摘要
在KOH和K2 CO3存在下 ,通过 2 ,6 二氯苯甲腈 (DCBN)与苯酚在N 甲基吡咯烷酮 (NMP)中的缩合反应 ,合成了一种新单体 2 ,6 二苯氧基苯甲腈 (DPOBN)。在无水AlCl3及NMP存在下 ,将其与对苯二甲酰氯(TPC)在 1,2 二氯乙烷 (DCE)中进行低温溶液缩聚 ,合成了含氰基聚芳醚醚酮酮 (PEEKK)。当n(DPOBN)∶n(TPC)控制在 1∶1,n(AlCl3) /n(TPC)控制在 6～ 6 5 ,n(NMP) /n(TPC)控制在 2 3 8～ 2 5 9时 ,聚合物的对数比浓粘度 ηinh可达 0 5 5。用IR、DSC、TG、WAXD等测试技术对其结构和性能进行了表征。结果表明 ,聚合物的Tg 为 180℃ ,比PEKK(Tg=15 6℃ )要高 ,聚合物的Td 为 495℃。DSC和WAXD分析表明 。
A novel monomer 2,6-diphenoxybenzonitrile(DPOBN) was prepared by condensation o f 2,6- dichlorobenzonitrile with phenol in NMP in the presence of KOH and K 2 CO 3 . A poly(arylether ether ketone ketone )(PEEKK) containing cy ano groups was synthesized by low temperature solution polycondensation of 2,6-diphenoxybenzonitrile with terephthaloyl dichloride(TPC) in 1,2-dichloroethane and in the presence of AlC l 3 and NMP. Effects of the molar ratio of DPOBN to TPC and the amounts of AlCl 3 and NMP on polycondensation were investigated. IR, DSC, TG, WAXD tec hniques were used to characterize the polymer. The results showed that the T g of the polymer was 180 ℃, 24 ℃ more than that of the PEKK(T g=15 6 ℃) and the polymer was noncrystalline. The polymer has an excellent heat-res istance(T d=495 ℃) and good solubility in DMF, NMP and DMSO.
出处
《应用化学》
CAS
CSCD
北大核心
2003年第3期238-241,共4页
Chinese Journal of Applied Chemistry
基金
江西省自然科学基金资助课题 ( 0 2 0 312)
关键词
聚芳醚醚酮酮
PEEKK
合成
二苯氧基苯甲腈
对苯二甲酰氯
低温溶液缩聚
poly(arylether ether ketone ketone),diphenoxybenzonitrile,terephthaloyl chloride ,low temperature solution polycondensation
