界面聚合法成膜过程观测及分离CO_2复合膜制备
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摘要
界面聚合法已成功应用于商业化反渗透膜和纳滤膜的制备，在制备气体分离膜方面也表现出巨大的应用潜力。然而，界面聚合成膜过程的相关研究报道较少，同时，界面聚合分离气体复合膜的“制备—结构—性能”关系尚不明晰。基于此，本文分别以N-甲基二乙醇胺（MEDA）和均苯三甲酰氯（TMC）为水相和有机相单体，开发了两种可视化技术对界面聚合成膜过程进行研究，同时还探明了界面聚合分离气体复合膜的“制备—结构—性能”关系。
采用视频光学接触角测量仪（OCA）对界面聚合过程中水相悬滴浸入有机相中的形貌以及所形成的膜的形貌进行了研究。首先，通过观察水相悬滴浸入有机相中的形貌变化，证实界面聚合膜朝有机相生长。其次，研究了多种聚合条件对界面聚合过程中膜形貌的影响，结果发现界面聚合膜上通常会出现“胞状”结构。膜上的“胞状”结构的产生归因于所形成的具有巨大表面能的初生膜处于热力学不稳定状态。最后，实验验证了界面聚合过程中形成的膜表面“胞状”结构最终会形成粗糙的复合膜表面。
采用光学显微镜对界面聚合过程中膜形貌进行可视化研究。首先对界面聚合过程中两相单体的扩散进行分析，结果表明两相单体的扩散都导致水相-有机相界面处界面不稳定性的产生。其次，研究发现界面聚合膜形貌为典型的多尺度形貌，膜表面较小尺度的“胞状”结构均匀分布在较大尺度的凹凸不平的结构上。界面聚合膜表面较小尺度的“胞状”结构的产生归因于所形成的具有巨大表面能的初生膜处于热力学不稳定状态；而反映了水相-有机相界面处波动的膜表面较大尺度的凹凸不平归因于聚合过程中界面处存在的水相单体浓度梯度所引起的界面不稳定性。
在涂敷一层硅橡胶（PDMS）涂层的聚砜（PS）超滤膜上界面聚合制备复合膜用于CO_2/N_2分离。利用多种测试手段对复合膜分离层的结构参数进行表征。研究了复合膜的“制备—结构—性能”关系。结果表明，同时具有高CO_2渗透速率和高CO_2/N_2分离因子的复合膜具有较薄的分离层厚度、较高的分离层交联度和较低的分离层结晶度。上述高性能气体分离膜可以按照以下两条原则制得：①增加水相单体在有机溶剂中的扩散性而降低水相单体在有机溶剂中的溶解性；②适当降低有机相单体浓度同时适当增加水相单体浓度。以上结论对气体分离复合膜的可控制备具有重要意义。
Interfacial polymerization (IP) has been a well-established method for thepreparation of commercially thin film composite (TFC) reverse osmosis (RO) andnanofiltration (NF) membranes. Moreover, it has been proved that IP is also aneffective way for the synthesis of gas separation membranes. However, little attentionhas been paid to the study of IP film formation. Meanwhile, no information has beenreported on studying the formation-structure-performance relationship for interfaciallypolymerized TFC gas separation membranes. Based on the above consideration, thisstudy makes attempts to develop two techniques to visualize the film formation by IP,as well as to elucidate the formation-structure-performance relationship forinterfacially polymerized TFC gas separation membranes based on the reaction ofN-methyldiethanolamine (MEDA) and trimesoyl chloride (TMC).
An optical contact angle measuring device (OCA) was used to visualize themorphology of pendant drop of aqueous solution immersed in organic solution andthe film formed during IP process. Firstly, the variations of the morphology ofpendant drop of aqueous solution were studied, the results offered in-situexperimental evidence for the growth of interfacial film towards the organic phase.Furthermore, the effects of various synthesis conditions on film morphology werestudied. It was found that the bubbles were generally appeared on the films. Thebubbles on the films were attributed to the instability arising from the formation of thenascent solid thin film with a huge surface energy. The bubbles on the films couldultimately result in the rough membrane surface.
A digital microscope was used to visualize the film morphology during IPprocess. Firstly, the diffusion of the monomers in both aqueous and organic phaseswas analyzed, and the results show that the diffusion of the monomers in both phasescould cause the interfacial instability of the aqueous-organic interface. Moreover, itwas found that the morphology of interfacially polymerized film is of multi-scalecharacteristic, wherein small-scale bubbles were evenly distributed on large-scalerugged film surfaces. The small-scale bubbles on the films were attributed to theinstability arising from the formation of the nascent solid thin film with a huge surfaceenergy. And the large-scale rugged film surfaces, which reflected the fluctuations of the aqueous-organic interface, were attributed to the interfacial instability arising fromthe presence of very steep concentration gradient of aqueous monomer near theaqueous-organic interface.
TFC membranes for CO_2/N_2separation were prepared by IP on crosslinkedpolydimethylsiloxane (PDMS) coating polysulfone (PS) support membrane. Thestructural properties of TFC membrane surfaces were characterized by severaltechniques. The relationships among the skin layer formation conditions, skin layerstructure, and membrane separation performance were investigated. Results show thatmembranes with higher CO_2permeance and good CO_2/N_2selectivity appeared toconsist of thinner, more crosslinked, and less crystalline skin layer structures. Suchhigh performance gas separation membranes were obtained by (1) increasingdiffusivity and decreasing solubility of the aqueous monomer in the organic solvent,and (2) reducing the concentration of the organic monomer and raising theconcentration of the aqueous monomer. These findings have great theoreticalsignificance for the controlled preparation of gas separation membranes.
采用视频光学接触角测量仪（OCA）对界面聚合过程中水相悬滴浸入有机相中的形貌以及所形成的膜的形貌进行了研究。首先，通过观察水相悬滴浸入有机相中的形貌变化，证实界面聚合膜朝有机相生长。其次，研究了多种聚合条件对界面聚合过程中膜形貌的影响，结果发现界面聚合膜上通常会出现“胞状”结构。膜上的“胞状”结构的产生归因于所形成的具有巨大表面能的初生膜处于热力学不稳定状态。最后，实验验证了界面聚合过程中形成的膜表面“胞状”结构最终会形成粗糙的复合膜表面。
采用光学显微镜对界面聚合过程中膜形貌进行可视化研究。首先对界面聚合过程中两相单体的扩散进行分析，结果表明两相单体的扩散都导致水相-有机相界面处界面不稳定性的产生。其次，研究发现界面聚合膜形貌为典型的多尺度形貌，膜表面较小尺度的“胞状”结构均匀分布在较大尺度的凹凸不平的结构上。界面聚合膜表面较小尺度的“胞状”结构的产生归因于所形成的具有巨大表面能的初生膜处于热力学不稳定状态；而反映了水相-有机相界面处波动的膜表面较大尺度的凹凸不平归因于聚合过程中界面处存在的水相单体浓度梯度所引起的界面不稳定性。
在涂敷一层硅橡胶（PDMS）涂层的聚砜（PS）超滤膜上界面聚合制备复合膜用于CO_2/N_2分离。利用多种测试手段对复合膜分离层的结构参数进行表征。研究了复合膜的“制备—结构—性能”关系。结果表明，同时具有高CO_2渗透速率和高CO_2/N_2分离因子的复合膜具有较薄的分离层厚度、较高的分离层交联度和较低的分离层结晶度。上述高性能气体分离膜可以按照以下两条原则制得：①增加水相单体在有机溶剂中的扩散性而降低水相单体在有机溶剂中的溶解性；②适当降低有机相单体浓度同时适当增加水相单体浓度。以上结论对气体分离复合膜的可控制备具有重要意义。
Interfacial polymerization (IP) has been a well-established method for thepreparation of commercially thin film composite (TFC) reverse osmosis (RO) andnanofiltration (NF) membranes. Moreover, it has been proved that IP is also aneffective way for the synthesis of gas separation membranes. However, little attentionhas been paid to the study of IP film formation. Meanwhile, no information has beenreported on studying the formation-structure-performance relationship for interfaciallypolymerized TFC gas separation membranes. Based on the above consideration, thisstudy makes attempts to develop two techniques to visualize the film formation by IP,as well as to elucidate the formation-structure-performance relationship forinterfacially polymerized TFC gas separation membranes based on the reaction ofN-methyldiethanolamine (MEDA) and trimesoyl chloride (TMC).
An optical contact angle measuring device (OCA) was used to visualize themorphology of pendant drop of aqueous solution immersed in organic solution andthe film formed during IP process. Firstly, the variations of the morphology ofpendant drop of aqueous solution were studied, the results offered in-situexperimental evidence for the growth of interfacial film towards the organic phase.Furthermore, the effects of various synthesis conditions on film morphology werestudied. It was found that the bubbles were generally appeared on the films. Thebubbles on the films were attributed to the instability arising from the formation of thenascent solid thin film with a huge surface energy. The bubbles on the films couldultimately result in the rough membrane surface.
A digital microscope was used to visualize the film morphology during IPprocess. Firstly, the diffusion of the monomers in both aqueous and organic phaseswas analyzed, and the results show that the diffusion of the monomers in both phasescould cause the interfacial instability of the aqueous-organic interface. Moreover, itwas found that the morphology of interfacially polymerized film is of multi-scalecharacteristic, wherein small-scale bubbles were evenly distributed on large-scalerugged film surfaces. The small-scale bubbles on the films were attributed to theinstability arising from the formation of the nascent solid thin film with a huge surfaceenergy. And the large-scale rugged film surfaces, which reflected the fluctuations of the aqueous-organic interface, were attributed to the interfacial instability arising fromthe presence of very steep concentration gradient of aqueous monomer near theaqueous-organic interface.
TFC membranes for CO_2/N_2separation were prepared by IP on crosslinkedpolydimethylsiloxane (PDMS) coating polysulfone (PS) support membrane. Thestructural properties of TFC membrane surfaces were characterized by severaltechniques. The relationships among the skin layer formation conditions, skin layerstructure, and membrane separation performance were investigated. Results show thatmembranes with higher CO_2permeance and good CO_2/N_2selectivity appeared toconsist of thinner, more crosslinked, and less crystalline skin layer structures. Suchhigh performance gas separation membranes were obtained by (1) increasingdiffusivity and decreasing solubility of the aqueous monomer in the organic solvent,and (2) reducing the concentration of the organic monomer and raising theconcentration of the aqueous monomer. These findings have great theoreticalsignificance for the controlled preparation of gas separation membranes.
引文
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