SOLID STATE OF NYLON66 STUDIED BY HIGH RESOLUTION SOLID STATE &lt;sup&gt;13&lt;/sup&gt;C NMR

Yamazaki, Shoko; Kimura, Tunehisa; Neki, Kazuya; Tamura, Nobuhiro

doi:10.2116/analsci.7.supple_1613

Cited by 3 publications

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“…Isotopic enrichment has been used to study a wide variety of polymer systems. Numerous solid-state NMR studies of nylon-6,6 polymers have been reported, , including several employing 2 H, 13 C, and 15 N stable-isotope labeling. − In this manuscript, we describe two different studies of nylon-6,6 that combine stable isotope enrichment and solid-state NMR detection. In the first study, we describe solid-state 15 N NMR characterization of nylon-6,6 heated in the presence of [ 15 N]BHMT, a molecule previously implicated in the formation of nylon gel. − These studies, designed to monitor the incorporation and subsequent reaction of BHMT in nylon-6,6, provide insights into the chemistry and reactivity of this triamine.…”

Section: Introductionmentioning

confidence: 99%

“…Isotopic enrichment has been used to study a wide variety of polymer systems. Numerous solid-state NMR studies of nylon-6,6 polymers have been reported, 17,18 including several employing 2 H, 13 C, and 15 N stableisotope labeling. [19][20][21][22] In this manuscript, we describe two different studies of nylon-6,6 that combine stable isotope enrichment and solid-state NMR detection.…”

Section: Introductionmentioning

confidence: 99%

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Monitoring Nylon-6,6 Thermochemistry by Solid-State NMR

et al. 1998

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Solid-state 13C and 15N NMR spectroscopy was used to study the structure and thermochemistry of nylon-6,6. Experiments were performed on samples of nylon-6,6 heated in the presence of labeled adipic acid and hexamethylenediamine (HMD) monomers as well as labeled bis(hexamethylenetriamine) (BHMT), a molecule previously implicated as a potential nylon cross-linker. The uptake and subsequent reaction of labeled materials were characterized by a variety of solid-state NMR techniques. Reaction of the central (α) nitrogen of BHMT to form an amide occurs very rapidly. With time, transamidation causes this position to become indistinguishable from the bulk amide nitrogen in nylon. Rotational-echo double resonance (REDOR), a solid-state NMR experiment that permits the quantitative measurement of 13C−15N labeled chemical bonds, was used to detect the formation and breaking of carbon−nitrogen bonds due to polymerization and transamidation. The reaction of adipic acid and hexamethylenediamine (HMD) and the transamidation reaction between the resulting oligomers and bulk nylon were studied by heating nylon-6,6 in the presence of [13C]adipic acid and [15N]HMD and characterizing the resulting polymers with REDOR. The combination of stable isotope labeling and NMR spectroscopy illustrated in this work should be applicable to the study of a wide variety of polymers.

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