侧链改性的含磷阻燃聚丙烯腈的合成

Synthesis of Phosphorous-Containing Flame Retardant Side Chain Modified Polyacrylonitrile

以N,N'-二甲基甲酰胺为溶剂,将聚丙烯腈(PAN)制成一种侧链上具有高活性噁唑啉基团的改性聚丙烯腈(MPAN),并用傅里叶变换红外光谱(FTIR)、13C核磁共振光谱(NMR)对其结构进行了表征。通过13C NMR积分峰的强度计算得知,聚丙烯腈中大约33%的氰基发生了噁唑啉化反应。在生成的噁唑啉基团中,有1/4的基团在改性的过程中和乙醇胺发生副反应而开环。随后,将制得的MPAN和二苯基磷酸反应制得了侧链上含有磷的改性聚丙烯腈(PMPAN),并用FTIR、31P NMR对反应结果进行了表征。接着,用极限氧指数法(LOI)对PAN和PMPAN的燃烧行为进行了研究,结果显示:PMPAN中磷含量达2.1%时,PMPAN的LOI值为27%。

The modified polyacrylonitrile（MPAN） with oxazoline group in the side chain was prepared using N,N-Dimethyl formamide as solvent. The structure of MPAN was experimentally confirmed by Fourier transform infrared spectroscopy （FTIR） and carbon nuclear magnetic resonance spectroscopy （13C NMR）. 13C NMR and FTIR showed that 33 % cyan groups were turned into oxazoline group in this process, and they showed some 1/4 oxazoline rings were opened through reaction with ethanolamine. Then PMPAN was obtained after the reaction between MPAM and diphenylphosphate. The structure of PMPAN was characterized by FTIR and 31P NMR. Test results of LOI indicate that, when the P weight precentage in the modified PAN exceeded 2.1%, the PMPAN sample demonstrated LOI values 〉27 %.