Investigation of the decomposition pathway of polyamide 6/ammonium sulfamate fibers

Coquelle, Mathieu; Duquesne, Sophie; Casetta, Mathilde; Sun, Jun; Zhang, Sheng; Bourbigot, Serge

doi:10.1016/j.polymdegradstab.2014.02.007

Cited by 50 publications

(46 citation statements)

References 13 publications

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“…This allows determining the minimum concentration of oxygen (in vol%) in a nitrogen/oxygen mixture that is required for the combustion of a material in vertical position ignited at the top. LOI was measured on samples of 100 × 10 × 3 mm 3 , and the values are repeatable within ±1 vol%. UL 94 tests were performed on a Fire Testing Technology equipment using barrels of 127 × 12.7 × 1.6 mm 3 , in accordance with the recommendations of the standard [8].…”

Section: Fire Testing Methodsmentioning

confidence: 96%

“…It was shown that this compound was active at very low loadings (<5 wt%). More recently, ammonium sulfamate was effectively added to PA6 fibers to improve their fire behavior; however, it was shown that the FR loadings and processing parameters might be issues regarding the matrix degradation, because of the high temperature usually involved in PA6 processing [3]. This was attributed to the release of ammonia from AS, leading to aminolysis of the PA6 during processing.…”

Section: Introductionmentioning

confidence: 99%

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Flame Retardancy of PA6 Using a Guanidine Sulfamate/Melamine Polyphosphate Mixture

et al. 2015

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Polyamide 6 (PA6) is a widely-used polymer that could find applications in various sectors, including home textiles, transportation or construction. However, due to its organic nature, PA6 is flammable, and flame-retardant formulations have to be developed to comply with fire safety standards. Recently, it was proposed to use ammonium sulfamate as an effective flame retardant for PA6, even at low loading content. However, processing issues could occur with this additive considering large-scale production. This paper thus studies the use of another sulfamate salt-guanidine sulfamate (GAS)-and evidences its high efficiency when combined with melamine polyphosphate (MPP) as a flame retardant for PA6. A decrease of the peak of the heat release rate by 30% compared to pure PA6 was obtained using only 5 wt% of a GAS/MPP mixture in a microscale calorimeter. Moreover, PA6 containing the mixture GAS/MPP exhibits a Limiting Oxygen Index (LOI) of 37 vol% and is rated V0 for the UL 94 test (Vertical Burning Test; ASTM D 3801). The mechanisms of degradation were investigated analyzing the gas phase and solid phase when the material degrades. It was proposed that MPP and GAS modify the degradation pathway of PA6, leading to the formation of nitrile end-group-containing molecules. Moreover, the formation of a polyaromatic structure by the reaction of MPP and PA6 was also shown. OPEN ACCESSPolymers 2015, 7 317

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Section: Fire Testing Methodsmentioning

confidence: 96%

Section: Introductionmentioning

confidence: 99%

Flame Retardancy of PA6 Using a Guanidine Sulfamate/Melamine Polyphosphate Mixture

et al. 2015

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“…Thanks to the epoxy resin, the whey protein is immobilized in a stable position for analysis. The samples studied in this article are cross‐linked polymers; however, the experiment is also suitable for thermoplastics, such as polyamide‐6 for instance . Indeed, the voltage and intensity of the electron beam are low enough to avoid polymer degradation.…”

Section: Experimental Partmentioning

confidence: 99%

The electron microanalyzer (EPMA): a powerful device for the microanalysis of filled polymeric materials

Bellayer

Jimenez

Gardelle

et al. 2015

Polym. Adv. Technol.

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The electron probe microanalyzer is a device often used in the field of geology or in the glass and steel industries. However, it is barely known or used in the polymer field. Thus, in this paper, we investigate the use of electron probe microanalyzer for polymer microanalyses and compared it with a scanning electron microscope equipped with an energy dispersive spectrometer. To show the unique potential of this technique only develop in our lab for polymer application, three different samples were studied: (i) a fire protective epoxy-based coating submitted to aging in salt water, (ii) the distribution of organometallic catalysts into a thermal isolative silicone polymer, and (iii) the fouling growth of milk protein (biopolymer) on a stainless steel surface. Compared to an energy dispersive spectrometer, with an electron probe microanalyzer it is possible to quickly create X-ray mappings of low concentration elements at a good resolution, as well as allowing the interpretation of the mechanism of action for the three samples which was impossible using only an energy dispersive spectrometer because of its too low detection resolution. Copyright

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“…[10][11][12][13] Furthermore, some modified LDHs with intercalated flameretardant anions such as NO 2 3 and PO 32 4 enhance its flame retardancy. 14,15 Sulfamic acid (SA) and its derivatives have been documented for their flame retardancy in polymers, 16,17 and the synergistic flame retardancy of SA/MMT in PA6 has been reported by Lewin. 18,19 In this work, a novel sulfamic acid-intercalated MgAl-LDH (SA-LDH) was prepared.…”

Section: Introductionmentioning

confidence: 99%

Flame retardancy and thermal and mechanical performance of intercalated, layered double hydroxide composites of polyamide 11, aluminum phosphinate, and sulfamic acid

Zhang

Tang

Jiang

et al. 2016

J of Applied Polymer Sci

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Sulfamic acid-intercalated MgAl-layered double hydroxide (SA-LDH) was prepared and added with aluminum phosphinate (AlPi) into polyamide 11 (PA11). The results showed that AlPi/SA-LDH made a positive contribution to both flame retardancy and thermostability, and the effect was demonstrated with the limiting oxygen index (LOI), vertical burning tests (UL-94), cone calorimetry (CONE), and thermogravimetric analysis (TGA). The char morphologies were observed by SEM, and its chemical composition was investigated by Fourier transform infrared spectroscopy (FTIR). The decomposition mechanism was examined by TGA-FTIR. The results showed that the LOI of PA11 was only 23.0 and cannot pass any UL-94 rating. The addition of 20% AlPi increased the LOI to 31.5 and passed the UL-94 V-1 rating, and AlPi/SA-LDH 15%/5% increased the LOI to 32.4 and also passed the UL-94 V-1 rating. The CONE results revealed that 20% of either AlPi or AlPi/SA-LDH brought about a 30% decrease in the peak heat release rate (pHRR). The contribution of SA-LDH to flame behavior was especially reflected in the postponement of pHRR. SEM showed that the char morphologies became denser after SA-LDH incorporation. The improvement in thermal stability of the AlPi/SA-LDH combination was documented by TGA in both N 2 and air atmospheres. The mechanical performance deterioration caused by AlPi was partly improved by SA-LDH. The storage modulus (E 0 ) below the T g of AlPi/SA-LDH 15%/5% was about 300 MPa higher than with 20% AlPi. This was attributed to a compatibility improvement. The interaction forces among PA11, AlPi, and SA-LDH were probed by X-ray photoelectron spectrometry.

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Investigation of the decomposition pathway of polyamide 6/ammonium sulfamate fibers

Cited by 50 publications

References 13 publications

Flame Retardancy of PA6 Using a Guanidine Sulfamate/Melamine Polyphosphate Mixture

Flame Retardancy of PA6 Using a Guanidine Sulfamate/Melamine Polyphosphate Mixture

The electron microanalyzer (EPMA): a powerful device for the microanalysis of filled polymeric materials

Flame retardancy and thermal and mechanical performance of intercalated, layered double hydroxide composites of polyamide 11, aluminum phosphinate, and sulfamic acid

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