聚苯胺纳米纤维复合超滤膜制备研究
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摘要
把纳米材料应用于分离膜制备,得到高性能纳米复合膜近年来已成为膜技术领域内的一个前沿研究方向。本文首次将聚苯胺(PANI)纳米纤维用于分离膜制备,对PANI纳米纤维/聚砜(PS)复合超滤膜的制备方法和性能进行了较深入的研究。
利用PS膜过滤PANI纳米纤维分散液制备出PANI/PS复合膜。复合膜具有亲水的PANI纳米纤维多孔层。在相同条件下,复合膜的纯水通量比PS膜提高了60%。PS膜对BSA和PEG-20000的截留率分别为98.8%和27.2%,复合膜对BSA和PEG-20000的截留率分别为99.2%和27%。当进水pH值小于7时,复合膜表面的氨基和亚氨基会被质子化,膜表面带正电荷。复合膜表现出较低的BSA平衡吸附量,大约是PS膜平衡吸附量的六分之一。在过滤BSA溶液过程中,复合膜比PS膜表现出较高的渗透通量和较慢的通量下降速率。
利用浸没相转化法制备出PANI/PS共混膜。与PS膜相比,共混膜具有更好的亲水性和较高的孔隙率。PANI纳米纤维在成膜过程中的迁移行为提高了共混膜的孔连通性。共混膜的纯水通量明显高于PS膜,PANI纳米纤维与PS质量比为1%的共混膜的纯水通量比PS膜提高了60%,而PANI纳米纤维与PS质量比为15%的共混膜的纯水通量比PS膜提高了140%。PS膜对BSA和AE的截留率分别是96%和93%,共混膜对BSA和AE的截留率范围分别在96%~99%和93%~98%。在过滤BSA溶液过程中,所有的PANI/PS共混膜与PS膜相比都具有较高的渗透通量,而且共混膜的渗透通量随着PANI纳米纤维含量的增加而升高。PANI纳米纤维与PS质量比为1%和15%的共混膜的稳态渗透通量分别是PS膜的2倍和2.5倍。此外,PANI/PS共混膜具有较慢的通量下降速率和较高的通量恢复率。共混膜的拉伸强度随着PANI纳米纤维含量的增加而增大,而膜的断裂伸长率随着PANI纳米纤维含量的增加而减小。当PANI纳米纤维与PS质量比为1%时,共混膜与PS膜相比机械性能没有明显改变。PANI/PS共混膜的热稳定性与PS膜相近。
初步探索了PANI纳米纤维在PS膜表面的原位生长过程。通过控制苯胺聚合体系中的掺杂酸和十二烷基苯磺酸钠浓度,在低温和较短的搅拌时间下能够使PANI纳米纤维在PS膜表面均匀生长,得到PANI/PS复合膜。随着反应时间延长,聚苯胺/聚砜复合膜的亲水性能不断提高。随着反应时间延长,复合膜的纯水通量不断下降,而PEG-35K截留率呈上升趋势。复合膜的导电性随反应时间的延长而提高,反应24小时所得复合膜的电导率为0.04 S/cm。
In recent years, to prepare nanocomposite membrane with high performance through the incorporation of nanomaterials has been a new research direction of membrane technology. This paper initially investigated the preparation and characterization of polyaniline (PANI) nanofibers/polysulfone (PS) nanocomposite UF membrane.
PANI/PS nanocomposite membrane was prepared through the filtration of PANI aqueous dispersion with PS membrane. PANI/PS membrane had a hydrophilic and porous layer of PANI nanofibers. Pure water flux of PANI/PS membrane was 1.6 times that of PS membrane. For PS membrane, rejections of BSA and PEG-20000 were 98.8% and 27.2%, respectively. For PANI/PS membrane, rejections of BSA and PEG-20000 were 99.2% and 27%, respectively. When feed pH was less than 7, the amines and imines of PANI were protonated and PANI/PS membrane surface had positive charge. The BSA adsorption quantity of PS membrane was 6 times than that of PANI/PS membrane. During the filtration of BSA solution, PANI/PS membrane showed higher permeate flux and lower flux decline rate than PS membrane.
PANI/PS blend membrane was prepared with the immersion phase inversion method. Compared with PS membrane, PANI/PS blend membrane had better hydrophilic property and higher porosity. The connectivity of blend membrane pores was improved by the migration of PANI nanofibers. Pure water flux of the blend membrane was higher than that of PS membrane. Pure water flux of the blend membrane with PANI– PS mass ratio of 1 wt. % was 1.6 times that of PS membrane, and pure water flux of the blend membrane with PANI– PS mass ratio of 15 wt. % was 2.4 times that of PS membrane. For PS membrane, rejections of BSA and AE were 96% and 93%, respectively. For the blend membrane, rejections of BSA and AE were in the range of 96%~99% and 93%~98%, respectively. During the filtration of BSA solution, all the blend membranes showed higher permeate fluxes than PS membrane and their fluxes increased with the rise of PANI nanofibers content. Stable permeate fluxes of the blend membranes with PANI– PS mass ratio of 1 wt. % and 15 wt. % were 2.0 and 2.5 times that of pure PS membrane, respectively. In addition, PANI/PS blend membrane showed lower flux decline rate and higher flux recovery ratio. With the rise of PANI nanofibers content, the breaking strength of the blend membrane increased and the elongation at break decreased. Mechanical property of the blend membrane with PANI– PS mass ratio of 1 wt. % had no obvious change. The blend membranes presented similar thermal behavior to PS membrane.
The in-situ growth of PANI nanofibers on PS membrane surface was explored. PANI nanofibers could grow homogeneously on PS membrane under lower temperature, shorter stir time, and suitable doping acid and SDBS concentration to form PANI/PS composite membrane. With the extension of polymerization time, the composite membrane had better hydrophilic property, lower pure water flux, higher PEG-35K rejection, and higher conductivity. After 24 h polymerization, the conductivity of the composite membrane was 0.04 S/cm.
利用PS膜过滤PANI纳米纤维分散液制备出PANI/PS复合膜。复合膜具有亲水的PANI纳米纤维多孔层。在相同条件下,复合膜的纯水通量比PS膜提高了60%。PS膜对BSA和PEG-20000的截留率分别为98.8%和27.2%,复合膜对BSA和PEG-20000的截留率分别为99.2%和27%。当进水pH值小于7时,复合膜表面的氨基和亚氨基会被质子化,膜表面带正电荷。复合膜表现出较低的BSA平衡吸附量,大约是PS膜平衡吸附量的六分之一。在过滤BSA溶液过程中,复合膜比PS膜表现出较高的渗透通量和较慢的通量下降速率。
利用浸没相转化法制备出PANI/PS共混膜。与PS膜相比,共混膜具有更好的亲水性和较高的孔隙率。PANI纳米纤维在成膜过程中的迁移行为提高了共混膜的孔连通性。共混膜的纯水通量明显高于PS膜,PANI纳米纤维与PS质量比为1%的共混膜的纯水通量比PS膜提高了60%,而PANI纳米纤维与PS质量比为15%的共混膜的纯水通量比PS膜提高了140%。PS膜对BSA和AE的截留率分别是96%和93%,共混膜对BSA和AE的截留率范围分别在96%~99%和93%~98%。在过滤BSA溶液过程中,所有的PANI/PS共混膜与PS膜相比都具有较高的渗透通量,而且共混膜的渗透通量随着PANI纳米纤维含量的增加而升高。PANI纳米纤维与PS质量比为1%和15%的共混膜的稳态渗透通量分别是PS膜的2倍和2.5倍。此外,PANI/PS共混膜具有较慢的通量下降速率和较高的通量恢复率。共混膜的拉伸强度随着PANI纳米纤维含量的增加而增大,而膜的断裂伸长率随着PANI纳米纤维含量的增加而减小。当PANI纳米纤维与PS质量比为1%时,共混膜与PS膜相比机械性能没有明显改变。PANI/PS共混膜的热稳定性与PS膜相近。
初步探索了PANI纳米纤维在PS膜表面的原位生长过程。通过控制苯胺聚合体系中的掺杂酸和十二烷基苯磺酸钠浓度,在低温和较短的搅拌时间下能够使PANI纳米纤维在PS膜表面均匀生长,得到PANI/PS复合膜。随着反应时间延长,聚苯胺/聚砜复合膜的亲水性能不断提高。随着反应时间延长,复合膜的纯水通量不断下降,而PEG-35K截留率呈上升趋势。复合膜的导电性随反应时间的延长而提高,反应24小时所得复合膜的电导率为0.04 S/cm。
In recent years, to prepare nanocomposite membrane with high performance through the incorporation of nanomaterials has been a new research direction of membrane technology. This paper initially investigated the preparation and characterization of polyaniline (PANI) nanofibers/polysulfone (PS) nanocomposite UF membrane.
PANI/PS nanocomposite membrane was prepared through the filtration of PANI aqueous dispersion with PS membrane. PANI/PS membrane had a hydrophilic and porous layer of PANI nanofibers. Pure water flux of PANI/PS membrane was 1.6 times that of PS membrane. For PS membrane, rejections of BSA and PEG-20000 were 98.8% and 27.2%, respectively. For PANI/PS membrane, rejections of BSA and PEG-20000 were 99.2% and 27%, respectively. When feed pH was less than 7, the amines and imines of PANI were protonated and PANI/PS membrane surface had positive charge. The BSA adsorption quantity of PS membrane was 6 times than that of PANI/PS membrane. During the filtration of BSA solution, PANI/PS membrane showed higher permeate flux and lower flux decline rate than PS membrane.
PANI/PS blend membrane was prepared with the immersion phase inversion method. Compared with PS membrane, PANI/PS blend membrane had better hydrophilic property and higher porosity. The connectivity of blend membrane pores was improved by the migration of PANI nanofibers. Pure water flux of the blend membrane was higher than that of PS membrane. Pure water flux of the blend membrane with PANI– PS mass ratio of 1 wt. % was 1.6 times that of PS membrane, and pure water flux of the blend membrane with PANI– PS mass ratio of 15 wt. % was 2.4 times that of PS membrane. For PS membrane, rejections of BSA and AE were 96% and 93%, respectively. For the blend membrane, rejections of BSA and AE were in the range of 96%~99% and 93%~98%, respectively. During the filtration of BSA solution, all the blend membranes showed higher permeate fluxes than PS membrane and their fluxes increased with the rise of PANI nanofibers content. Stable permeate fluxes of the blend membranes with PANI– PS mass ratio of 1 wt. % and 15 wt. % were 2.0 and 2.5 times that of pure PS membrane, respectively. In addition, PANI/PS blend membrane showed lower flux decline rate and higher flux recovery ratio. With the rise of PANI nanofibers content, the breaking strength of the blend membrane increased and the elongation at break decreased. Mechanical property of the blend membrane with PANI– PS mass ratio of 1 wt. % had no obvious change. The blend membranes presented similar thermal behavior to PS membrane.
The in-situ growth of PANI nanofibers on PS membrane surface was explored. PANI nanofibers could grow homogeneously on PS membrane under lower temperature, shorter stir time, and suitable doping acid and SDBS concentration to form PANI/PS composite membrane. With the extension of polymerization time, the composite membrane had better hydrophilic property, lower pure water flux, higher PEG-35K rejection, and higher conductivity. After 24 h polymerization, the conductivity of the composite membrane was 0.04 S/cm.
引文
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