ Si(OEt)₃ Mixtures by F^- -Catalyzed Hydrolysis

Chemistry. 2018 Jan 2;24(1):274-280. doi: 10.1002/chem.201704941. Epub 2017 Nov 29.

Authors

Joseph C Furgal^{1

2}, Honami Yamane³, Timothy R Odykirk⁴, Eongyu Yi⁴, Yoshiki Chujo³, Richard M Laine^{4

5}

Affiliations

¹ Department of Chemistry, University of Michigan, Ann Arbor, MI, 48109, USA.
² Department of Chemistry & Center for Photochemical Sciences, Bowling Green State University, Bowling Green, OH, 43403, USA.
³ Department Polymer Chemistry, Kyoto University, Kyoto, Kyoto, 606-8501, Japan.
⁴ Department of Materials Science and Engineering, University of Michigan, Ann Arbor, MI, 48109, USA.
⁵ Department of Macromolecular Science & Engineering, University of Michigan, Ann Arbor, MI, 48109, USA.

PMID: 29053171
DOI: 10.1002/chem.201704941

Abstract

High surface area materials are of considerable interest for gas storage/capture, molecular sieving, catalyst supports, as well as for slow-release drug-delivery systems. We report here a very simple and fast route to very high surface area, mechanically robust, hydrophobic polymer gels prepared by fluoride-catalyzed hydrolysis of mixtures of MeSi(OEt)₃ and bis-triethoxysilylethane (BTSE) at room temperature. These materials offer specific surface areas up to 1300 m² g^-1 , peak pore sizes of 0.8 nm and thermal stabilities above 200 °C. The gelation times and surface areas can be controlled by adjusting the solvent volume (dichloromethane), percent fluoride (as nBu₄ NF or TBAF) and the BTSE contents. Polymers with other corners and linkers were also explored. These materials will further expand the materials databank for use in vacuum insulation panels and as thermally stable release and capture media.

Keywords: gels; high surface area; hydrolysis; materials chemistry; polymers.