NDLI: Highly functionalized bridged silsesquioxanes

Content Provider	SpringerLink
Author	Zhou, Guannan Simerly, Thomas Golovko, Leonid Tychinin, Igor Trachevsky, Vladimir Gomza, Yury Vasiliev, Aleksey
Copyright Year	2012
Abstract	The objective of this work was to synthesize functionalized mesoporous silsesquioxanes with high concentrations of amine groups. During typical sol–gel syntheses, these materials are obtained by co-condensation of organic precursors with suitable linkers, such as tetraethoxysilane, necessary to prevent the mesoporous structure from collapsing. Thus, concentrations of amine groups in organosilicas usually do not exceed 2.7–3.4 mmol g$^{−1}$. The use of bridged bis-trimethoxysilanes, however, allowed formation of mesoporous materials with no linker. Polycondensation of bis-trimethoxysilanes containing amine groups was conducted in acidic, neutral and basic media, resulting in high yields of solid bridged silsesquioxanes. Gelation occurred quickly if no acid or base was added to the reaction mixture. The hybrid organic/inorganic nature of obtained materials was confirmed by FT-IR and MAS CP NMR spectroscopy. Elemental analysis showed that amino group concentration in the products was 3.3–4.1 mmol g$^{−1}$. Measurement of particle size distribution confirmed that choice of reaction media significantly affects particle sizes and agglomeration degrees, with the largest agglomerates (up to 50 μm) formed in basic media. A morphology study, using small-angle X-Ray scattering, displayed two-level fractal structures composed of aggregated 6.5–10.5 nm particles. Reactions in the presence of a surfactant resulted in formation of mesoporous structures. Furthermore, the obtained bridged silsesquioxanes were thermally stable down to 260 °C, but could reversibly absorb water and CO$_{2}$ at temperatures below 120 °C. Thus, condensation of the bridged precursor without a linker resulted in formation of a highly functionalized mesoporous material.
Starting Page	470
Ending Page	482
Page Count	13
File Format	PDF
ISSN	09280707
Journal	Journal of Sol-Gel Science and Technology
Volume Number	62
Issue Number	3
e-ISSN	15734846
Language	English
Publisher	Springer US
Publisher Date	2012-04-13
Publisher Place	Boston
Access Restriction	Subscribed
Subject Keyword	Sol–gel synthesis Silsesquioxanes Mesoporous materials Microstructure Amine groups Optical and Electronic Materials Inorganic Chemistry Ceramics, Glass, Composites, Natural Methods Nanotechnology
Content Type	Text
Resource Type	Article
Subject	Biomaterials Electronic, Optical and Magnetic Materials Condensed Matter Physics Ceramics and Composites Materials Chemistry Chemistry

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1	Ministry of Education (GoI), Department of Higher Education	Sanctioning Authority	https://www.education.gov.in/ict-initiatives
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3	National Digital Library of India Office, Indian Institute of Technology Kharagpur	The administrative and infrastructural headquarters of the project	Dr. B. Sutradhar bsutra@ndl.gov.in
4	Project PI / Joint PI	Principal Investigator and Joint Principal Investigators of the project	Dr. B. Sutradhar bsutra@ndl.gov.in Prof. Saswat Chakrabarti will be added soon
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