聚醚砜（PES）/醋酸纤维素（CA）共混膜的制备及其在MBR中抗污染性能的研究
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摘要
本文以聚醚砜(PES)为膜材料、二甲基乙酰胺(DMAc)为溶剂、聚乙烯吡咯烷酮(PVP)K30为添加剂,纯水与DMAc混合液为凝固液,通过不同含量的聚醚砜(14%、18%、20%、22%)、不同含量的聚乙烯吡咯烷酮(PVP)(8%、12%、14%、16%)得到不同制膜液组成,并由浸没沉淀相转化法制备不同铸膜液组成的超滤膜。对不同组成和温度条件下制膜液的粘度、膜的厚度和膜的力学性能等物理性能进行了测试与研究。用自制超滤装置测定了膜的纯水通量和截留率,用扫描电镜观察膜的表面形态和断面结构,研究了各影响因素对膜结构和性能的影响,从而得到本研究范围内最优制膜工艺,考察了具体因素对PES成膜过程中相分离行为以及最终膜结构的影响。
结果表明:随着聚醚砜含量的增大,膜厚度、断裂强度增大;膜的通量逐渐减少而截留率逐渐增大;膜表面结构孔隙率减少,孔径稍微变小。不同含量的聚乙烯吡咯烷酮对膜的性能结构有重要的影响,含量增大,膜的纯水通量增大,但降低了膜的截留能力。采用正交试验分析,得到本实验研究范围内最优聚醚砜制备条件:PES含量为18%,PVP含量为12%,凝固液温度为313K。
为进一步提高聚醚砜超滤膜的亲水性能,提高其抗污染性,对实验制备的聚醚砜膜进行了改性。在自制聚醚砜超滤膜的基础上,添加不同含量的醋酸纤维素进行共混改性,寻找最佳改性条件。主要考察了改性前后制膜液粘度和膜厚度的变化,通过表面接触角测定仪、扫描电镜、改性膜的纯水通量和截留性能等方法来表征改性前后的结构性能变化情况。研究表明:当醋酸纤维素的添加含量为2%时,改性膜的通量和截留率达到最佳状态,达到了改性的目的。
通过上述工艺制备的聚醚砜超滤膜,用于污水处理厂生活污水和工业废水的处理。本实验以松江新城污水处理厂曝气池的污水为实验用水。考察了改性前后的渗透通量,研究了超滤膜在去除废水中COD、浊度、色度等方面的性能。实验结果表明:渗透通量随运行时间而逐渐变小,但经过改性的膜通量减少幅度稍小;超滤膜对COD的去除率为80%以上,浊度的去除率为98%以上,对色度的去除为80%以上。从两种膜运行通量和清洗效果看,改性膜的稳定通量高于未改性膜的稳定通量,未改性膜和改性膜化学清洗后恢复率都达到78%以上。
为了更好的了解膜的运行情况,本文进一步从膜污染阻力方面进行了较为具体的分析,考察了活性污泥在膜生物反应器中过滤时两种不同膜阻力及各部分阻力所占比例,具体考察了膜过滤过程中,膜阻力的主要来源、组成及不同膜的阻力变化,具体分析了膜过滤过程中膜阻力的变化特性,膜过滤的短期运行和长期运行时膜阻力及各部分阻力所占比例的变化情况,分析了可能出现这些现象的原因,给予了适当的解释。
通过膜生物反应器中膜阻力的测定,考察了膜过滤过程中膜阻力的主要来源、组成及变化,具体分析了膜阻力的变化特性和污染成因,得出膜污染主要是由于浓差极化及凝胶层形成的;通过对活性污泥进行终端过滤来反映膜污染机理,判断出污泥的终端过滤过程严格符合沉积过滤定律;扫描电镜照片也证实了膜污染主要是膜面沉积层引起的。
本研究为聚醚砜膜成膜工艺优化和膜性能的改进及提高提供了参考依据,为聚醚砜在生活污水和工业废水中的应用提供了参考。
Polyethersulfone(PES) ultra filtration membranes were prepared from a series of casting with different composition by phase inversion process. Dimethylacetamide(DMAc)/Polyvinylpyrrolidone(PVP) K30 were used as casting solvent and water was used as coagulant.The resulting membranes prepared by changing the polymer concentration(in the range of 14-22wt%)and the ratio of PVP were characterized property,scanning electron microscope observations,measurements of water flux and rejection.Results showed that the flux of the membrane decreased while the separation performance for particle solutes increased with an increase in polymer concentration.This means that the outer skin layer of the membranes became apparently thicker and denser with increasing polymer concentration.On the other hand,an UF membrane from a dilute polymer solution produced a thin and porous skin layer,leading to a high value of flux but a relatively low percentage of rejection for PVP.The experimental parameters are investigated by using orthoanal experiment based on the experiment results;the optimized PES membrane is made.
In order to enhance the polyether sulfone ultra filter diaphragm's water affinity performance,enhances its anti-pollution however nature,to tested the polyether sulfone membrane which prepared to carry on the modification.In the self-made polyether sulfone ultra filter diaphragm's foundation,an increase different content's cellulose acetate carries on the blending modification,seeks for the best modified condition,changed the polyether sulfone membrane structure.Mainly inspected the cellulose acetate increase to the polyether sulfone performance structure influence, through superficial angle of contact methods and so on cryoscopy, scanning electron microscope,modified membrane's pure water flux and interception performance attributes around modified the structure performance change situation.Research surface:Increases the different cellulose acetate content through the test,has discovered when increases 2%cellulose acetate,the modified membrane's flux and the interception rate achieves the optimum condition,has served the modified purpose.
Through the above craft preparation's polyether sulfone ultra filter diaphragm,uses in the Sewage treatment plant sanitary sewage and industrial waste processing.This experiment as tests the water used take the Songjiang District new town Sewage treatment plant aeration tank's sewage.Inspected around the modified seepage flux,has studied the ultra filter diaphragm in the elimination waste water aspect and so on COD, turbidity,chromaticity performance.Experimental result surface:The seepage flux changes gradually along with the running time is small,but is slightly small after the modified membrane flux reduction scope;The ultra filter diaphragm to the COD elimination rate is above 80%,the turbidity elimination rate is above 98%,to the chromaticity elimination is above 80%.Andt after both membrane clean,the restoration ratio achieves above 78%.
The reason of the two membranes fouling is investigated by membrane resistance determination in membrane bio-reactor;it is found that membrane fouling mainly result from concentration polarization and gelatin layer.The dead-end filtration of sludge reflects the mechanism of membrane fouling,and it is in street conformity with the cake filtration law.It verifies the Membrane fouling is mainly caused by deposit on membrane surface to scan the electric mirror photo.
The research results provide a theory basis on the optimization of preparation for PES membrane and for the improvement of the membrane performance.It also provides a prospect for the application of ultra filtration membranes on wastewater treatment.
结果表明:随着聚醚砜含量的增大,膜厚度、断裂强度增大;膜的通量逐渐减少而截留率逐渐增大;膜表面结构孔隙率减少,孔径稍微变小。不同含量的聚乙烯吡咯烷酮对膜的性能结构有重要的影响,含量增大,膜的纯水通量增大,但降低了膜的截留能力。采用正交试验分析,得到本实验研究范围内最优聚醚砜制备条件:PES含量为18%,PVP含量为12%,凝固液温度为313K。
为进一步提高聚醚砜超滤膜的亲水性能,提高其抗污染性,对实验制备的聚醚砜膜进行了改性。在自制聚醚砜超滤膜的基础上,添加不同含量的醋酸纤维素进行共混改性,寻找最佳改性条件。主要考察了改性前后制膜液粘度和膜厚度的变化,通过表面接触角测定仪、扫描电镜、改性膜的纯水通量和截留性能等方法来表征改性前后的结构性能变化情况。研究表明:当醋酸纤维素的添加含量为2%时,改性膜的通量和截留率达到最佳状态,达到了改性的目的。
通过上述工艺制备的聚醚砜超滤膜,用于污水处理厂生活污水和工业废水的处理。本实验以松江新城污水处理厂曝气池的污水为实验用水。考察了改性前后的渗透通量,研究了超滤膜在去除废水中COD、浊度、色度等方面的性能。实验结果表明:渗透通量随运行时间而逐渐变小,但经过改性的膜通量减少幅度稍小;超滤膜对COD的去除率为80%以上,浊度的去除率为98%以上,对色度的去除为80%以上。从两种膜运行通量和清洗效果看,改性膜的稳定通量高于未改性膜的稳定通量,未改性膜和改性膜化学清洗后恢复率都达到78%以上。
为了更好的了解膜的运行情况,本文进一步从膜污染阻力方面进行了较为具体的分析,考察了活性污泥在膜生物反应器中过滤时两种不同膜阻力及各部分阻力所占比例,具体考察了膜过滤过程中,膜阻力的主要来源、组成及不同膜的阻力变化,具体分析了膜过滤过程中膜阻力的变化特性,膜过滤的短期运行和长期运行时膜阻力及各部分阻力所占比例的变化情况,分析了可能出现这些现象的原因,给予了适当的解释。
通过膜生物反应器中膜阻力的测定,考察了膜过滤过程中膜阻力的主要来源、组成及变化,具体分析了膜阻力的变化特性和污染成因,得出膜污染主要是由于浓差极化及凝胶层形成的;通过对活性污泥进行终端过滤来反映膜污染机理,判断出污泥的终端过滤过程严格符合沉积过滤定律;扫描电镜照片也证实了膜污染主要是膜面沉积层引起的。
本研究为聚醚砜膜成膜工艺优化和膜性能的改进及提高提供了参考依据,为聚醚砜在生活污水和工业废水中的应用提供了参考。
Polyethersulfone(PES) ultra filtration membranes were prepared from a series of casting with different composition by phase inversion process. Dimethylacetamide(DMAc)/Polyvinylpyrrolidone(PVP) K30 were used as casting solvent and water was used as coagulant.The resulting membranes prepared by changing the polymer concentration(in the range of 14-22wt%)and the ratio of PVP were characterized property,scanning electron microscope observations,measurements of water flux and rejection.Results showed that the flux of the membrane decreased while the separation performance for particle solutes increased with an increase in polymer concentration.This means that the outer skin layer of the membranes became apparently thicker and denser with increasing polymer concentration.On the other hand,an UF membrane from a dilute polymer solution produced a thin and porous skin layer,leading to a high value of flux but a relatively low percentage of rejection for PVP.The experimental parameters are investigated by using orthoanal experiment based on the experiment results;the optimized PES membrane is made.
In order to enhance the polyether sulfone ultra filter diaphragm's water affinity performance,enhances its anti-pollution however nature,to tested the polyether sulfone membrane which prepared to carry on the modification.In the self-made polyether sulfone ultra filter diaphragm's foundation,an increase different content's cellulose acetate carries on the blending modification,seeks for the best modified condition,changed the polyether sulfone membrane structure.Mainly inspected the cellulose acetate increase to the polyether sulfone performance structure influence, through superficial angle of contact methods and so on cryoscopy, scanning electron microscope,modified membrane's pure water flux and interception performance attributes around modified the structure performance change situation.Research surface:Increases the different cellulose acetate content through the test,has discovered when increases 2%cellulose acetate,the modified membrane's flux and the interception rate achieves the optimum condition,has served the modified purpose.
Through the above craft preparation's polyether sulfone ultra filter diaphragm,uses in the Sewage treatment plant sanitary sewage and industrial waste processing.This experiment as tests the water used take the Songjiang District new town Sewage treatment plant aeration tank's sewage.Inspected around the modified seepage flux,has studied the ultra filter diaphragm in the elimination waste water aspect and so on COD, turbidity,chromaticity performance.Experimental result surface:The seepage flux changes gradually along with the running time is small,but is slightly small after the modified membrane flux reduction scope;The ultra filter diaphragm to the COD elimination rate is above 80%,the turbidity elimination rate is above 98%,to the chromaticity elimination is above 80%.Andt after both membrane clean,the restoration ratio achieves above 78%.
The reason of the two membranes fouling is investigated by membrane resistance determination in membrane bio-reactor;it is found that membrane fouling mainly result from concentration polarization and gelatin layer.The dead-end filtration of sludge reflects the mechanism of membrane fouling,and it is in street conformity with the cake filtration law.It verifies the Membrane fouling is mainly caused by deposit on membrane surface to scan the electric mirror photo.
The research results provide a theory basis on the optimization of preparation for PES membrane and for the improvement of the membrane performance.It also provides a prospect for the application of ultra filtration membranes on wastewater treatment.
引文
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