Synthesis of a phosphorus and sulfur-containing aromatic diamine curing agent and its application in flame retarded epoxy resins

Synthesis of a phosphorus and sulfur-containing aromatic diamine curing agent and its application in flame retarded epoxy resins
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含磷硫芳香二胺固化剂的合成及其在阻燃环氧树脂中的应用

DOI:
10.1002/fam.2252
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发表时间:
2015-08-01
期刊:
影响因子:
1.9
通讯作者:
Lin, Li
Lin, Li
中科院分区:
材料科学4区
文献类型:
--
作者:
Xu, Miaojun;Zhao, Wei;Lin, Li

文献摘要

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合成了一种新型的环氧树脂固化剂--双(3-氨基-2-噻吩基)苯基氧膦(ABTPPO),并用傅里叶变换红外光谱、核磁共振氢谱、碳谱和核磁共振谱对其进行了表征。以ABTPPO为阻燃固化剂,制备了一种新型的无卤阻燃EPO复合材料。用极限氧指数和垂直燃烧试验(UL-94)评价了ABTPPO固化EPO的阻燃性能,用锥形量热仪(CONE)和热重分析研究了其燃烧和热降解行为。当样品厚度为3.0 mm和1.6 mm时,固化的EPO复合材料分别通过了UL-94V-1和V-2级,极限氧指数达到38.3%。扫描电子显微镜测试表明,ABTPPO有利于在材料燃烧过程中在材料表面形成更致密、更均匀的炭层,保护底层基质不分解,提高材料的阻燃性能。固化后的EPO由于吸水率较低(0.6wt%),耐水性较好,说明阻燃EPO复合材料具有优良的耐水性能。版权所有(C)2014 John Wiley&Sons,Ltd.
A novel curing agent of epoxy resins (EPO), bis(3-amino-2-thienyl) phenylphosphine oxide (ABTPPO), was synthesized and characterized by Fourier transform infrared spectroscopy, H-1 nuclear magnetic resonance (NMR), C-13 NMR, and P-31 NMR. ABTPPO was used as a flame retardant curing agent, and a novel halogen-free flame retardant EPO composite was prepared. The flame retardant properties of ABTPPO-cured EPO were evaluated in terms of limiting oxygen index and vertical burning test (UL-94), while the combustion and thermal degradation behaviors were investigated by cone calorimeter test (CONE) and thermogravimetric analysis, respectively. The cured EPO composite passed the UL-94 V-1 and V-2 rating when the sample thickness is 3.0 and 1.6mm, respectively, and the limiting oxygen index value reached 38.3%. The morphological structures of char residue tested by scanning electron microscopy demonstrated that ABTPPO benefited to the formation of a more compact and homogeneous char layer on the materials' surface during burning, which protected the underlying matrix from decomposition and enhanced the flame retardancy of materials. The cured EPO showed excellent fire performance after the water resistance test because of the low water uptake (0.6wt%), which demonstrated that the flame retardant EPO composite possessed excellent water resistance property. Copyright (C) 2014 John Wiley & Sons, Ltd.