通过苯基磷酰二氯、香草醛和4-氨基苯酚制备一种含磷席夫碱阻燃剂PH-VAN-AP。采用红外光谱、核磁共振氢谱和核磁共振磷谱表征PH-VAN-AP的结构。通过垂直燃烧、极限氧指数和锥形量热测试分析了环氧树脂的阻燃性能。利用热失重和差热扫描量热分析了环氧树脂的热稳定性、热降解过程及玻璃化转变温度(Tg)。结果表明,制备的PH-VAN-AP为预期结构。PH-VAN-AP能抑制环氧树脂的燃烧滴落与烟雾产生,在气相和凝聚相中发挥阻燃作用。当阻燃剂PH-VAN-AP的质量分数为5%时,阻燃环氧树脂的氧指数值从24.7%提高到35.4%,峰值热释放速率(pHRR)、总热释放(THR)及总烟雾释放(TSP)分别降低了165kW/m2、5MJ/m2和1.2m2,使其残留量提高9.6%。PH-VAN-AP能够提高环氧树脂的Tg,含5%PH-VAN-AP的环氧树脂的Tg从156.9℃提高到162.9℃。
A phosphorus-containing Schiff base flame retardant,PH-VAN-AP,was prepared from phenylphosphonic dichloride,vanillin and 4-aminophenol.The structure of PH-VAN-AP was characterized by FT-IR,1H-NMR and 31P-NMR.The flame retardant properties of epoxy resin (EP) were analyzed by vertical burning,limiting oxygen index and cone calorimeter tests.The thermal stability,thermal degradation process and glass transition temperature (Tg) of the EP were analyzed by TG and DSC tests.The results showed that the prepared PH-VAN-AP had the expected structure.PH-VAN-AP was able to inhibit combustion dripping and smoke generation of EP,and played the flame-retardant role in gas phase and condensed phase.The loading of 5 wt% PH-VAN-AP made the LOI value of the EP increase from 24.7% to 35.4%,and the peak heat release rate,total heat release and total smoke production reduced by 165kW/m2,5MJ/m2 and 1.2m2,respectively,and increased its residual amount by 9.6wt%.PH-VAN-AP could improve the Tg of EP,and the Tg of EP with 5 wt% PH-VAN-AP increased from 156.9℃ to 162.9℃.
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