摘要以2,3,5,6-四氨基吡啶(TAP)三盐酸盐单体与2,5-二羟基对苯二甲酸(DHTA)单体为原料,在无氧条件下经由酸碱中和反应进行成盐,得到复合盐2,3,5,6-四氨基吡啶-2,5-二羟基对苯二甲酸盐(TD盐),再通过缩合聚合的方法制备高分子量的聚对苯撑吡啶并二咪唑(PIPD)。通过IR、NMR、MS、DSC等手段表征TD盐的结构及纯度,通过IR、相对粘度表征PIPD的结构与分子量。
以2,3-二氨基吡啶、水杨酸、2,5-二羟基对苯二甲酸(DHTA)和2,3,5,6-四氨基吡啶(TAP)为原料合成了3种模型化合物,并通过改变反应条件考察了温度和反应时间对生成2-邻羟苯基吡啶并咪唑(Mod1)的影响。通过MS、NMR、IR等表征模型化合物以及Mod1中间体的结构,结合理论知识初步对其成环机理进行了探索。5938
关键词 聚对苯撑吡啶并二咪唑 缩聚反应 模型化合物 成环机理
Title Synthesis and study of the Mechanism for poly {2,6-dimidazo[4,5-b:4’,5’-e]pridinylene-1,4(2,5-dihydroxy)phenylene}
Abstract
Compound salt of 2,3,5,6 -tereaaminopyridine-2 ,5-dihydroxy phthalate (TD salt) was synthesized with 2,3,5,6-tetraaminopyridine(TAP) hydrochloride and 2,5 - dihydroxy terephthalic acid (DHTA), through the acid-base neutralization reaction under anaerobic condition. PIPD was synthesized with TD salt by condensation polymerization method. IR, NMR, MS, DSC were used to study structure and purity of TD salt . Relative viscosity of PIPD was detected to konw molecular weight of PIPD.
2,3-diminopyridine, salicylic acid, DHTA and TAP were used for the synthesis of three kinds of model compounds. The influence of temperature and reaction time were investigated by changing the reaction conditions when ModⅠwas synthesized. Model compounds and the intermediate structure of ModⅠwere characterized by MS, NMR, IR. Combined with theoretical knowledge, the cyclization mechanism was explored.
Keywords PIPD condensation polymerization model compounds cyclization mechanism
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