摘要
以二硫化碳为溶剂、无水三氯化铝作催化剂、对苯二甲酰氯与氟苯为反应原料,在20℃利用Friedel-crafts酰基化反应合成了产率为76.7%、纯度为99.758%的1,4-双(对氟苯甲酰)苯(P,P-BFB)。经IR、1HNMR和MS光谱对其结构分析,确定为P,P-BFB。以二苯砜为溶剂,在无水碳酸钾/碳酸钠的催化下,以P,P-BFB为单体与对苯二酚进行亲核取代反应合成了特性粘度为0.87的聚醚醚酮酮(PEEKK)。通过IR、DSC、TG和XRD对其结构与性能进行了表征,确定其结构为PEEKK;TG测试表明在氮气气氛下开始分解温度为557℃,且到1200℃时也没分解完全;DSC和XRD衍射图表明其为半晶态聚合物,且由DSC曲线可知其熔点Tm为367℃。
Synthesis of 1,4-bis （4-fluorbenzoyl）-benzene by reacting terephthaloyl chloride with fluoro- benzene by Friedel-crafts acylation reaction in the presence of aluminum chloride as the catalyst and CS2 as the solvent in 20℃. The yield was up to 76.7 % and purity was up to 99.75 % on the optimum conditions of the reac-tion. The struction that was analysed by IR,^1HNMRand MS was sure to P,P-BFB. Polyether ether ketone ketone was prepared by the nucleophilic reaction of hydroquinone with 1,4-bis （4-fluorbenzoyl）-benzene using diphe-nylsulfone solvents in the presence of anhydrous K2CO3/Na2CO3 ,of which inherent viscosity was 0.87; The poly- mers were characterized by IR,DSC,TG and XRD,and the struction was sure to PEEKK.. TG studies showed the polymer was stable up to 557℃ with a char yield at 1200℃ in N2 atmosphere;the DSC and XRD studies showed the polymer was semicrystallization, and the DSC studies showed the melting point of the polymer was 367℃.
出处
《有机氟工业》
CAS
2007年第2期13-17,共5页
Organo-Fluorine Industry
