以季戊四醇双磷酸酯二膦酰氯(SPDPC)和1,2-环己二胺(DACH)为原料,合成一种磷-氮阻燃固化剂——聚-1,2-环己二胺季戊四醇双磷酸酯(PDASP),通过傅里叶变换红外光谱仪、电喷雾电离质谱仪和热重分析仪对其结构和热性能进行了表征。以PDASP和4,4′-二氨基二苯砜(DDS)为固化剂对环氧树脂(E-44)进行固化并制备了不同磷含量的阻燃环氧树脂复合材料。通过极限氧指数(LOI)和UL-94垂直燃烧测试复合材料的阻燃性能,用热重分析仪和扫描电子显微镜对复合材料的热性能、残炭形貌及冲击断面进行了研究。结果表明:每100g E-44中PDASP用量为25g时(磷质量分数为2.30%),复合材料的LOI可达28.4%且通过UL-94 V0级测试,其拉伸强度和冲击强度分别达到43.5MPa和4.8kJ/m2;随着PDASP添加量的增加,复合材料的残炭率显著增加。通过扫描电子显微镜观察复合材料燃烧后残炭表面形貌,发现复合材料表面形成致密的炭层且明显发泡,表明PDASP的阻燃固化性能良好。
A phosphorus-nitrogen flame retardant curing agent poly-1,2-cyclohexanediamine pentaerythritol diphosphate (PDASP) was synthesized from pentaerythritol diphosphosphate chloride (SPDPC) and 1,2-cyclohexanediamine (DACH).The structure and thermal properties were characterized by fourier transform infrared spectrometer,electrospray ionization mass spectrometry and thermogravimetric analyzer.The epoxy resin (E-44) was cured with PDASP and DDS (4,4′-diaminodiphenylsulfone) as curing agent,and the flame retardant epoxy resin(EP) composite with different phosphorus content was prepared.The flame retardancy of the composite was tested by limit oxygen index (LOI) and UL-94 vertical combustion.The thermal properties,carbon residue morphology and impact section of the composite were studied by thermogravimetry and scanning electron microscope.The results shown that the LOI of the composite can reach 28.4% when 25g PDASP added to 100g E-44 (the content of phosphorus was 2.30%).The tensile strength and impact strength of the sample reached 43.5MPa and 4.8kJ/m2 respectively by UL-94 V0 test.With the increase of the content of PDASP,the carbon residue rate of the composite increased significantly.The morphology of the carbon residue after combustion of the composite was observed by scanning electron microscope.It was found that the carbon layer on the surface of the composite was dense and foamed obviously,indicating that the flame retardant and curing performance of PDASP was excellent.
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基金资助
沈阳科技计划2017项目(17-9-6-00)
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