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Solid-state NMR characterization of copolymers of nylon 11 and nylon 12

โœ Scribed by C.Gregory Johnson; Lon J Mathias


Book ID
104357832
Publisher
Elsevier Science
Year
1997
Tongue
English
Weight
141 KB
Volume
8
Category
Article
ISSN
0926-2040

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โœฆ Synopsis


Solid-state 13 C and 15 N NMR spectroscopy, in conjunction with differential scanning calorimetry, wide-angle X-ray diffraction and infrared spectroscopy, were used to characterize a series of nylon 11 and 12 copolymers with mole ลฝ . percentages of nylon 12 monomer of 0, 15, 35, 50, 65, 85, and 100%. Monotonic melting point T and heat of fusion m depressions were observed for the copolymer series with the 65 mol% nylon 12 copolymer having the lowest apparent crystallinity and T at 1488C. Solid-state 15 N NMR spectra showed a smooth shift of the main peak position for the m as-prepared copolymers from 84 ppm for the a-form of pure nylon 11 to 89 ppm for the g-form of pure nylon 12. Similar behavior was seen for FTIR amide V and VI modes which are also sensitive to the aand g-crystal forms. 13 C NMR T 1 measurements showed that the overall most mobile sample was the 65:35 copolymer. The amide group of the 1:1 copolymer was labelled using 15 N-labelled amino acids available through the Gabriel synthesis; an annealed, solution-cast film of this sample showed a T value of 349 s, similar to values seen for annealed nylon 11 and nylon 12 homopolymers. The WAXS 1N pattern for the 65 mol% nylon 12 sample showed a sharp peak at 2u s 21.3, overlapping a broad peak centered at 2u s 21.0.

ลฝ 15 . These are consistent with the values seen for g-form nylon 12. The 1:1 copolymer N labelled was shown to be polymorphic, like the homopolymers after specific treatments, with a g-like phase formed upon solvent casting, and an a-like phase dominating for as-polymerized material and precipitated flakes.


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