Solid state 13C and in situ 1H NMR study on the effect of melamine on the thermal degradation of a flexible polyurethane foam

C.M. Dick, C. Denecker, J.J. Liggat, M.H. Mohammed, Colin Snape, G. Seeley, C.I. Lindsay, B. Eling

Research output: Contribution to journalArticle

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Abstract

The aim of this investigation is to ascertain whether the mode of action of melamine in flexible polyurethane (PU) involves condensed phase chemistry in terms of promoting char formation. A combination of in situ 1HNMR analysis, solid state 13CNMR characterization of chars prepared ex situ, and normal TGA and DSC has been employed. Solid state 13CNMR indicates that there is no major discernible difference in the structure of the dichloromethane-insoluble chars prepared with and without melamine, the remaining polyol only accounting for 20-25% of the total carbon at 350°C, but still being quite mobile. However, in situ 1HNMR provides definitive evidence that melamine acts in the condensed phase in terms of promoting the formation of rigid char which forms in more significant quantity by 450°C. No increase in the residue yields is observed by TGA upon melamine addition, probably due to a combination of the small sample size and open sample holder in relation to the in situ 1HNMR analysis which also involves fairly slow heating.
LanguageEnglish
Pages1177-1182
Number of pages5
JournalPolymer International
Volume49
Issue number10
DOIs
Publication statusPublished - Oct 2000

Fingerprint

Melamine
Polyurethanes
Foams
Pyrolysis
Nuclear magnetic resonance
Methylene Chloride
Polyols
Dichloromethane
Carbon
Heating
melamine
polyurethane foam

Keywords

  • polyurethane
  • melamine
  • solid state (CNMR)-C-13
  • in situ (HNMR)-H-1
  • DSC
  • TGA

Cite this

Dick, C.M. ; Denecker, C. ; Liggat, J.J. ; Mohammed, M.H. ; Snape, Colin ; Seeley, G. ; Lindsay, C.I. ; Eling, B. / Solid state 13C and in situ 1H NMR study on the effect of melamine on the thermal degradation of a flexible polyurethane foam. In: Polymer International. 2000 ; Vol. 49, No. 10. pp. 1177-1182.
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abstract = "The aim of this investigation is to ascertain whether the mode of action of melamine in flexible polyurethane (PU) involves condensed phase chemistry in terms of promoting char formation. A combination of in situ 1HNMR analysis, solid state 13CNMR characterization of chars prepared ex situ, and normal TGA and DSC has been employed. Solid state 13CNMR indicates that there is no major discernible difference in the structure of the dichloromethane-insoluble chars prepared with and without melamine, the remaining polyol only accounting for 20-25{\%} of the total carbon at 350°C, but still being quite mobile. However, in situ 1HNMR provides definitive evidence that melamine acts in the condensed phase in terms of promoting the formation of rigid char which forms in more significant quantity by 450°C. No increase in the residue yields is observed by TGA upon melamine addition, probably due to a combination of the small sample size and open sample holder in relation to the in situ 1HNMR analysis which also involves fairly slow heating.",
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Solid state 13C and in situ 1H NMR study on the effect of melamine on the thermal degradation of a flexible polyurethane foam. / Dick, C.M.; Denecker, C.; Liggat, J.J.; Mohammed, M.H.; Snape, Colin; Seeley, G.; Lindsay, C.I.; Eling, B.

In: Polymer International, Vol. 49, No. 10, 10.2000, p. 1177-1182.

Research output: Contribution to journalArticle

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T1 - Solid state 13C and in situ 1H NMR study on the effect of melamine on the thermal degradation of a flexible polyurethane foam

AU - Dick, C.M.

AU - Denecker, C.

AU - Liggat, J.J.

AU - Mohammed, M.H.

AU - Snape, Colin

AU - Seeley, G.

AU - Lindsay, C.I.

AU - Eling, B.

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N2 - The aim of this investigation is to ascertain whether the mode of action of melamine in flexible polyurethane (PU) involves condensed phase chemistry in terms of promoting char formation. A combination of in situ 1HNMR analysis, solid state 13CNMR characterization of chars prepared ex situ, and normal TGA and DSC has been employed. Solid state 13CNMR indicates that there is no major discernible difference in the structure of the dichloromethane-insoluble chars prepared with and without melamine, the remaining polyol only accounting for 20-25% of the total carbon at 350°C, but still being quite mobile. However, in situ 1HNMR provides definitive evidence that melamine acts in the condensed phase in terms of promoting the formation of rigid char which forms in more significant quantity by 450°C. No increase in the residue yields is observed by TGA upon melamine addition, probably due to a combination of the small sample size and open sample holder in relation to the in situ 1HNMR analysis which also involves fairly slow heating.

AB - The aim of this investigation is to ascertain whether the mode of action of melamine in flexible polyurethane (PU) involves condensed phase chemistry in terms of promoting char formation. A combination of in situ 1HNMR analysis, solid state 13CNMR characterization of chars prepared ex situ, and normal TGA and DSC has been employed. Solid state 13CNMR indicates that there is no major discernible difference in the structure of the dichloromethane-insoluble chars prepared with and without melamine, the remaining polyol only accounting for 20-25% of the total carbon at 350°C, but still being quite mobile. However, in situ 1HNMR provides definitive evidence that melamine acts in the condensed phase in terms of promoting the formation of rigid char which forms in more significant quantity by 450°C. No increase in the residue yields is observed by TGA upon melamine addition, probably due to a combination of the small sample size and open sample holder in relation to the in situ 1HNMR analysis which also involves fairly slow heating.

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