AB型改性PPTA新单体的合成与表征

针对聚对苯二甲酰对苯二胺(PPTA)聚合及硫酸中纺丝的不足,提出以增加酰胺类有机溶剂的溶解度,从合成改性基团―CH3在聚合物的分子链中均匀且完全有序排列的改性PPTA(M-PPTA)出发,创新研究了AB型M-PPTA新单体4-(4-氨基-2-甲基苯胺羰基)苯甲酸甲酯(MACB)的合成,考察了溶剂、反应时间、还原剂等对反应的影响,结果表明:采用以4-氨基-2′,3-二甲基偶氮苯(C.I.11160)和对甲氧羰基苯甲酰氯(MBC)为原料,先缩合合成中间体MDCB,后经铁粉还原工艺合成出的黄色结晶MACB,精制后的纯度和总收率分别达99%和70%以上,并经FT-IR、13 CNMR和MS等定性分析确认.合成过程已呈现工艺简练、操作安全以及原料价廉易得等特点.

Synthesis and characterization of AB-modified PPTA new monomer

To increase the concentration of poly(p-phenylene terephthalamide)(PPTA) polymerization and spinning,in this paper we proposed to increase the solubility of amide organic solvent,started from the synthesis of modifiedCH3 group arranged uniformly and fully ordered in the polymer chain of the modified PPTA(M-PPTA),a new AB-type M-PPTA monomer: methyl 4-((4-amino-2-methylphenyl)carbamoyl)benzoate(MACB) was synthesized.And the effects of solvent,reaction time,reducing agent on reaction were investigated.The experimental results showed that high-purity MACB,which was synthesized from 4-amino-2′,3-dimethyl-azobenzene(C.I.11160)and methoxycarbonyl benzoic chloride(MBC) as raw materials to synthesis the intermediate MDCB and followed by iron reduction process,was obtained with purity above 99% and overall yields of 70% after being refined.The MACB was identified by FT-IR,13C NMR and MS.And its appearance is yellow crystalline.The synthesis technology had some advantages such as simple procedure,safe operation,low cost and commercially available materials.