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新型多氯取代聚芳醚酮砜的合成与表征
Synthesis and Characterization of Novel Polychloro-substituted Poly(aryl ether ketone sulfone) Random Copolymers
【摘要】 由对苯二甲酰氯(TPC)经FeCl3催化氯化制备了四氯对苯二甲酰氯(TCTPC),并用元素分析、质谱和红外光谱分析技术进行了结构表征。在无水AlCl3及NMP存在下,将TCTPC、4, 4′-二苯氧基二苯砜(DPODPS)和TPC进行三元低温溶液共缩聚反应,合成了一系列新型多氯取代的高分子量聚芳醚酮砜(PESEKK/C PESEKK)无规共聚物。经FT-IR、DSC、TG及WAXD等分析表明,共聚物为非晶态结构,其玻璃化转变温度(Tg)介于168~232℃之间,高于已商品化的PEEK和PEKK,且随共聚物中多氯取代C-PESEKK结构单元含量增加而增加, 5%热失重温度(Td)则稍低于PEEK和PEKK。共聚物易溶于氯仿及DMF和DMSO等强极性非质子有机溶剂中。
【Abstract】 Tetrachloroterephthaloyl chloride(TCTPC) was synthesized via chlorination of terephthaloyl (chloride)(TPC) catalyzed by ferric chloride at 175~180 ℃ for 10 h, and confirmed by means of FTIR, MS and (elemental) analysis. A series of novel polychloro substituted poly(aryl ether ketone sulfone)(PESEKK/(C-PESEKK)) copolymers with high molecular weights were prepared by low-temperature solution polycondensation of TCTPC, 4,4-diphenoxydiphenyl sulfone(DPODPS) and TPC in 1,2-dichloroethane in the presence of AlCl3 and NMP. The copolymers were characterized by FT-IR, DSC and WAXD, etc. The results show that the copolymers are non-crystalline, exhibit high Tg′s(168~232 ℃), which are higher than that of commercial PEEK and PEKK, and increase with increasing C-PESEKK content. But the decomposition onset temperatures(Td)(5% mass loss) of the copolymers were a little lower than that of commercial PEEK and PEKK. The (copolymers) are soluble in CHCl3, and especially in strong aprotogenic organic solvents such as DMF, (DMSO) and NMP at room temperature.
【Key words】 poly(aryl ether ketone sulfone); tetrachloroterephthaloyl chloride; low-temperature solution polycondensation; random copolymer;
- 【文献出处】 应用化学 ,Chinese Journal of Applied Chemistry , 编辑部邮箱 ,2005年04期
- 【分类号】TQ326.5
- 【被引频次】18
- 【下载频次】145