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13C- and 1H-NMR and FTIR spectroscopic evidence for aggregate formation of organosilanes in toluene

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Abstract

Changes in the 13C and 1H NMR chemical shifts of the silane coupling agent (3-aminopropyltri-ethoxysilane, APTS) in toluene, which were detected as the concentration of APTS increased, have been interpreted in terms of the formation of micelles and the presence of a critical micelle concentration (CMC) equal to ca. 0.47 mol 1 -1. For the protons of the n-propyl segment, 1H NMR splitting patterns have been analyzed and conformations of the propyl segment have been discussed. Plots of relative absorbance of the two NH2 stretch IR bands at 3324 and 3384 cm -1 against concentration provided an inflection point (corresponding to the CMC) at a value equal to 0.46 mol 1 -1 Thus, consideration of the interaction of APTS with a surface must take into account the presence of both APTS aggregates as well as APTS monomers.

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Authors and Affiliations

  1. Maruyasu Industries Co., Ltd., Hashime-cho Kitayama 1, 444, Okazaki, Japan

    I. Shimizu

  2. Department of Applied Chemistry, Nagoya Institute of Technology Gokiso-cho, 466, Showa-ku, Nagoya, Japan

    H. Okabayashi, N. Hattori, K. Taga & A. Yoshino

  3. Department of Chemistry, The University of Auckland, Private Bag 92019, Auckland, New Zealand

    C. J. O’Connor

Authors
  1. I. Shimizu
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  2. H. Okabayashi
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  3. N. Hattori
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  4. K. Taga
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  5. A. Yoshino
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  6. C. J. O’Connor
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Shimizu, I., Okabayashi, H., Hattori, N. et al. 13C- and 1H-NMR and FTIR spectroscopic evidence for aggregate formation of organosilanes in toluene. Colloid Polym Sci 275, 293–297 (1997). https://doi.org/10.1007/s003960050084

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  • DOI: https://doi.org/10.1007/s003960050084

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