Bestimmung von sekundären aminogruppen als fehlstrukturen‐in polyamid‐6.6

Horbach, A.; Alewelt, Wolfgang; Müller, H.

doi:10.1002/macp.1985.021861214

Cited by 4 publications

(2 citation statements)

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“…Cross-linking chemistries associated with amine-containing cyclopentanones and BHMT have been investigated with a variety of analytical methodologies, − but many mechanistic questions remain regarding the incorporation and distribution of cross-linkers formed during thermal degradation and the formation of other species via transamidation. New insight into both of these topics is provided in the present study via solid-state NMR characterization of nylon-6,6 thermally degraded in the presence of stable isotope-labeled reagents.…”

Section: Introductionmentioning

confidence: 99%

“…Of the potential cross-linkages identified to date, most experimental evidence points to two species; amine-containing cyclopentanone (derived from cyclization of adipic acid) and bis(hexamethylenetriamine) (BHMT), as key cross-linkers. [4][5][6] Cross-linking chemistries associated with aminecontaining cyclopentanones and BHMT have been investigated with a variety of analytical methodologies, [7][8][9][10] but many mechanistic questions remain regarding the incorporation and distribution of cross-linkers formed during thermal degradation and the formation of other species via transamidation. New insight into both of these topics is provided in the present study via solidstate NMR characterization of nylon-6,6 thermally degraded in the presence of stable isotope-labeled reagents.…”

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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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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

et al. 1998

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Thermal Degradation Kinetics of Nylon 66: Experimental Study and Comparison with Model Predictions

Schaffer

McAuley

Marchildon

et al. 2007

Macro Reaction Engineering

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An experimental investigation of nonoxidative thermal degradation kinetics of nylon 66 melt under high temperature (280–300 °C) and low water content (0.02–0.14 wt.‐%) conditions is presented. Experimental data for the time evolution of polymer end‐group concentrations and degradation‐product generation rates were compared with the predictions of the only published kinetic model. The omitted influence of water content is a plausible partial explanation for the considerable discrepancy between model predictions and some data. Several previously unreported or unquantified degradation products were identified and measured. Potential additional reactions to account for these results in future kinetic models are proposed.magnified image

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