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- Title
Solid state polymerization in a micro-reactor: The case of poly(tetramethylene terephthalamide).
- Authors
Papaspyrides, Constantine D.; Porfyris, Athanasios D.; Vouyiouka, Stamatina; Rulkens, Ruud; Grolman, Eric; Poel, Geert Vanden
- Abstract
ABSTRACT The aim of this work was to develop and optimize a direct solid state polymerization (DSSP) process on a micro scale for alkyldiammonium-terephthalate salts. This was successfully demonstrated for the first time by the case of tetramethylenediammonium-terepththalate salt (4T salt). The derived polymer (PA4T) presents interesting properties, but the temperature-favored acid catalyzed cyclization of tetramethylenediamine (TMD) to mono-functional pyrrolidine and ammonia inhibits a high polymerization conversion. DSSP was performed in a thermogravimetrical analysis (TGA) chamber, and the continuously monitored weight loss was correlated to polymerization conversion via the release of water, excluding any mass and heat transfer limitations. It was found that the conditions under which the DSSP is performed and the morphology of the starting material affect both the reaction rate and the product quality. The effect of the critical process parameters, namely vent size, heating rate to reach SSP temperature, and reaction temperature were quantified by the observed mass loss and by 1H NMR analysis. It was noticed that, besides the water formed by amidation, other volatile compounds were also released during the DSSP reaction, with main component, the TMD. In particular, it was observed that conditions favoring the evaporation of TMD also favored a higher reaction rate. The TMD loss was minimized by optimization of the aforementioned process conditions, leading to a more thermally stable and a higher molecular weight final product. The thermal stability of the PA4T was found to be inversely correlated to the concentration of carboxylic end groups present in the formed polymer. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43271.
- Subjects
SOLID state chemistry; POLYMERIZATION; MICROREACTORS; CYCLOBUTANE; PHTHALAMIDES
- Publication
Journal of Applied Polymer Science, 2016, Vol 133, Issue 14, pn/a
- ISSN
0021-8995
- Publication type
Article
- DOI
10.1002/app.43271