29Si-NMR study of hydrolysis and initial polycondensation processes of organoalkoxysilanes. I. Dimethyldiethoxysilane

Yoshiyuki Sugahara, Seigo Okada, Kazuyuki Kuroda, Chuzo Kato

    研究成果: Article

    68 引用 (Scopus)

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    The hydrolysis and initial polycondensation processes of dimethyldiethoxysilane (DMDES) have been investigated by high-resolution 29Si nuclear magnetic resonance spectroscopy (NMR) in a variety of acidic system (DMDES:ethyl alcohol:water:HCl = 1:4:x:y; x = 2 or 4, 1 × 10-5 ≤ y ≤ 1 × 10-2). On the basis of the behavior of signal intensities, those due to the following monomers and oligomers have been identified: Me2Si(OEt)(OH), Me2Si(OH)2, Me2(HO)SiOSi(OH)Me2, Me2(EtO)SiOSi(OH)Me2, Me2(EtO)SiOSiMe2OSi(OH)Me2, Me2(HO)SiOSiMe2OSi(OH)Me2, (Me2SiO)3, Me2(HO)SiO(SiMe2O)2Si(OH)Me2, and (Me2SiO)4 (where Me = CH3, Et = C2H5). It was shown that the substitution of the hydroxyl group for the ethoxy group resulted in an upfield shift of a signal, which was not consistent with the previous observations in tetra-functional alkoxysilane systems. In the course of the polycondensation process, cyclization reactions became predominant to form a considerable amount of the cyclic tetramer directly from the completely hydrolyzed dimer (Me2(HO)SiOSi(OH)Me2).

    元の言語English
    ページ(範囲)25-34
    ページ数10
    ジャーナルJournal of Non-Crystalline Solids
    139
    発行部数C
    DOI
    出版物ステータスPublished - 1992

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    magnetic resonance spectroscopy
    Polycondensation
    Nuclear magnetic resonance spectroscopy
    hydrolysis
    Hydrolysis
    nuclear magnetic resonance
    Cyclization
    oligomers
    Oligomers
    Hydroxyl Radical
    Dimers
    Ethanol
    ethyl alcohol
    Substitution reactions
    monomers
    Monomers
    dimers
    substitutes
    Water
    shift

    ASJC Scopus subject areas

    • Ceramics and Composites
    • Electronic, Optical and Magnetic Materials

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    title = "29Si-NMR study of hydrolysis and initial polycondensation processes of organoalkoxysilanes. I. Dimethyldiethoxysilane",
    abstract = "The hydrolysis and initial polycondensation processes of dimethyldiethoxysilane (DMDES) have been investigated by high-resolution 29Si nuclear magnetic resonance spectroscopy (NMR) in a variety of acidic system (DMDES:ethyl alcohol:water:HCl = 1:4:x:y; x = 2 or 4, 1 × 10-5 ≤ y ≤ 1 × 10-2). On the basis of the behavior of signal intensities, those due to the following monomers and oligomers have been identified: Me2Si(OEt)(OH), Me2Si(OH)2, Me2(HO)SiOSi(OH)Me2, Me2(EtO)SiOSi(OH)Me2, Me2(EtO)SiOSiMe2OSi(OH)Me2, Me2(HO)SiOSiMe2OSi(OH)Me2, (Me2SiO)3, Me2(HO)SiO(SiMe2O)2Si(OH)Me2, and (Me2SiO)4 (where Me = CH3, Et = C2H5). It was shown that the substitution of the hydroxyl group for the ethoxy group resulted in an upfield shift of a signal, which was not consistent with the previous observations in tetra-functional alkoxysilane systems. In the course of the polycondensation process, cyclization reactions became predominant to form a considerable amount of the cyclic tetramer directly from the completely hydrolyzed dimer (Me2(HO)SiOSi(OH)Me2).",
    author = "Yoshiyuki Sugahara and Seigo Okada and Kazuyuki Kuroda and Chuzo Kato",
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    T1 - 29Si-NMR study of hydrolysis and initial polycondensation processes of organoalkoxysilanes. I. Dimethyldiethoxysilane

    AU - Sugahara, Yoshiyuki

    AU - Okada, Seigo

    AU - Kuroda, Kazuyuki

    AU - Kato, Chuzo

    PY - 1992

    Y1 - 1992

    N2 - The hydrolysis and initial polycondensation processes of dimethyldiethoxysilane (DMDES) have been investigated by high-resolution 29Si nuclear magnetic resonance spectroscopy (NMR) in a variety of acidic system (DMDES:ethyl alcohol:water:HCl = 1:4:x:y; x = 2 or 4, 1 × 10-5 ≤ y ≤ 1 × 10-2). On the basis of the behavior of signal intensities, those due to the following monomers and oligomers have been identified: Me2Si(OEt)(OH), Me2Si(OH)2, Me2(HO)SiOSi(OH)Me2, Me2(EtO)SiOSi(OH)Me2, Me2(EtO)SiOSiMe2OSi(OH)Me2, Me2(HO)SiOSiMe2OSi(OH)Me2, (Me2SiO)3, Me2(HO)SiO(SiMe2O)2Si(OH)Me2, and (Me2SiO)4 (where Me = CH3, Et = C2H5). It was shown that the substitution of the hydroxyl group for the ethoxy group resulted in an upfield shift of a signal, which was not consistent with the previous observations in tetra-functional alkoxysilane systems. In the course of the polycondensation process, cyclization reactions became predominant to form a considerable amount of the cyclic tetramer directly from the completely hydrolyzed dimer (Me2(HO)SiOSi(OH)Me2).

    AB - The hydrolysis and initial polycondensation processes of dimethyldiethoxysilane (DMDES) have been investigated by high-resolution 29Si nuclear magnetic resonance spectroscopy (NMR) in a variety of acidic system (DMDES:ethyl alcohol:water:HCl = 1:4:x:y; x = 2 or 4, 1 × 10-5 ≤ y ≤ 1 × 10-2). On the basis of the behavior of signal intensities, those due to the following monomers and oligomers have been identified: Me2Si(OEt)(OH), Me2Si(OH)2, Me2(HO)SiOSi(OH)Me2, Me2(EtO)SiOSi(OH)Me2, Me2(EtO)SiOSiMe2OSi(OH)Me2, Me2(HO)SiOSiMe2OSi(OH)Me2, (Me2SiO)3, Me2(HO)SiO(SiMe2O)2Si(OH)Me2, and (Me2SiO)4 (where Me = CH3, Et = C2H5). It was shown that the substitution of the hydroxyl group for the ethoxy group resulted in an upfield shift of a signal, which was not consistent with the previous observations in tetra-functional alkoxysilane systems. In the course of the polycondensation process, cyclization reactions became predominant to form a considerable amount of the cyclic tetramer directly from the completely hydrolyzed dimer (Me2(HO)SiOSi(OH)Me2).

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