耐高温阻燃聚苯腈树脂的制备及性能

Preparation and Characterization of High-Temperature Flameresistant Phthalonitrile Resin

利用间苯二酚、双酚A和联苯二酚分别与4-硝基邻苯二甲腈发生亲核取代反应合成了3种耐高温苯腈单体,并利用4-氨基苯氧邻苯二甲腈为催化剂制备了3种聚苯腈树脂。采用红外光谱、核磁氢谱、差示扫描量热、热重分析、动态力学分析、扫描电镜、导热系数仪和X射线衍射分析表征了苯腈单体和半本征型聚苯腈树脂的结构与性能。结果表明,3种苯腈单体的熔点在180~226℃,加工温度窗口为40~75℃。所制备3种聚苯腈树脂的起始分解温度(Td5%)高于480℃,玻璃化转变温度高于335℃,极限氧指数(LOI)高于57,导热系数大于0.21 W/(m·K),表现出良好的加工性、优异的热稳定性、突出的阻燃性和良好的导热性能。

Three high-temperature phthalonitrile monomers were synthesized by the nucleophilic substitution reaction of resorcinol,bisphenol A and dihydroxybenzene with 4-nitrophthalonitrile,respectively.Three phthalonitrile resins were prepared using 4-aminophenoxy phthalonitrile as catalyst.The structures and properties of phthalonitrile monomers and resins were confirmed by infrared spectra,nuclear magnetic hydrogen spectrum,differential scanning calorimetry,thermogravimetric analysis,dynamic mechanical analysis,scanning electron microscopy,thermal conductivity analysis and X-ray diffraction.The results show that the melting points of three monomers are 180~226℃,and the processing temperature windows are about 40~75℃.The initial decomposition temperature(Td5%)of three phthalonitrile resins is higher than 480℃,the glass transition temperatures greater(Tg)than 335℃,the limited oxygen indexs(LOI)higher than 57 and the thermal conductivity greater than 0.21 W/(m·K).The polymers exhibit fine processability,excellent thermal stability,outstanding flame retardancy and good thermal conductivity.