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研究了在N-甲基吡咯烷酮-氯化钙(NMP-CaCl_2)溶剂体系中,各种主要因素对对苯二甲酰氯(TPC)、间苯二甲酰氯(IPC)和对苯二胺(PPD)、间苯二胺(MPD)低温溶液共缩聚反应的影响。并对共聚物进行了红外光谱(IR)和热分析的测试及表征。实验结果表明,当间位苯基和对位苯基摩尔比(M/P)为3/7时,反应最佳条件是:单体摩尔浓度为0.40mol/L,反应起始温度5—12℃,CaCl_2用量为4%(wt%),反应搅拌时间15min以上,获得的聚合物对数比浓粘度(ηinh)≥2;当W/P=1/1时,单体浓度0.60mol/L,CaCL用量4—6%,反应起始温度为0—5℃,聚合物ηinh>1;M/P≥3/7,聚合物溶于反应体系。随着PPTA分子链中间位苯基组分(W/P)增加,所得聚合物的热稳定性降低,溶解度增加。
In this paper, the effects of various main factors on the crystallization of terephthalic acid (TPC), isophthalic acid chloride (IPC) and p-phenylenediamine (PPD) were studied in the solvent system of NMP-CaCl 2 ), M-phenylenediamine (MPD) low temperature solution copolycondensation reaction. The copolymer was tested and characterized by infrared spectroscopy (IR) and thermal analysis. The experimental results showed that when the molar ratio of meta to para phenyl was 3/7, the optimum reaction conditions were: the molar concentration of monomer was 0.40mol / L, the reaction initiation temperature was 5-12 ℃, the dosage of CaCl 2 was 4% (wt%) and the reaction time was more than 15min, the polymer had a logarithmic viscosity (ηinh) ≥2. When W / P = 1/1, the monomer concentration was 0.60mol / L 4-6% of CaCL, the initial reaction temperature is 0-5 ℃, the polymer ηinh> 1; M / P ≥ 3/7, the polymer is dissolved in the reaction system. As the phenyl component (W / P) in the meditope of PPTA increases, the thermal stability of the resulting polymer decreases and the solubility increases.