表面偏析超滤膜的制备及其抗污染机理研究
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摘要
膜污染是限制超滤过程广泛应用的瓶颈,因而研究膜污染机理和开发抑制膜污染的方法已经成为超滤领域的一个研究热点。论文以解决高分子超滤膜污染为出发点,采用蛋白质溶液为模型体系,聚醚砜(PES)为膜主体,聚氧乙烯-聚氧丙烯-聚氧乙烯(Pluronic)两亲嵌段共聚物为表面改性剂,制备了不同类型表面偏析超滤膜。
采用DSC、XPS、FTIR、静态接触角和SEM等方法对PES-Pluronic表面偏析超滤膜进行了表征。结果表明:由于Pluronic与PES之间的部分相容性,使Pluronic在成膜过程中发生表面偏析,增大了膜表面亲水性,但并未改变膜原有的不对称结构。通过计算Pluronic在膜表面覆盖度和膜中残留率,考察了影响湿法相转化过程中Pluronic表面偏析行为的因素。结果表明:Pluronic的亲疏水链段长度之比和分子量是影响Pluronic表面偏析行为的两个重要因素。
通过对PES-Pluronic表面偏析超滤膜分离特性和抗污染特性的系统研究,发现:Pluronic的引入增大了超滤膜的膜孔径,降低了蛋白质截留率;膜表面高密度PEO链段,使PES-Pluronic表面偏析超滤膜具有优良的抑制蛋白质吸附能力和抗污染特性,蛋白质吸附量最低可降到0,通量恢复率最高可达到89%,高于空白膜的62%。
为了进一步提高膜表面PEO链段覆盖度,利用Pluronic P123制备一系列枝状嵌段共聚物,并将其用于表面偏析超滤膜的制备。结果表明:枝状嵌段共聚物具有较高的表面偏析能力,由其制备的表面偏析改性膜具有较高的亲水性和抗污染性能,并且增大枝状嵌段共聚物中PEO臂数可以提升表面偏析超滤膜的抗污染特性。
测量了PES铸膜液浊点线和凝胶值,考察了Pluronic的引入对铸膜液相行为的影响,研究表明Pluronic的加入改善了铸膜液的稳定性。采用分子模拟对Pluronic表面偏析机理以及铸膜液相行为进行了初步研究,结果表明:由Pluronic结构不同引起的相互作用力差异是导致表面偏析行为差异的根本原因;加入Pluronic后,铸膜液中容易形成体积较大的反胶团,使得表面偏析超滤膜中出现较大的膜孔。最后研究了Pluronic结构和抗污染特性之间的内在关系,初步提出了表面偏析超滤膜的设计原则。
Membrane fouling constitutes a bottleneck limiting the wide application of ultrafiltration technology; therefore, investigating the antifouling mechanism and developing methods to inhibit membrane fouling have become an important research issue in ultrafiltration area. In this dissertation, we have prepared different kinds of surface segregated membranes through segregation method, using poly(ether sulfone) as membrane bulk material, different amphiphilic polymer poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) as membrane surface modifying agent(MSMA), and protein solutions as model system. .
DSC, XPS, FTIR, the static contact angle, and SEM were all introduced to characterize PES-Pluronic surface segregated ultrafiltration membranes. Due to the partial compatibility between PES and Pluronic, Pluronic segregated substantially during membrane formation, which increased the hydrophicity of membrane surface. And the SEM results indicated that the addition of Pluronic did not cause remarkable change on the asymmetry structure of membrane. In order to investigate segregation behavior of Pluronic during phase inversion in a wet processs, the surface coverage and residual ratio of Pluronic were calculated basing on XPS and FTIR results. It can be concluded that the molecular weight and the length ratio of hydrophilic segments to hydrophobic segments of Pluronic were two important factors influenceing Pluronic segregation behavior.
Separation performance and anti-fouling properties of PES-Pluronic surface segregated ultrafiltration membranes were systematically investigated, and it was found that the addition of Pluronic enlarged the membrane pores, which decreased the protein rejection ratio; and the high density PEO segments appearring at membrane surface rendered the membrane with excellent protein-resistant ability and anti-fouling property. The protein adsorption amount on membrane surface decreased to as low as zero, and the flux recovery ratio could reach as high as 89%, which was much higher than that of PES control membrane, 62%.
In order to increase the PEO density on membrane surface, a series of novel branched block polymers were prepared by simple substitution reaction based on Pluronic P123, and the effect of chemical structure of these MSMAs on the separation performance and anti-fouling ability of membranes was studied. The experimental results revealed that the block polymer with higher PEO arms number or PEO content exhibited stronger segregation ability, which rendered the membrane better anti-fouling ability.
In order to investigate the effect of Pluronic on the phase behavior of membrane casting solution, the cloudy point line was plotted and coagulation value was measured, the results showed that the addition of Pluronic improved the stability of membrane casting solution. The molecular simulation calculation was conducted to preliminarily invesitgate the segregation performance of Pluronic during membrane formation and the phase behavior of membrane casting solution. The simulation results indicated that the difference of interaction between different components constituted the dominant reason for the different segregation performance of Pluronic; and the addition of Pluronic in casting solution resulted in larger reverse micelle, which might correspondingly lead to larger membrane pore appearing at membrane surface. Finally, the inherent relationship between the structural characteristics of block polymers and the anti-fouling ability of the membranes was studied; the guidance for the rational design and preparation of surface segregated ultrafiltration membrane was tentatively proposed.
采用DSC、XPS、FTIR、静态接触角和SEM等方法对PES-Pluronic表面偏析超滤膜进行了表征。结果表明:由于Pluronic与PES之间的部分相容性,使Pluronic在成膜过程中发生表面偏析,增大了膜表面亲水性,但并未改变膜原有的不对称结构。通过计算Pluronic在膜表面覆盖度和膜中残留率,考察了影响湿法相转化过程中Pluronic表面偏析行为的因素。结果表明:Pluronic的亲疏水链段长度之比和分子量是影响Pluronic表面偏析行为的两个重要因素。
通过对PES-Pluronic表面偏析超滤膜分离特性和抗污染特性的系统研究,发现:Pluronic的引入增大了超滤膜的膜孔径,降低了蛋白质截留率;膜表面高密度PEO链段,使PES-Pluronic表面偏析超滤膜具有优良的抑制蛋白质吸附能力和抗污染特性,蛋白质吸附量最低可降到0,通量恢复率最高可达到89%,高于空白膜的62%。
为了进一步提高膜表面PEO链段覆盖度,利用Pluronic P123制备一系列枝状嵌段共聚物,并将其用于表面偏析超滤膜的制备。结果表明:枝状嵌段共聚物具有较高的表面偏析能力,由其制备的表面偏析改性膜具有较高的亲水性和抗污染性能,并且增大枝状嵌段共聚物中PEO臂数可以提升表面偏析超滤膜的抗污染特性。
测量了PES铸膜液浊点线和凝胶值,考察了Pluronic的引入对铸膜液相行为的影响,研究表明Pluronic的加入改善了铸膜液的稳定性。采用分子模拟对Pluronic表面偏析机理以及铸膜液相行为进行了初步研究,结果表明:由Pluronic结构不同引起的相互作用力差异是导致表面偏析行为差异的根本原因;加入Pluronic后,铸膜液中容易形成体积较大的反胶团,使得表面偏析超滤膜中出现较大的膜孔。最后研究了Pluronic结构和抗污染特性之间的内在关系,初步提出了表面偏析超滤膜的设计原则。
Membrane fouling constitutes a bottleneck limiting the wide application of ultrafiltration technology; therefore, investigating the antifouling mechanism and developing methods to inhibit membrane fouling have become an important research issue in ultrafiltration area. In this dissertation, we have prepared different kinds of surface segregated membranes through segregation method, using poly(ether sulfone) as membrane bulk material, different amphiphilic polymer poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) as membrane surface modifying agent(MSMA), and protein solutions as model system. .
DSC, XPS, FTIR, the static contact angle, and SEM were all introduced to characterize PES-Pluronic surface segregated ultrafiltration membranes. Due to the partial compatibility between PES and Pluronic, Pluronic segregated substantially during membrane formation, which increased the hydrophicity of membrane surface. And the SEM results indicated that the addition of Pluronic did not cause remarkable change on the asymmetry structure of membrane. In order to investigate segregation behavior of Pluronic during phase inversion in a wet processs, the surface coverage and residual ratio of Pluronic were calculated basing on XPS and FTIR results. It can be concluded that the molecular weight and the length ratio of hydrophilic segments to hydrophobic segments of Pluronic were two important factors influenceing Pluronic segregation behavior.
Separation performance and anti-fouling properties of PES-Pluronic surface segregated ultrafiltration membranes were systematically investigated, and it was found that the addition of Pluronic enlarged the membrane pores, which decreased the protein rejection ratio; and the high density PEO segments appearring at membrane surface rendered the membrane with excellent protein-resistant ability and anti-fouling property. The protein adsorption amount on membrane surface decreased to as low as zero, and the flux recovery ratio could reach as high as 89%, which was much higher than that of PES control membrane, 62%.
In order to increase the PEO density on membrane surface, a series of novel branched block polymers were prepared by simple substitution reaction based on Pluronic P123, and the effect of chemical structure of these MSMAs on the separation performance and anti-fouling ability of membranes was studied. The experimental results revealed that the block polymer with higher PEO arms number or PEO content exhibited stronger segregation ability, which rendered the membrane better anti-fouling ability.
In order to investigate the effect of Pluronic on the phase behavior of membrane casting solution, the cloudy point line was plotted and coagulation value was measured, the results showed that the addition of Pluronic improved the stability of membrane casting solution. The molecular simulation calculation was conducted to preliminarily invesitgate the segregation performance of Pluronic during membrane formation and the phase behavior of membrane casting solution. The simulation results indicated that the difference of interaction between different components constituted the dominant reason for the different segregation performance of Pluronic; and the addition of Pluronic in casting solution resulted in larger reverse micelle, which might correspondingly lead to larger membrane pore appearing at membrane surface. Finally, the inherent relationship between the structural characteristics of block polymers and the anti-fouling ability of the membranes was studied; the guidance for the rational design and preparation of surface segregated ultrafiltration membrane was tentatively proposed.
引文
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