Study of thermal properties of flame retardant epoxy resin treated with hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene
Study of thermal properties of flame retardant epoxy resin treated with hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene
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DOI：
10.1007/s10973-013-3151-y
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发表时间：
2013-04
影响因子：
4.4
通讯作者：
Jianzhong Xu;Z. He;Weihong Wu;Haiyun Ma;Jixing Xie;H. Qu;Y. Jiao
中科院分区：
文献类型：
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作者：
Jianzhong Xu;Z. He;Weihong Wu;Haiyun Ma;Jixing Xie;H. Qu;Y. Jiao
合成了Hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene(HHPCP)，并用傅立叶变换红外光谱、核磁共振氢谱和核磁共振31P谱对其进行了表征。采用极限氧(LOI)试验、水平火焰试验、烟密度试验(SDR)、热重分析(TG)和热重分析-质谱仪(TG-MS)研究了含HHPCP的环氧树脂(EP)的阻燃和热分解行为。用TG-MS和FTIR研究了HHPCP的分解过程。结果表明，当EP中加入质量分数为7.5%的HHPCP时，EP的LOI值由20.5提高到26.5%。在EP-7.5质量%HHPCP样品中加入质量分数为1%的纳米蒙脱土(NMMT)作为增效剂，可将EP-7.5质量%HHPCP-1质量%nMMT样品的LOI值从26.5%提高到27.5%。SDR测试表明，HHPCP对EP的抑烟效果不明显。热重分析表明，EP-7.5质量%HHPCP样品和EP-7.5质量%HHPCP-1质量%nMMT样品具有较高的热稳定性，与NEAT-EP相比，Tonset和Tmax增大。TG-MS结果表明，EP的主要热解产物为H2O、CO、CO2、C6H6、C6H5OH、HOC6H4CH3和可燃碳氢化合物碎片CxHy。与NEAT-EP样品相比，EP-7.5质量分数HHPCP样品的不可燃水汽含量增加，而CO2、可燃碳氢化合物碎片CxH和可燃气体CO含量降低。TG-MS和FTIR结果表明，HHPCP首先发生分子间脱水分解，然后在470℃和560℃分解HHPCP的P-N六原子环，少量含氮的无焰气体挥发到气相中。
Hexakis[p-(hydroxymethyl)phenoxy]cyclotriphosphazene (HHPCP) is prepared and characterized by FTIR,1H-NMR, and31P-NMR spectroscopy. Then an investigation of the flame retardancy, thermal decomposition behavior of epoxy resin (EP) containing HHPCP is carried out using limiting oxygen (LOI) test, horizontal flame test, smoke density rate (SDR) test, thermogravimetric analysis (TG), and thermal gravimetric analyzer-mass spectrometry (TG-MS). The decomposition process of HHPCP is studied by TG-MS and FTIR. The result shows that the LOI value of EP increase from 20.5 to 26.5 %, when 7.5 mass% HHPCP is added into EP. The addition of 1 mass% nano-montmorillonite (nMMT) into EP–7.5 mass% HHPCP sample as synergist can increase the LOI value of EP–7.5 mass% HHPCP–1 mass% nMMT sample from 26.5 to 27.5 %. The SDR test indicates that smoke suppression of HHPCP on EP is not significant. TG analysis reflects that the EP–7.5 mass% HHPCP sample and EP–7.5 mass% HHPCP–1 mass% nMMT show higher thermal stability properties with an increasingTonsetandTmaxcomparing with neat-EP. TG-MS result indicates that the main pyrolysis product of EP is H2O, CO, CO2, C6H6, C6H5OH, HOC6H4CH3, and flammable hydrocarbon fragments CxHy. Compared with neat-EP sample, nonflammable water vapor of EP–7.5 mass% HHPCP sample increased, whereas CO2and the flammable hydrocarbon fragments CxHyand flammable gas CO decreased. TG-MS and FTIR result suggests that HHPCP decomposed first by inter-molecular dehydration, then P–N hexatomic ring of HHPCP decomposed during 470 and 560 °C, and a little no-flame gas containing nitrogen element volatilized into the gaseous phase.