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Structural Analysis of Aromatic Liquid Crystalline Polyesters

1
Department of Chemistry and Biochemistry, University of Arizona, 1306 E University Blvd, Tucson, AZ 85721, USA
2
Solvay Advanced Polymers, 4500 McGinnis Ferry Rd., Alpharetta, GA 30005, USA
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Author to whom correspondence should be addressed.
Polymers 2011, 3(1), 367-387; https://doi.org/10.3390/polym3010367
Received: 21 December 2010 / Revised: 13 January 2011 / Accepted: 20 January 2011 / Published: 27 January 2011
(This article belongs to the Special Issue Liquid Crystalline Polymers)
Laboratory preparations of liquid crystalline prepolymers, distillates accompanying prepolymers, final polymers, and sublimates accompanying final polymers were examined. NaOD/D2O depolymerization of prepolymers and polymers back to monomers with integration of the 1H NMR spectra showed up to 6% excess of carboxyls over phenol groups, caused partly by loss of the low-boiling comonomer hydroquinone through distillation during prepolymerization and leaving anhydride units in the polymer chain. ESI MS and MS/MS of hexafluoroisopropanol extracts of the prepolymer detected small molecules including some containing anhydride groups; ESI+ MS showed the presence of small cyclic oligomers. 1H NMR (including TOCSY) spectra provided more quantitative analyses of these oligomers. The final polymerization increases the length of the polymer chains and sublimes out the small oligomers. Anhydride linkages remaining in the polymer must make LCP’s more susceptible to degradation by nucleophilic reagents such as water, alkalis, and amines. View Full-Text
Keywords: copolymerization; LCP’s; mass spectrometry; NMR; polyesters copolymerization; LCP’s; mass spectrometry; NMR; polyesters
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Hall, H.; Ahad, S.; Bates, R.; Bertucci, M.; Contreras, C.; Dospinoiu, A.; Lin, G.; Singletary, N.; Somogyi, A. Structural Analysis of Aromatic Liquid Crystalline Polyesters. Polymers 2011, 3, 367-387.

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