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Thermal Decomposition Analysis of Spin-Coated Films of Partly Protected Polyvinylphenol with the t -Butoxycarbonyl Group Using Time-Resolved IR
Volume 51, Number 9 (Sept. 1997) Page 1352-1354
Tanimura, Sachiko; Kumada, Teruhiko; Ueyama, Akemi; Kobayashi, Junji; Kuramoto, Kazuo
Thermal decomposition of spin-coated films of partly protected polyvinylphenol with the t -butoxycalbonyl ( t BOC-PVP) group has been investigated by monitoring the intensity of the carbonyl stretching peak of the t BOC group by using temperature-variable time-resolved infrared spectroscopy (TR/IR). The temperature programming method has been used for determining the activation energy ( Ea ) of the thermal decomposition. We compared the thermal decomposition behavior of t BOC-PVP films with that of the powders and the behavior of a 22% protected t BOC-PVP film with that of a 66% protected t BOC-PVP film. It was found that the Ea of the 22% protected tBOC-PVP film is distinctively higher than the others including the result given from thermogravimetric analysis (TG). In addition, the Ea of the 22% protected t BOC-PVP film in creased up to 50 kcal/mol with the decrease of the remaining t BOC group, while the others were constant at 30 kcal/mol. Diglyme, which was used as the solvent in the 22% protected t BOC-PVP film, was residual after the temperature increased above 80 C, and the reaction velocity of the t BOC group increased in accordance with the generation of the OH group. These results suggest that the OH group, which accelerates the thermal decomposition of t BOC-PVP, is hindered by the residual solvent in the case of the 22% protected t BOC-PVP films.