1,4-二(4-苯氧基苯甲酰基)苯的合成与表征

该文采用亲核和亲电两种路线合成了1,4-二(4-苯氧基苯甲酰基)苯(Ⅱ)和1,3-二(4-苯氧基苯甲酰基)苯(Ⅲ)两种PEKK的小分子模型化合物,以Ⅱ和TPC缩聚,合成了全对位聚芳醚酮酮(p-PEKK),并用FT-IR1、H NMR、DSC、WAXD、SEM等技术对Ⅱ和Ⅲ以及PEKK的结构与性能进行了分析表征.研究表明:加入适量的Lewis碱以TPC和过量的DPE合成Ⅱ时,没有发现邻位结构及吨醇产物生成;Ⅱ为片状结晶,WAXD分析显示:2θ角10.76°,13.8°,17.5°,21°,38.7°,41.84°处出现尖的晶面衍射峰,p-PEKK在10.76°,13.8°,17.5°,21°,38.7°,41.84°处出现较宽的晶面衍射峰.说明Ⅱ的结晶较完整,当其作为PEKK大分子链的结构单元时虽能形成结晶,但结晶不完整,存在很多缺陷.

Synthesis and Characterization of 1,4-Bis (4-Phenoxybenzoyl) benzene

1,4-bis(4-phenoxybenzoyl)benzene was synthesized by nucleophilic and electrophilic substitution routes:(1)1,4-bis(4-chlorobenzoyl)benzene was obtained from chlorobenzene and terephthaloyl chloride(TPC).Then,the resulting compound DPOPKK was synthesized by 1,4-bis(4-chlorobenzoyl)benzene with natrium phenate,taking N-methyl-2-pyrrolidone(NMP) as solvent.(2) DPOPKK was synthesized by Friedel-Crafts acylation of terephthaloyl chloride(TPC) and excessive diphenylether(DPE) in 1,2-dichloroethane with aluminium trichloride(AlCl3) as catalyst.Its structure was characterized by FT-IR,1H NMR,Micromelting point apparatus,WAXD SEM and DSC etc.The results show that the compound is anticipated and has high purity.DPOPKK has the same crystalline diffraction peak as PEKK which is the unqiue crystallinaion characterization of PEKK.