S. Tanimura et al., THERMAL-DECOMPOSITION ANALYSIS OF SPIN-COATED FILMS OF PARTLY PROTECTED POLYVINYLPHENOL WITH THE T-BUTOXYCARBONYL GROUP USING TIME-RESOLVEDIR, Applied spectroscopy, 51(9), 1997, pp. 1352-1354
Thermal decomposition of spin-coated films of partly protected polyvin
ylphenol with the t-butoxycalbonyl (tBOC-PVP) group has been investiga
ted by monitoring the intensity of the carbonyl stretching peak of the
tBOC group by using temperature-variable time-resolved infrared spect
roscopy (TR/IR). The temperature programming method has been used far
determining the activation energy (E-a) of the thermal decomposition.
We compared the thermal decomposition behavior of tBOC-PVP films with
that of the powders and the behavior of a 22% protected tBOC-PVP film
with that of a 66% protected tBOC-PVP film. It was found that the E-a
of the 22% protected tBOC-PVP film is distinctively higher than the ot
hers including the result given from thermogravimetric analysis (TG).
In addition, the E-a of the 22% protected tBOC-PVP him increased up to
50 kcal/mol with the decrease of the remaining tBOC group, while the
others were constant at 30 kcal/mol. Diglyme, which was used as the so
lvent in the 22% protected tBOC-PVP him, was residual after the temper
ature increased above 80 degrees 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 therma
l decomposition of tBOC-PVP, is hindered by the residual solvent in th
e case of the 22% protected tBOC-PVP films.