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

doi:10.16085/j.issn.1000-6613.2019-1791

Abstract

Abstract:

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 (¹H 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.

Key words: DOPO derivative, polybutylene terephthalate, thermoplastic polyurethane, composites, thermal stability

摘要：

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。

关键词: DOPO衍生物, 聚对苯二甲酸丁二醇酯, 热塑性聚氨酯, 复合材料, 热稳定性

CLC Number:

TQ327.8

Jiyong LUO, Daohai ZHANG, Mi ZHOU, Qin TIAN, Shuhao QIN. Preparation and properties of PBT/TPU/DOPO-MA flame retardant composites[J]. Chemical Industry and Engineering Progress, 2020, 39(8): 3221-3229.

罗继永, 张道海, 周密, 田琴, 秦舒浩. PBT/TPU/DOPO-MA阻燃复合材料的制备及性能[J]. 化工进展, 2020, 39(8): 3221-3229.

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