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  • 1
    ISSN: 1435-1536
    Keywords: Key words Time-resolved near infrared ; Two-dimensional correlation ; Perfluorooctyltri methoxysilane ; Condensation water, alcohol and silanol behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  The polymerization behavior of perfluorooctyltrimethoxysilane (PFOS) in ethanol, which is acid-catalyzed by 0.25 M HCl, has been examined using time-resolved near-IR and 2D near-IR correlation spectra. In the time-resolved near-IR spectra, the bands at 5164 and 4825 cm−1 have been assigned to the combination bands of water and ethanol OH groups, respectively. It has been found that the absorbance variation of the two near-IR bands occurs in a two-step process. The absorbance of the 5164 cm−1 band rapidly decreases in the initial step but increases exponentially in the second step, while that of the 4825 cm−1 band rapidly increases both in the initial step and, exponentially, in the second step. These results indicate that the time-dependent absorbance variation of the two near-IR bands reflects the polymerization process of PFOS, in which consumption and release of water molecules and release of methanol in the two-step process occur as a consequence of the acid-catalyzed hydrolysis of methoxy groups and the formation of silanols (SiOH) to form a siloxane bond. It has also been found that this polymerization process is distinctly reflected in the 2D near-IR correlation spectra.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1435-1536
    Keywords: Key words Time-resolved near-infrared ; Two-dimensional correlation ; 3-Aminopropyltriethoxysilane ; Condensation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The polymerization behavior of 3-aminopropyltriethoxysilane, a process initiated by water molecules, has been examined using time-resolved near-IR and 2D near-IR correlation spectra. By deconvolution of the time-resolved near-IR spectra, the existence of the component bands at 5189, 5265 and 5300 cm−1, whose intensities decrease markedly as the reaction proceeds, has been confirmed in the 5000–5400 cm−1 region. The band at 5189 cm−1 has been assigned to water molecules, while those at 5265 and 5300 cm−1 have been assigned to the strongly and weakly associated silanol groups, respectively. The kinetics of the hydrolysis of the ethoxy groups and of the formation of a siloxane bond have been analyzed using the time-dependent integral intensities of these three bands and the mechanisms of the reactions have been discussed. Evidence for this polymerization process is also clearly evident in the 2D near-IR correlation spectra.
    Type of Medium: Electronic Resource
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