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作 者:程海龙[1] 徐晶美[1] 马丽[1] 刘伯军[1] 任春丽[1] 白洪伟[1] 王哲[1,2] 张会轩[1,2]
机构地区:[1]长春工业大学化学工程学院合成树脂与特种纤维工程研究中心,吉林长春130012 [2]中国科学院长春应用化学研究所,吉林长春130012
出 处:《光谱学与光谱分析》2013年第10期2675-2678,共4页Spectroscopy and Spectral Analysis
基 金:国家自然科学基金项目(51273024);吉林省教育厅重点项目(2011103)资助
摘 要:采用直接缩聚的方法,通过调整氨基单体用量,合成出了系列带有不同氨基含量的聚芳醚酮砜(Am-PAEKS)聚合物,在聚合物侧链上进行后磺化接枝制备出了系列不同磺化度的侧链型磺化聚芳醚酮砜(S-SPAEKS),并且通过调整磺酸基团含量来控制聚合物的磺化度。通过红外光谱(FTIR)和氢核磁谱(1 HNMR),对所合成的单体及其聚合物的结构进行了表征,S-SPAEKS红外光谱在1 239和1 060cm-1处出现了磺酸基团中O=S=O的特征吸收峰,氢核磁谱中1.64ppm处出现了处于烷基链中间位置的两个氢(—CH2—CH2—)化学位移,证明得到了S-SPAEKS聚合物。经热失重分析发现,聚合物中磺酸基团的脱落温度都高于240℃,聚合物主链降解温度都高于450℃。研究表明,该系列聚合物具有良好的热性能,可以用作质子交换膜材料。A series of poly (arylene ether ketone sulfone) s containing different amino content (Am-PAEKS) were prepared via direct polycondensation reactions, and then the sulfobutyl groups were grafted onto the Am-PAEKS by amidating reaction be- tween the amide groups in Am-PAEKS and carboxylic acid groups in 4-(N-butane sulfonic) aminobenzoic acid. The structures of the compounds and the polymer were confirmed by WI'IR and H-NMR. The new characteristic bands at 1 239 and 1 060 cm 1 were assigned to O==S-~O symmetric stretching vibration and asymmetric stretching vibration of the sulfonic groups in sulfon- ated poly (arylene ether ketone sulfone) on side chain (S-SPAEKS), and the structures of the polymers were further confirmed by 1H NMR spectra, and the proton peak at 1.64 ppm was assigned to the methyl in the middle of the pendant sulfonated ali- phatic side chains, which show that the S-SPAEKS had been prepared successfully. In TGA curves we can observe two distinct weight loss steps, the first step was mainly attributed to the splitting-off of the sulfonic acid groups at 300 ℃, and the second step was mainly attributed to the decomposition of the main chain of the S-SPAEKS at 450 ℃. This series of S-SPAEKS poly- mers exhibit excellent thermal properties by thermo gravimetric analysis, which can satisfy the basic requirements of proton ex- change membrane (PEM) for fuel cells.
关 键 词:侧链型磺化聚芳醚酮砜 红外光谱 氢核磁谱 热重分析
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