Chen Gong, Chen Yuan, Huang Tingjian, He Zhongchen, Xu Jianjun, Liu Pengqing
College of Polymer Science & Engineering, Sichuan University, Chengdu 610065, China.
Polymers (Basel). 2019 Aug 26;11(9):1398. doi: 10.3390/polym11091398.
Poly(ether ether ketone) (PEEK) hollow fiber membranes were successfully prepared from miscible blends of PEEK and polyetherimide (PEI) via thermally-induced phase separation (TIPS) with subsequent extraction of the PEI diluent. The phase structure evolution, extraction kinetics, membrane morphology, pore size distribution and permeability for the hollow fiber membrane were studied in detail. Extraction experiments, differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMA) studies showed that the heat treatment had a significant influence on the two-phase structure of PEEK/PEI, and that it was controlled by the crystallization kinetic of PEEK and the diffusion kinetic of PEI. As the annealing temperature increased, the controlling factor of the phase separation changed from PEEK crystallization to PEI diffusion, and the main distribution of the amorphous PEI chains were changed from the interlamellar region to the interfibrillar or interspherulitic regions of PEEK crystallization. When the annealing temperature increased from 240 °C to 280 °C, the extracted amount of PEI increased from 85.19 to 96.24 wt %, and the pore diameter of PEEK membrane increased from 10.59 to 37.85 nm, while the surface area of the PEEK membrane decreased from 111.9 to 83.69 m/g. Moreover, the water flux of the PEEK hollow fiber membranes increased from 1.91 × 10 to 1.65 × 10 L h m bar as the annealing temperature increased from 240 °C to 270 °C. The structure and properties of the PEEK hollow fiber membrane can be effectively controlled by regulating heat treatment conditions.
通过热致相分离（TIPS），随后萃取聚醚酰亚胺（PEI）稀释剂，由聚醚醚酮（PEEK）和聚醚酰亚胺（PEI）的互溶共混物成功制备了聚醚醚酮（PEEK）中空纤维膜。详细研究了中空纤维膜的相结构演变、萃取动力学、膜形态、孔径分布和渗透性。萃取实验、差示扫描量热法（DSC）和动态热机械分析（DMA）研究表明，热处理对PEEK/PEI的两相结构有显著影响，且受PEEK的结晶动力学和PEI的扩散动力学控制。随着退火温度升高，相分离的控制因素从PEEK结晶转变为PEI扩散，无定形PEI链的主要分布从PEEK结晶的片层间区域转变为原纤维间或球晶间区域。当退火温度从240℃升高到280℃时，PEI的萃取量从85.19 wt%增加到96.24 wt%，PEEK膜的孔径从10.59 nm增加到37.85 nm，而PEEK膜的表面积从111.9 m²/g减小到83.69 m²/g。此外，随着退火温度从240℃升高到270℃，PEEK中空纤维膜的水通量从1.91×10⁻² L·h⁻¹·m⁻²·bar⁻¹增加到1.65×10⁻¹ L·h⁻¹·m⁻²·bar⁻¹。通过调节热处理条件，可以有效控制PEEK中空纤维膜的结构和性能。
