Bo Xu,Simiao Wei,Yanting Liu,Siheng Zhao,Lijun Qian
An organo-cobalt coordination complex (Co-H4APD), based on phosphonitrile-azacycles, was prepared by hydrothermal method . The flame retardancy, smoke suppression and thermal stability of epoxy (EP) composites were investigate by means of limited oxygen index (LOI), cone calorimeter test (CONE) and thermogravimetric analysis (TGA). The flame retardant modes of action of Co-H4APD in EP were confirmed by experiments, such as thermogravimetry-Fourier transform infrared spectroscopy-gas chromatograph/mass spectrometer (TG-FTIR-GC/MS), exploring condense and gas-phase products after composites pyrolysis or combustion. Results revealed that the introduction of 6 wt.% Co-H4APD increased LOI value to 29.8% and effectively suppressed heat/smoke release of EP composites. The synergistic charring effect of Co-H4APD improved the thermal stability and char-forming ability of composites. The char strength may be well-correlated with gas release for EP/Co-H4APD, conducive to form dense and regularly expanded char layer, with more phosphorus-rich graphitic structures and cross-linking structures catalyzed by cobalt ions . This high-quality char layer was regarded as the most critical side in improving the flame retardant and smoke suppression performance of EP composites. The gas-phase function of Co-H4APD should not be overlooked due to releasing phosphorous-based radicals during pyrolysis, exhibiting flame inhibition effect in gas phase. More efficient interactions between phosphazene and cobalt within one molecule unit of Co-H4APD contributed to its more obvious reduction of the combustion and smoke production than those of the physical mixing system of CoO + H4APD.
Hongda Chen,Jihui Wang,Aiqing Ni,Anxin Ding,Xia Han,Ziheng Sun
In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and1H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry–Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively.
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