Title :

Salen Complexes as Fire Protective Agents for Thermoplastic Polyurethane: Deep Electron Paramagnetic Resonance Spectroscopy Investigation

Author(s) :

Naik, Anil D. [Auteur]
Unité Matériaux et Transformations - UMR 8207 [UMET]
Bourbigot, Serge [Auteur]
Unité Matériaux et Transformations - UMR 8207 [UMET]
Bellayer, Séverine [Auteur]
Unité Matériaux et Transformations - UMR 8207 [UMET]
Touati, Nadia [Auteur]
Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE]
Ben Tayeb Meziane, Karima [Auteur]
Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE]
Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement (LASIRE) - UMR 8516
Vezin, Herve [Auteur]
Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE]
Fontaine, Gaelle [Auteur]
Ingénierie des Systèmes Polymères
Unité Matériaux et Transformations - UMR 8207 [UMET]

Journal title :

ACS Applied Materials & Interfaces

Abbreviated title :

ACS Appl. Mater. Interfaces

Volume number :

10

Pages :

24860-24875

Publisher :

American Chemical Society (ACS)

Publication date :

2018-06-29

HAL domain(s) :

Chimie
Chimie/Matériaux

English abstract : [en]

The contribution to flame retard thermoplastic polyurethane (TPU) of Copper complexes of Salen based Schiff bases N,N’-bis(salicylidene)ethylenediamine (C1), N,N’-bis(4- hydroxysalicylidene)ethylenediamine (C2) and ...
Show more >The contribution to flame retard thermoplastic polyurethane (TPU) of Copper complexes of Salen based Schiff bases N,N’-bis(salicylidene)ethylenediamine (C1), N,N’-bis(4- hydroxysalicylidene)ethylenediamine (C2) and N,N’-bis(5- hydroxysalicylidene)ethylenediamine (C3) is investigated in the context of minimizing TPU inherent flammability. Thermal and fire properties of TPU are evaluated. It is observed that fire performances vary depending upon the substitution of Salen framework. Cone calorimetry (MLC) results show that, in TPU at 10 wt.-% loading, C2 and C3 reduce peak of heat release (pHRR) by 46 and 50% respectively. At high temperature, these copper complexes undergo polycondensation leading to resorcinol type resin in the condensed phase and thus acting as intumescence reinforcing agents. C3 in TPU is particularly interesting since it delays significantly the time to ignition (MLC experiment). In addition, Pyrolysis combustion flow calorimetry (PCFC) shows reduction in HRR curve suggesting its involvement in gas phase action. Structural changes of copper complexes and radical formation during thermal treatment as well as their influence on fire retardancy of TPU in the condensed phase is investigated by spectroscopic studies supported by microscopic and powder diffraction studies. Electron paramagnetic resonance spectroscopy (EPR) was fully used to follow redox changes of Cu(II) ions as well as radical formation of copper complexes/TPU formulations in their degradation pathways. Pulsed EPR technique of Hyperfine Sublevel Correlation Spectroscopy (HYSCORE) reveals evolution of local surrounding of copper and radicals with strong contribution of nitrogen fragments in the degradation products. Further, spin state of radicals were investigated by 2D technique of Phase-inverted Echo-Amplitude detected Nutation (PEANUT) experiment. Two different radicals were detected i.e. one mono carbon radical and an oxygen biradical. Thus, the EPR study permits to deeply investigate the mode of action of copper salen complexes in TPU.Show less >

Language :

Anglais

Peer reviewed article :

Oui

Audience :

Non spécifiée

Collections :

• Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement (LASIRE) - UMR 8516
• Unité Matériaux et Transformations (UMET) - UMR 8207

Research team(s) :

Ingénierie des Systèmes Polymères
Propriétés magnéto structurales des matériaux (PMSM)

Submission date :

2019-03-25T15:43:47Z
2019-04-03T10:19:20Z
2019-11-19T14:30:34Z