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The flammability and melt dripping of the widely used bio-based polyamide 11 (PA 11) have attracted much attention in the last decade, and they are still a big challenge for the fire science society. In this work, a novel single macromolecular intumescent flame retardant (AM-APP) that contains an acid source and a gas source was prepared by supramolecular reactions between melamine and p-aminobenzene sulfonic acid, followed by an ionic exchange with ammonium polyphosphate. The chemical structure of AM-APP was characterized by Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. AM-APP and TiO were then introduced into PA 11 by melt compounding to improve the fire resistance of the composite. The fire performance of PA 11 composites was evaluated by the limiting oxygen index (LOI), vertical burning (UL-94), and cone calorimetry tests. The results showed that the presence of 22% AM-APP and 3% TiO increased the LOI value from 22.2 to 29.2%, upgraded the UL-94 rating from no rating to V-0, completely eliminated melt dripping, and significantly decreased the peak heat release rate from 943.4 to 177.5 kW/m. The thermal behaviors were investigated by thermogravimetric (TG) analysis and TG-FTIR. It is suggested that AM-APP produces an intumescent char structure and releases inert gases, whereas TiO may consolidate the char layers, leading to the improvement in the fire resistance of PA 11.

An attractive intumescent flame retardant epoxy system was prepared from epoxy resin (diglycidyl ether of bisphenol A), low molecular weight polyamide (cure agent, LWPA), and ammonium polyphosphate (APP). The cured epoxy resin was served as carbonization agent as well as blowing agent itself in the intumescent flame retardant formulation. Flammability and thermal stability of the cured epoxy resins with different contents of APP and LWPA were investigated by limited oxygen index (LOI), UL-94 test, and thermogravimetric analysis (TGA). The results of LOI and UL-94 indicate that APP can improve the flame retardancy of LWPA-cured epoxy resins. Only 5 wt % of APP can increase the LOI value of epoxy resins from 19.6 to 27.1, and improve the UL-94 ratings, reaching V-0 rating from no rating when the mass ratio of epoxy resin to LWPA is 100/40. It is much interesting that LOI values of flame retardant cured epoxy resins (FR-CEP) increase with decreasing LWPA. The results of TGA, FTIR, and X-ray photoelectron spectroscopy (XPS) indicate that the process of thermal degradation of FR-CEP consists of two main stages: the first stage is that a phosphorus rich char is formed on the surface of the material under 5008C, and then a compact char yields over 5008C; the second stage is that the char residue layer can give more effective protection for the materials than the char formed at the first stage do. The flame retardant mechanism also has been discussed according to the results of TGA, FTIR, and XPS for FR-CEP.

The novel phosphorus/nitrogen-containing flame retardant hexa(phosphaphenanthrene aminophenoxyl)cyclotriphosphazene (HPAPC), which contains phosphaphenanthrene [9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO)] and phosphazene (hexachlorocyclotriphosphazene) groups, was synthesized by the classic Atherton−Todd reaction, and its chemical structure was characterized by Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopies. Poly(lactic acid) (PLA) composites containing HPAPC were prepared by melt blending, and their fire performance and thermal behaviors were investigated in terms of limiting oxygen index (LOI), vertical burning (UL-94), cone calorimeter tests, and thermogravimetric analysis (TGA). The LOI value could reach up to 34.7%, and UL-94 could pass V-0 for the PLA composite containing only 5 wt % HPAPC. TGA results showed that the char formation of PLA could be significantly improved by the presence of HPAPC. The evolved gas of the composite was analyzed by FTIR-TGA and pyrolysis−gas chromatography/mass spectrometry (Py−GC/MS). The dispersion of fillers in PLA was observed by back-scattered electron (BSE). The char morphology was characterized by FTIR spectroscopy and scanning electronic microscopy (SEM). It was suggested that the presence of HPAPC could release ammonia gas during combustion, which was beneficial to the formation of an intumescent char structure.

Polyethylene (PE) was treated with various formulations containing an intumescent fire retardant, which consists of melamine phosphate (MP), pentaerythritol (PER) and ammonium polyphosphate (APP), and one or none of following metal chelates: CuSAO, CoSAO and NiSAO. The behaviour of this intumescent system can be enhanced significantly by the addition of small amounts (0.2%) of metal chelate (CuSAO, CoSAO and NiSAO). The thermal stabilization, burning behaviour and char formation of the fire retardant PE system have been investigated by TGA, LOI, UL-94 test, SEM and cone calorimetry. All formulations studied provide good fire retardant behaviour, with LOI ! 27.4 and UL-94 V-0 rating. TGA results present more complicated thermal decomposition behaviour after the addition of small amounts (0.2%) of metal chelate when compared to that of PE-IFR. Cone calorimetry of PE-IFRemetal chelate (PE-IFReCuSAO, PE-IFReCoSAO and PE-IFRe NiSAO) shows a very significant decrease in HRR, PHRR, ML, THR and a very significant improvement of TTI compared to samples without metal chelate. Furthermore, SEM and photographs of the char layer show that the char layer from PE-IFRemetal chelate has a compact and tough char structure compared to the open porous char layer produced by sample without metal chelate.

In this manuscript, contradiction between the non-flammability and non-dripping of polyesters could be solved by copolymerizing terephthalic acid and ethylene glycol together with a pendent phenylethynyl-based monomer named 4-(phenylethynyl) di(ethylene glycol) phthalate (PEPE), which exhibited a cross-linkable nature at a proper temperature. TG-DSC simultaneous thermal analysis, FTIR, dissolution tests and rheological investigations proved the thermal cross-linking behavior of the copolyester, which was not active at the temperature of polymerization and processing but could crosslink rapidly at higher temperature before burning. LOI tests, cone calorimetry and small-scale flame tests further confirmed the self-extinguishment and inhibition for melt-dripping could be achieved through the cross-linking during burning, despite the absence of any flame-retardant element (say, bromine, chlorine, phosphorus, or nitrogen, etc.). Rheological analyses and the SEM microphotographs of the char showed P(ET-co-P)s exhibited a greater complex viscosity through the cross-linking at high temperature, leading to compact char residue, flame-retardant and anti-dripping effects.

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