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Sequential Reordering in Condensation Copolymers, 6. Average Block Lengths in Poly(ethylene terephthalate) – Polyamide 6 Copolymers As Revealed by NMR Spectroscopy
Author(s) -
Denchev Zlatan,
Kricheldorf Hans R.,
Fakirov Stoyko
Publication year - 2001
Publication title -
macromolecular chemistry and physics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.57
H-Index - 112
eISSN - 1521-3935
pISSN - 1022-1352
DOI - 10.1002/1521-3935(20010201)202:4<574::aid-macp574>3.0.co;2-v
Subject(s) - copolymer , polyamide , polymer chemistry , poly ethylene , ethylene , materials science , condensation , condensation polymer , nuclear magnetic resonance spectroscopy , chemistry , polymer , organic chemistry , composite material , catalysis , thermodynamics , physics
An equimolar physical blend comprising poly(ethylene terephthalate) (PET), polyamide 6 (PA6) and catalytic amounts of p ‐toluene sulfonic acid ( p TSA) was studied by differential scanning calorimetry (DSC) and 13 C NMR spectroscopy before and after reactive blending for various times at 280°C that enables interchange reactions. With the extension of the reaction time, DSC traces showed an abrupt decrease in ability to crystallize, and after two hours of blending the system did not reveal any crystallization or melting behavior. By means of 13 C NMR spectroscopy, a clear distinction was made between the PET/PA6 physical blend and the copolymers with different degrees of interchange reactions. The 13 C NMR sequence length determination in various PET–PA6 based copolyesteramides showed PET block lengths of 4–10 repeat units which was in good agreement with the crystallizability of these systems. A combination of selective degradation of the PET blocks and 1 H NMR allowed, for the first time, the characterization of both PET and PA6 sequence lengths. This method was shown to be more sensitive, as compared to 13 C NMR spectroscopy without selective degradation, for sequence analysis in copolymers with close to random distributions of PET and PA6 sequence lengths.