Characterization of Silanol Groups in Protonated Magadiite by <sup>1</sup>H and <sup>2</sup>H Solid-State Nuclear Magnetic Resonance

Komori, Yoshihiko; Miyoshi, Manabu; Hayashi, Shigenobu; Sugahara, Yoshiyuki; Kuroda, Kazuyuki

doi:10.1346/ccmn.2000.0480604

Cited by 16 publications

(3 citation statements)

References 41 publications

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“…Signals at 3.7, 5.5, and 8.2 ppm were also observed and are ascribed to protons of silanol groups of H-magadiite. The signal at 8.2 ppm occurs at a higher frequency than those found for silanol groups in H-magadiite (3.8, 5.7 ppm) . These particular interlamellar silanol groups display a particularly strong hydrogen bonding.…”

Section: Resultsmentioning

confidence: 74%

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

et al. 2001

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Magadiite, a layered sodium polysilicate, was organically modified by esterification of interlayer silanol groups with various aliphatic alcohols. Methanol was directly reacted with H-magadiite (acid-treated magadiite) by refluxing. The methanol-treated product showed an increase in the basal spacing and the 13C NMR signals due to methyl groups. The 2H NMR spectrum of CD3OD-treated H-magadiite showed Pake doublet patterns of quadrupole coupling constants of 43 and 48 kHz and asymmetry factors of 0, indicating the fixation of the C−O axis. When aliphatic alcohols with the carbon chain length longer than 4 were used, an H-magadiite/N-methylformamide (NMF) intercalation compound was used as an intermediate for esterification. The basal spacing of butanol-treated H-magadiite was 1.40 nm, the value of which was smaller than that of H-magadiite/NMF (1.63 nm) and larger than that of H-magadiite (1.15 nm). 13C spin−lattice relaxation times (T 1) of butyl groups showed a low mobility of the α carbon. Other alcohols (C n H2 n +1OH (n = 2−16) and (CH3)3COH) were also reacted with the silanol groups. The differential thermal analysis (DTA) curves of the products showed exothermic peaks. The alkyl chains are apparently lying parallel to the inner surface because almost constant basal spacings were observed despite the variation in the alkyl chain length. The butanol-treated H-magadiite was dispersed in toluene and cast, resulting in the formation of a transparent nanocomposite film.

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Section: Resultsmentioning

confidence: 74%

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

et al. 2001

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“…). After referring to the literature, the peak with a chemical shift of 3.66 ppm was assigned to Zr–O–C H 2 – in the zirconium precursor. This peak eventually disappeared and a zirconium hydroxy peak with a chemical shift of 3.93 ppm gradually became more intense while the reaction mixture was heated under reflux for 96 h. The Z‐6040 trimethoxy peak with a chemical shift of 3.55 ppm also disappeared, but the Z‐6040 γ‐glycidoxypropyl peaks with chemical shifts between 2.5 and 3.8 ppm remained when the solvents were removed and the Zr–QR was obtained.…”

Section: Resultsmentioning

confidence: 99%

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

et al. 2015

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A liquid zirconium hybrid resin (Zr–QR) was synthesized through sol‐gel reactions of zirconium butoxide with silanol‐terminated polydimethylsiloxane (DMS‐S12) and γ‐glycidoxypropyltrimethoxysilane (Z‐6040). The sol‐gel reactions were monitored using Fourier transform infrared (FTIR) spectroscopy and proton nuclear magnetic resonance spectroscopy. The Zr–QR morphology was investigated using field emission transmission electron microscopy. The Zr–QR had a well‐ordered morphology and the dimensions were less than 5 nm. These properties were achieved because DMS‐S12 was used to separate the zirconium clusters and Z‐6040 was used to stabilize the Zr–QR. The acceleration of the curing reaction between silicone‐modified cycloaliphatic epoxy (SEP) and methylhexahydrophthalic anhydride (MHHPA) caused by the Zr–QR was investigated. Differential scanning calorimetry and FTIR spectroscopy investigations showed that the Zr–QR first reacted with MHHPA, producing chelating ligands and carboxylic acid. Unlike in the conventional method (adding acetic acid to cause non‐reactive chelating ligands to form), the carboxylic acid produced effectively accelerated the curing reaction between the SEP and MHHPA. The chelating ligand produced from the Zr–QR and MHHPA suppressed the gelation of the Zr–QR itself during the nanocomposite (SEP–Zr–QR) curing process. The cured SEP–Zr–QR nanocomposite exhibited excellent optical transmittance at visible wavelengths.© 2015 Society of Chemical Industry

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“…30,41 Alguns modelos estruturais tem sido propostos, usando a sua forma ácida e sódica, baseados na sua composição química, na difração de elétrons 41,42 , em análises na região do infravermelho (FT-IR) e em estudos baseados na ressonância magnética nuclear de 29 Si, 1 H e 23 Na. 43,44,45,46,47,48,49 Algumas destas propostas são:…”

Section: Estruturaunclassified

A formação da [Al]-magadiita, sua funcionalização e pilarização

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Aos meus pais pelo carinho e apoio irrestritos e inquestionáveis em minhas decisões. viii ix "Olho para trás e vejo aquela menina que queria entender tudo, com medo de que não coubesse tamanha quantidade de informação dentro de si. Coube e ainda cabe. E quanto mais entra, mais sobra espaço para a dúvida." AgradecimentosPrimeiramente, aos meus pais, Eunice e José, e ao meu irmão, Saulo, pela família que somos e por serem responsáveis pela minha essência, princípios e valores.À minha família que, mesmo sem entender direito o que eu faço, compreenderam os momentos de renúncia.Às mulheres que foram inspirações para escolha da minha profissão: Prof as Maria Tereza, Dieine e Carol.À Lolly pela contínua inspiração e exemplo de profissional. Por ter me recebido de braços abertos ao GPM 3 e me incentivado irrestritamente. Por todas as oportunidades de aprendizado proporcionadas, pelas inúmeras conversas científicas e pessoais. Que a amizade construída ao longo desses anos cresça juntamente com o decorrer de nossas carreiras.À Chiara, ao Giorgio e ao Léo por terem me recebido tão carinhosamente em seu grupo de pesquisa durante meu estágio na Itália.Aos meus amigos 'piemontesi', Daniele, Cesare, Jonathan, Giulia, Ilaria, Giuseppe, Francesco, Fabio e Mariana pela amizade construída, pelos inúmeros jantares e noites tipicamente italianas. Por terem feito da minha estadia em Alessandria uma experiência inesquecível.A minha querida amiga Thais, a Maceió, que me fez despertar para uma carreira muito promissora.Às minhas amigas Ju, Su, Suéllen e Bruna por sempre estarem ao meu lado, por compartilharem a casa, as risadas, as festas, os problemas.... as suas vidas.Ao Shima e ao Lucas pelo companheirismo de todas as horas, fossem elas de almoço ou não.xii Às irmãs que a vida me permitiu escolher, Mari e Meire. Por doarem seu tempo, pelas respostas honestas, pelo cuidado e zelo, pela torcida, por abraçarem minhas causas. Obrigada pela amizade forte e ao mesmo tempo leve.A todos os outros amigos por terem feitos desses anos em Campinas os mais felizes! Citá-los aqui renderia outra dissertação.Aos meus atuais amigos de trabalho: Sol, Karine, Aline, Eliane, Rômulo, Ramon, Marcos e Fafá pelos bons momentos dentro do GPM 3 . Aos antigos que passaram pelo grupo e deixaram suas marcas registradas: Tereza, Mathias, Jean, Carlinhos, Mendinho, Filipe e Rafael.À Érica pela amizade, paciência e ensinamentos desde que iniciei no grupo. Por me salvar a qualquer momento seja com um conselho ou até mesmo quando congelo oxigênio.Ao Ricardo, ex e futuro integrante do GPM 3 , amigo para todos os momentos. E quem diria, o veterano se tornou instantaneamente um grande amigo, um grande parceiro e exemplo de pesquisador.Ao Fábio Bonk pelas inúmeras medidas de RMN e intensas discussões científicas.Aos professores Italo e Daniela pelas contribuições valiosas durante a qualificação. Aos técnicos Anderson, Raquel, Daniel e Fabi pelas análises. Ao Pimpim pelas inúmeras vezes que me ajudou pacientemente com os gases, nitrogênio e afins. À Petrobras pela bolsa co...

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Characterization of Silanol Groups in Protonated Magadiite by ¹H and ²H Solid-State Nuclear Magnetic Resonance

Cited by 16 publications

References 41 publications

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

A formação da [Al]-magadiita, sua funcionalização e pilarização

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Characterization of Silanol Groups in Protonated Magadiite by 1H and 2H Solid-State Nuclear Magnetic Resonance

Cited by 16 publications

References 41 publications

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

Interlamellar Esterification of H-Magadiite with Aliphatic Alcohols

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

A formação da [Al]-magadiita, sua funcionalização e pilarização

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Characterization of Silanol Groups in Protonated Magadiite by ¹H and ²H Solid-State Nuclear Magnetic Resonance