FTIR and GCMS analysis of epoxy resin decomposition products feeding the flame during UL 94 standard flammability test. Application to the understanding of the blowing-out effect in epoxy/polyhedral silsesquioxane formulations
FTIR and GCMS analysis of epoxy resin decomposition products feeding the flame during UL 94 standard flammability test. Application to the understanding of the blowing-out effect in epoxy/polyhedral silsesquioxane formulations
复制标题
对 UL 94 标准可燃性测试期间燃烧火焰的环氧树脂分解产物进行 FTIR 和 GCMS 分析。
DOI：
10.1016/j.jaap.2018.08.026
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发表时间：
2018-06
影响因子：
6
通讯作者：
Rongjie Yang
中科院分区：
文献类型：
--
作者：
Wenchao Zhang;Alberto Fina;Giuseppe Ferraro;Rongjie Yang
开发了一种新颖的方法，用于在UL-94标准可燃性测试期间对聚合物分解产生的挥发物进行取样，从而允许收集、分离和分析在真实的燃烧条件下供给火焰的燃料混合物的精确组成。该系统在环氧树脂/多面体低聚倍半硅氧烷（POSS）上进行了验证，并发现对于理解先前称为“吹出效应”的阻燃机制非常有用。通过红外光谱和气相色谱/质谱分析收集的产物，以确定气体和液体分解产物，从而描绘环氧树脂的全面分解途径。轻质挥发物，在室温下为气态，表现出有限的差异作为DOPO-POSS的函数（用9，10-二氢-9-氧杂-10-磷杂菲-10-氧化物官能化的多面体低聚倍半硅氧烷），而液体产物的混合物证明相对浓度随DOPO-POSS的变化而显著变化。萘和甲苯，沿着观察到少量的几十种其它芳族产物。低浓度（2.5%）的DOPO-POSS的存在从根本上改变了芳香族挥发物混合物的组成，因为没有产生显著量的苯，而苯酚成为主要产物，占总量的约一半，异丙基苯酚和双酚A，沿着还有几十种较低浓度的其它产物。这种对供给火焰的燃料混合物的修改为该配方的较低可燃性以及吹出效应的现象学提供了解释。
A novel method was developed for the sampling of volatiles produced by polymer decomposition during UL-94 standard flammability tests, allowing collecting, separating and analyzing the precise composition of the fuel mixture feeding the flame in the real flaming conditions. The system was validated on epoxy resin/Polyhedral Oligomeric SilSesquioxanes (POSS) and found extremely informative for the understanding of the flame retardancy mechanisms previously referred to as the “blowing-out effect”. Collected products were analyzed by infrared spectroscopy and gas chromatography/mass spectroscopy, to identify the gaseous and liquid decomposition products, allowing depicting a comprehensive decomposition pathway for the epoxy resin. Lightweight volatiles, gaseous at room temperature, showed limited differences as a function of DOPO-POSS (polyhedral oligomeric silsesquioxane functionalized with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), whereas mixtures of liquid products evidenced for dramatic changes in the relative concentration as a function of DOPO-POSS. In pristine epoxy resin, the most abundant products were recognized as benzene, phenol, naphthalene and toluene, along with several tens of other aromatic products observed in lower amounts. The presence of DOPO-POSS at low concentration (2.5%) radically changes the composition of the aromatic volatiles mixture, as no significant amount of benzene is produced, while phenol becomes the main product, accounting for about half of the total, isopropyl phenol and bisphenol A, along with several tens of other products in lower concentrations. Such modification of the fuel mixture feeding the flame provided an explanation for the lower flammability of this formulation, as well as for the phenomenology of the blowing out effect.
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影响因子：
5.5
作者：
Liu, HZ;Zheng, SX;Nie, KM
通讯作者：
Nie, KM
DOI：
10.3390/ma3104710
发表时间：
2010-09-30
期刊：
Materials (Basel, Switzerland)
影响因子：
--
作者：
Schartel B
通讯作者：
Schartel B
影响因子：
3
作者：
Wenchao Zhang;Rongjie Yang
通讯作者：
Wenchao Zhang;Rongjie Yang
影响因子：
4.9
作者：
F. Feher;Shawn H. Phillips;J. Ziller
通讯作者：
F. Feher;Shawn H. Phillips;J. Ziller
影响因子：
5.9
作者：
Wenchao Zhang;Xiangmei Li;Lamei Li;Rongjie Yang
通讯作者：
Wenchao Zhang;Xiangmei Li;Lamei Li;Rongjie Yang