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Low flammability and smoke epoxy resins with a novelDOPO-based imidazolone derivative

机译:低易燃性和烟雾环氧树脂与基于Noveldopo的咪唑酮衍生物

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摘要

In this work, a DOPO-based imidazolone derivative named DHI was synthesized using DOPO, 5-amino-2-benzimidazolinone and 4-hydroxybenzaldehyde as raw materials. The chemical structure of DHI was characterized by(1)H-NMR,P-31-NMR and Fourier transform infrared spectra (FTIR). Then, a series of different flame-retardant epoxy resin (EP) thermosets were prepared by mixing flame retardant DHI. The thermal properties of the cured EPs was investigated by thermogravimetry analysis (TGA) and differential scanning calorimeter (DSC), and the results showed the thermal stability and glass transition temperature (T-g) of the cured EP modified with DHI declined slightly compared with that of neat EP. The limited oxygen index (LOI) and UL94 test results exhibited DHI imparted good flame retardancy to EP. The EP-4 (phosphorus content of 1.25%) possessed a LOI value of 36.5% and achieved a V-0 rating. Furthermore, the peak of heat release rate (PHRR) and total heat release rate (THR) of EP-4 decreased by 38.7% and 24.5%, respectively. Excitedly, the total smoke production (TSP) of EP-4 sample declined by 62.5%, which meant DHI also made EP obtain excellent smoke suppression property. Moreover, the flame-retardant mechanism was studied by scanning electron microscopy (SEM) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). It was reasonable inferred that DHI could not only promote EP to form dense char layer in condensed phase, but also restrain combustion in gaseous phase through catching the free radicals sourced from the degradation of EP.
机译:本文以DOPO、5-氨基-2-苯并咪唑啉酮和4-羟基苯甲醛为原料,合成了一种基于DOPO的咪唑啉酮衍生物DHI。通过(1)H-NMR、P-31-NMR和傅里叶变换红外光谱(FTIR)对DHI的化学结构进行了表征。然后,通过混合阻燃剂DHI制备了一系列不同的阻燃环氧树脂(EP)热固性树脂。通过热重分析(TGA)和差示扫描量热仪(DSC)研究了固化EPs的热性能,结果表明,与纯EP相比,DHI改性EP的热稳定性和玻璃化转变温度(T-g)略有下降。极限氧指数(LOI)和UL94测试结果表明,DHI赋予EP良好的阻燃性。EP-4(磷含量为1.25%)的LOI值为36.5%,并达到V-0评级。此外,EP-4的热释放速率峰值(PHRR)和总热释放速率峰值(THR)分别降低了38.7%和24.5%。令人兴奋的是,EP-4样品的总发烟量(TSP)下降了62.5%,这意味着DHI也使EP获得了优异的抑烟性能。此外,通过扫描电子显微镜(SEM)和热解气相色谱/质谱(Py-GC/MS)研究了阻燃机理。可以合理推断,DHI不仅可以促进EP在凝聚相中形成致密的炭层,而且可以通过捕捉EP降解产生的自由基来抑制气相燃烧。

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