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Kim, Sun-Ha;Han, Oc-Hee;Kim, Jong-Kil;Lee, Kwang-Ho
- Bulletin of the Korean Chemical Society
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- 제32권10호
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- pp.3644-3649
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- 2011
Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.
https://doi.org/10.5012/bkcs.2011.32.10.3644 인용 PDF KSCI

Gwon, O Yun;Park, Gyeong Won;Jeong, Sun Yeong
- Bulletin of the Korean Chemical Society
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- 제22권7호
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- pp.678-684
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- 2001
Porous silica-pillared montmorillonites were prepared by simultaneous intercalation of dodecylamine-TEOS [tetraethylorthosilicate, Si(OC2H5)4] into the H-montmorillonite and intragallery amine-catalyzed hydrolysis of TEOS. Mixtures of the H-montmorillonite, dodecylamine and TEOS at molar ratios of 1 : 2 : 15-30 and 1 : 2-6 : 20 resulted to swollen and viscous gel once at room temperature, allowing intercalation compounds which dodecylamine and TEOS were simultaneously intercalated into interlayer of H-montmorillonite. The hydrolysis of the gallery TEOS was conducted in water solution for 40 min at room temperature, affording siloxane-pillared H-montmorillonite. Calcination of samples at 500 $^{\circ}C$ in air resulted in silica-pillared montmorillonite with large specific surface areas between 403 and 577 m2 /g, depending on the reaction stoichiometry. The reaction at H-montmorillonite : dodecylamine : TEOS reaction stoichiometries of 1 : 2 : 15 and 1 : 4 : 20 resulted in high specific surface areas and mesopores with a narrow pore size distribution. Result indicates that the intragallery-amine catalyze the hydrolysis of gallery-TEOS and simultaneously have a role of gallery-templated micellar assemblies.
https://doi.org/10.5012/bkcs.2001.22.7.678 인용 PDF