共缩聚型可溶性耐高温聚芳酰胺合成与表征

Synthesis and properties of novel soluble heterocyclic polyamides

采用二胺1,2-二氢-2-(4-氨基苯基)-4-[4-(4-氨基苯氧基)-苯基]-二氮杂萘-1-酮(二胺A)、对苯二胺为共缩聚二胺单体,与对苯二甲酸在Yamazaki膦酰化法聚合体系中,选择直接缩聚法,成功得到高分子量的聚芳酰胺,其特性粘数为0.96～1.44 dL/g。以傅里叶变换红外光谱、核磁共振氢谱等分析手段研究了聚合物的结构,利用差示扫描量热法、热失重分析研究了聚合物的耐热性能。结果表明,该系列聚合物具有高的玻璃化转变温度(约为300℃),氮气氛中5%热失重温度在450℃以上;当二胺A与对苯二胺的物质的量比例为10∶0～5∶5时,所得聚合物溶解于强极性溶剂。同时,系统研究了影响聚合物特性粘数的诸多因素,从而确定了最佳工艺条件。

A series of new aromatic polyamides were synthesized by direct polycondensation of the l,2-dihydro-2-(4-aminophenyl)-4-[4-(4-aminophenonxyl)-phenyl]-phthalazin-l-one (diamine A) and p-phenylenediamine with terephthalic acid. The polymers with high molecular weight possessed inherent viscosities in the range of 0.96 - 1.44 dL/g. The structures of the polymers were characterized by Fourier transform infra-red spectrom-etry (FTIR) and nuclear magnetic resonance spectrometry (NMR); the heat resistance of the polymers was studied by differential scanning calorimetry and thermogravimetric analysis (TGA). The results showed that this series of polymers possessed glass transition temperatures of over 300 ℃ and 5% weight loss temperatures of over 450 ℃ in nitrogen atmosphere. When the mass ratio of diamine A to p -phenylenediamine reached 10 : 0 - 5 : 5, the resultant polymers were soluble in strong polar solvent. In addition, the factors effecting inherent viscosity of the polymers were examined systematically and the optimum process conditions were determined.