磺化度对磺化聚醚醚酮微观结构及热性能影响分析

Influence of sulfonation degree on the microstructure and thermal property of sulfonated poly(ether ether ketone)

采用浓硫酸和聚醚醚酮(PEEK)制备了不同磺化度(DS)的磺化聚醚醚酮(SPEEK)。通过1 H-核磁(1 HNMR)对SPEEK化学结构进行表征。同时,根据1 H-NMR积分面积计算并确定了70℃条件下,磺化时间分别为2、4、6、8和10h制备的SPEEK磺化度分别为25.6%、48.7%、71.6%、85.4%和91.0%。采用扫描电镜(SEM)、差式扫描量热仪(DSC)以及热重分析(TGA)对比分析了磺化度对SPEEK微观结构、玻璃化转变温度(Tg)和热稳定性能的影响。研究结果表明,磺化度为71.6%的SPEEK具有均匀的微观结构和最优异的热稳定性能。

Sulfonated poly（ether ether ketone）（SPEEK） materials with various sulfonation degree（DS） were pre- pared through concentrated H2 SO4 and poly（ether ether ketone）（PEEK）. The chemical structure of SPPEK was measured via 1 H-nuclear magnetic resonance （1 H-NMR）. Meanwhile,DS of SPEEK undergoing sulfonated time of 2,4,6,8 and 10 h was 25.6% ,48.7% ,71.6% ,85.4% and 91.0% ,respectively,which was calculated according to the integral area from 1 H- NMR. The microstructure,glass transition temperature （Tg） and thermal stability of SPEEK were measured by scanning e- lectron microscope（SEM）, differential scanning calorimetry （DSC） and thermogravimetric analysis （TGA）, respectively. The results demonstrated that SPEEK with DS of 71.6% owned uniform microstructure and the best thermal stability a- mong the prepared SPEEK.