Enhanced mechanical and flame retardancy properties of vinyl ester resin systems with the synthesis of two flame retardants with vinyl group
Enhanced mechanical and flame retardancy properties of vinyl ester resin systems with the synthesis of two flame retardants with vinyl group
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DOI：
10.1002/pi.6062
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发表时间：
2020-07
影响因子：
3.2
通讯作者：
Xin Zhang;Weiwei Zhang;Wenchao Zhang;Rongjie Yang
中科院分区：
文献类型：
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作者：
Xin Zhang;Weiwei Zhang;Wenchao Zhang;Rongjie Yang
以1-氧磷杂-4-羟甲基-2，6，7-三氧杂双环[2.2.2]辛烷（PEPA）和9，10-二氢-9-氧杂-10-磷杂菲10-氧化物（DOPO）为原料，与甲基丙烯酸异氰基乙酯（MMA）反应，采用一锅法成功合成了两种乙烯基阻燃剂PEPABFR和DOPOBFR。通过傅立叶变换红外光谱、1H NMR和31 P NMR光谱以及基质辅助激光解吸电离飞行时间质谱确证了它们的结构。通过弯曲试验、差示扫描量热法、热重分析、极限氧指数（LOI）测定和锥形量热仪测试，研究了含15wt%合成阻燃剂体系的力学性能、热性能和阻燃性能。结果表明，改性后的复合材料的弯曲强度和弯曲模量有明显的提高。加入15wt%PEPABFR和15wt%DOPOBFR后，氧指数分别从纯乙烯基酯树脂（VER）的20.3%和30.7%提高到29.3%和30.7%。VER/PEPABFR和VER/DOPOBFR体系的峰值放热速率分别降低了16.9%和39.3%，总放热量分别降低了20.1%和36.4%。采用热重分析结合傅里叶变换红外光谱、扫描电子显微镜和X射线光电子能谱研究了阻燃剂的阻燃机理。© 2020化学工业学会
Two PEPA‐based (PEPABFR) and DOPO‐based (DOPOBFR) flame retardants with vinyl groups were synthesized successfully via 1‐oxyphospha‐4‐hydroxymethyl‐2,6,7‐trioxabicyclo[2.2.2]octane (PEPA) or 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene 10‐oxide (DOPO) with isocyanoethyl methacrylate using a one‐pot method. Their structures were confirmed using Fourier transform infrared,1H NMR and31P NMR spectroscopies and matrix‐assisted laser desorption ionization time‐of‐flight mass spectrometry. The mechanical performance, thermal properties and flame retardant performance of systems with 15 wt% synthetic flame retardants were investigated using bending tests, differential scanning calorimetry, thermogravimetric analysis, limiting oxygen index (LOI) measurements and cone calorimeter tests. The results show that the bending strength and flexural modulus are improved significantly. The LOI increases to 29.3% and 30.7% with incorporation to 15 wt% PEPABFR and 15% wt% DOPOBFR from the 20.3% corresponding to pure vinyl ester resin (VER). The peak heat release rate decreases by 16.9% and 39.3% and total heat release decreases by 20.1% and 36.4% for VER/PEPABFR and VER/DOPOBFR systems. Furthermore, the flame retardancy mechanism of the flame retardants was studied using thermogravimetric analysis coupled with Fourier transform infrared spectroscopy, scanning electron microscopy and X‐ray photoelectron spectroscopy. © 2020 Society of Chemical Industry