摘要
以乙酰氨基苯酚为原料,经过BrCF2CF2Br氟烷基化、Zn催化脱卤、热环化二聚,以及水解去保护,合成了一种含全氟环丁烷环的二胺单体1,2,3,3,4,4-六氟-1,2-双[4-(氨基)苯氧基]环丁烷.用该单体分别与酯环二酐双环[2·2·1]辛烷-2,3,5,6-四羧基2,3,5,6-二酐(BHDA)、芳香性二酐3,3′,4,4′-联苯四酸二酐(BPDA)和3,3′,4,4′-二苯酮四酸二酐(BTDA)通过“一步法”制备了3种新型含全氟环丁烷环聚酰亚胺.通过粘度测试、溶解性实验、FT-IR、热失重分析(TGA)和差热扫描量热(DSC)分析等手段,对所合成的聚酰亚胺的结构与性能进行了表征.结果显示该类聚酰亚胺可溶于大多数常用极性有机溶剂,热分解温度高于480℃,其中两种聚合物玻璃化温度低于150℃,表明含全氟环丁烷环聚酰亚胺具有良好的溶解性和可加工性.
Polyimides containing perfluorocyclobutane rings were synthesized from a new diamine 1,2,3,3,4,4- hexafluoro- 1,2-bis （4-aminophenoxy） cyclobutane with three dianhydrides, namely bicyclo [ 2.2.1 ] octane-2,3,5,6- tetracarboxylic 2,3,5,6-dianhydride （ BHDA）, biphenyhetracarboxylic dianhydride （BPDA） and benzophenone-3, 3＇ ,4,4＇-tetracarboxylic dianhydride （BTDA）,respectively.The new diamine was synthesized v/a fluoroalkylation of 4-acetamidophenol with BrCF2CF2 Br followed by Zn-mediated elimination and exothermic cyclodimerization. The polymers were characterized by means of FT-IR, inherent viscosity, solubility determination, differential scanning calorimetry （DSC） and thermogravimetric analysis （TGA）. TGA studies indicated that the polymers were all stable up to 480℃. DSC results show that two of the three polymers have a Ts below 150℃. The polymers were found to be soluble in the commonly used polar solvents. Thus the polymers containing perflurocyclobutane rings exhibited excellent solubility and processability.
出处
《高分子学报》
SCIE
CAS
CSCD
北大核心
2007年第2期114-118,共5页
Acta Polymerica Sinica
关键词
全氟环丁烷环
聚酰亚胺
合成
表征
Perfluorocyclobutane, Polyimide, Synthesis, Characterization
