PBT/TPU/DOPO-MA阻燃复合材料的制备及性能

Preparation and properties of PBT/TPU/DOPO-MA flame retardant composites

通过使用9,10-二氢-9-氧杂-10-磷朵菲-10-氧化物(DOPO)和马来酸酐反应合成制备DOPO衍生物阻燃剂DOPO-MA,并且其结构使用傅里叶红外光谱分析(FTIR)和核磁共振氢谱分析(1H NMR)技术进行表征。将阻燃剂与聚对苯二甲酸丁二醇酯(PBT)和热塑性聚氨酯(TPU)熔融共混以制备PBT/TPU/DOPO-MA阻燃复合材料。通过运用锥形量热、UL-94、极限氧指数(LOI)、热重分析(TGA)、差热分析(DSC)和力学测试,研究了阻燃剂对复合材料的性能影响。测试结果表明,PBT/TPU/DOPO-MA复合材料具有良好的阻燃性能,加入10%DOPO-MA后,LOI从23.2增加到31.6,可达到UL-94 V-1等级,热释放率峰值(PHRR)和最大成热辐射速率(MAHRE)值降低;热重分析测试结果表明,添加DOPO-MA可以使得阻燃复合材料的热稳定性有显著的提高,当加入10%DOPO-MA后,残炭量可从6.87增加到14.36。此外,随着DOPO-MA含量的增加,阻燃复合材料的结晶度可得到一定的提高。

The DOPO derivative flame retardant(DOPO-MA) was synthesized via the synthetic reaction of DOPO and maleic anhydride.Its structure was characterized through Fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance proton spectroscopy(1 H NMR) techniques.The flame retardant was melt-blended with polybutylene terephthalate(PBT) and thermoplastic polyurethane(TPU) for the synthesis of PBT/TPU/DOPO-MA flame retardant composite.The performance of flame retardants on composites was investigated based on cone calorimeter,UL-94,limiting oxygen index(LOI),thermogravimetric analysis(TGA),differential scanning calorimetry(DSC) and mechanical tests.The results showed that the PBT/TPU/DOPO-MA composite materials had good flame-retardancy performance.The LOI increased from 23.2 to 31.6 with additional 10% DOPO-MA,which could reach the UL-94 V-1 level.In addition,the decrease in peak heat release rate(PHRR) and the maximum heat radiation rate(MAHRE) was observed.The results based on thermogravimetric analysis revealed that the DOPO-MA introduced could improve the thermal stability of flame-retardant composites significantly.The amount of residual carbon increased from 6.87 to 14.36 with the addition of 10% DOPO-MA.Furthermore,the crystallinity of flame-retardant composites could be improved with the increase of DOPO-MA content.