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Naik A.D.,Ecole Nationale Superieure de Chimie de Lille | Fontaine G.,Ecole Nationale Superieure de Chimie de Lille | Samyn F.,Ecole Nationale Superieure de Chimie de Lille | Delva X.,Floridienne Chimie | And 2 more authors.
Polymer Degradation and Stability | Year: 2013

An integrated multicomponent molecule, Melamine-poly(aluminium phosphate) (Safire®200), its zinc and magnesium analogues namely Safire®400 and Safire®600 respectively were used as flame retardants for glass fiber reinforced polyamide 66 in combination with aluminium phosphinate. Characterisation, thermal stability, combustion properties, glow-wire flammability index and glow-wire ignition temperature and cone calorimetry results are reported. Lower threshold of loading of flame retardants that pass V0 rating in UL-94 vertical burning test have been determined. Effect of Zinc borate (Firebrake®500 grade) in these formulations was investigated. Influence of additives on endothermic and exothermic transitions of polyamide 66 in these formulations were studied by differential scanning calorimetry. The formulations were evaluated against the properties and fire performances of classical commercial combination of aluminium phosphinate and melamine polyphosphate. All the new formulations down to 15% of additives loading achieve V0 rating according to UL-94 protocol. This synergistic combination of additives significantly reduces the peak of heat release rate (pHRR) and total heat release (THR) in formulations exhibiting various degrees of intumescence. © 2013 Elsevier Ltd. All rights reserved. Source


Naik A.D.,Ecole Nationale Superieure de Chimie de Lille | Fontaine G.,Ecole Nationale Superieure de Chimie de Lille | Samyn F.,Ecole Nationale Superieure de Chimie de Lille | Delva X.,Floridienne Chimie | And 4 more authors.
Fire Safety Journal | Year: 2014

Glass-fiber reinforced polyamide 66 is flame retarded with a mixture of melamine-poly(zinc phosphate), (Safire®400) and diethyl aluminium phosphinate. The performance of this synergistic combination of additives is multi-modal and a comprehensive investigation is undertaken to elucidate the underlying flame retardancy mechanism. The strategy was to characterize the different chemical species responsible for flame retardancy that are generated in gas and condensed phases under different fire scenarios. Following heat release rate (HRR) curve of flame retarded polyamide formulations obtained by mass loss calorimeter, samples in different stages of degradation are collected and investigated. Further flame retardants and formulations were degraded in tubular furnace whose temperature protocol relied on thermal degradation profile obtained from thermogravimetric analysis (TGA). In either case, species generated in condensed phase were studied by solid state nuclear magnetic resonance spectroscopy (magic angle spinning (MAS) NMR; 27Al, 31P and 13C), Fourier transform Infra-red spectroscopy (FTIR), X-ray powder diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM), and optical microscopy, whereas TGA coupled FTIR, and pyrolysis gas chromatography mass spectrometry (Py/GC/MS) were utilised to investigate species released in gas phase. Flame retardancy mechanism is elaborated based on the identification of the chemical species in both gas and condensed phases and their specific contributing role. © 2014 Elsevier Ltd. Source


Naik A.D.,Ecole Nationale Superieure de Chimie de Lille | Fontaine G.,Ecole Nationale Superieure de Chimie de Lille | Samyn F.,Ecole Nationale Superieure de Chimie de Lille | Delva X.,Floridienne Chimie | And 4 more authors.
RSC Advances | Year: 2014

A higher analogue in the melamine polyphosphate family, melamine-poly(aluminium phosphate) (Safire®200), that has shown flame retardancy along with aluminium phosphinate in glass-fibre reinforced polyamide 66 was investigated to elucidate their mode of action. The mechanistic investigation is based on examining the chemical species formed in the condensed and gas phase under different fire scenarios. Samples at different stages of degradation were collected based on the heat release rate (HRR) curve of cone calorimetry and further analysed. Additionally, formulations and flame retardants were also pyrolysed at characteristic temperatures in a tubular furnace based on their thermogravimetric analysis (TGA) profile and investigated. A fire retardancy-quenching mechanism is mapped out on the basis of input from solid state nuclear magnetic resonance spectroscopy (MAS NMR; 27Al, 31P and 13C), Fourier transform Infra-red spectroscopy (FTIR), X-ray powder diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM), and optical microscopy on degraded samples. Gas phase analysis was studied by TGA coupled FTIR. © 2014 The Partner Organisations. Source

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