改性超滤膜去除水中天然有机物的研究
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摘要
天然有机物（Natural Organic Matter，NOM）广泛存在于地表和地下水中，是多种消毒副产物的前驱物。如何有效地去除水中NOM对于提高给水水质、满足日益严格的饮用水标准具有重要意义。超滤（Ultrafiltration，UF）能有效去除水中的悬浮颗粒、胶体杂质、微生物、细菌病毒和一定量的可溶性有机物，是替代传统饮用水处理技术的理想选择，目前正在饮用水处理领域得到广泛应用。然而，由于超滤膜的截留分子量较大，导致它不能有效地去除水中的NOM。同时，膜污染问题是制约其广泛应用的另一个原因。
本研究通过对再生纤维素膜（Regenerated Cellulose，RC）进行荷电改性，比较中性膜和荷电超滤膜对水中NOM的去除率和膜通量的衰减情况。考察膜改性的荷电量、截留分子量、膜材料和NOM的不同组分对荷电超滤过程的影响。此外，还研究了溶液pH值、离子强度和代表水体硬度的钙离子浓度等溶液环境因素对荷电超滤行为的影响。最后进一步比较了荷电超滤膜与纳滤膜对水中NOM的去除效果。
为了获得更加耐用、抗污染的超滤膜，本研究还通过添加聚乙二醇（Polyethylene Glycol，PEG）、氯化锂（LiCl）和二氧化钛（TiO_2）等添加剂，制备并表征了改性后的聚偏氟乙烯（Polyvinylidene Fluoride，PVDF）超滤膜。在死端过滤和错流过滤的实验条件下，研究了不同种类的改性PVDF超滤膜对水中NOM的去除率和膜通量的衰减情况。同时，重点考察了TiO_2改性后的PVDF超滤膜的光催化性能。
研究结果表明，对中性RC膜进行荷电改性，在传统筛分机理和静电相互作用力的共同作用下，可以有效提高截留率，同时减轻膜污染。对比实验结果表明，在去除水中NOM的应用环境中，荷电超滤膜具备替代纳滤膜的技术可行性。膜的截留分子量、改性后的荷电量、膜材料的性质以及NOM组分的亲疏水性对荷电超滤过程有着重要影响。此外，溶液环境因素同样影响荷电超滤膜的性能。尽管溶液环境因素对中性膜和荷电超滤膜的截留率和膜通量衰减的影响幅度不同，但趋势基本一致。水体的pH值通过质子化作用影响NOM分子和荷电膜表面的荷电量。水体的离子强度影响NOM分子的物理化学性质，改变NOM分子的形状以及膜表面的静电屏蔽作用力。代表水体硬度的钙离子浓度影响膜与NOM分子的静电相互作用力的大小以及膜表面滤饼层的致密/疏松程度。所以，在应用超滤膜去除水中天然有机物的过程中，不仅要考察膜本身的性质（如截留分子量、荷电量、膜材料的亲疏水性），还要考虑溶液环境等诸多影响因素，以便在提高截留率的同时，减轻膜污染。
在研究具有光催化性能的TiO_2改性PVDF超滤膜的制备与改性实验中，研究结果表明，将TiO_2纳米颗粒按适当比例添加到PVDF膜中，可以有效提高截留率，同时减轻膜污染。TiO_2纳米颗粒的添加可以改善PVDF膜的亲水性，同时提高截留率。TiO_2改性PVDF膜在光催化条件下还具有良好的自清洁性能。光催化条件下的TiO_2改性PVDF膜在错流过滤实验中，污染物在膜表面的沉积与污染物的光催化降解这两种过程可能会达到一种平衡状态。对于TiO_2光催化膜，UV辐照有望成为一种新的膜清洗方法。与传统的物理化学清洗方法相比，这种新型膜清洗方法具有节能环保、高效彻底以及无二次污染等优点，技术应用前景广阔。
Natural organic matter (NOM) is commonly found in surface and ground waterand considered to react with the major disinfectants to produce a host of disinfectionby-products (DBPs). Therefore, the removal of NOM effectively is of significantimportance in meeting the stringent DBPs regulations and providing safe drinkingwater. Ultrafiltration (UF) allows the removal of particle, colloids, microorganism,variety of water born viruses, and certain amount of the dissolved organic matter. Ithas proved to be one of the best alternatives replacing conventional drinking watertreatment technologies and is increasingly used in drinking water treatment. However,UF is not very effectively to remove NOM due to the comparatively larger pore sizecompared with the size of NOM. Membrane fouling is another factor which restrictsits widespread application.
In this study, the effect of charge modification of regenerated cellulose (RC)membrane was studied by discussing NOM removal and flux decline with neutral andnegatively charged version of RC membranes. Effects of the membrane charge,molecular weight cut-off (MWCO), membrane material and NOM fractions on NOMremoval and flux decline with charged UF membranes were also investigated. Inaddition, solution environment, including pH, ionic strength and calcium ionconcentration, affecting NOM removal and flux decline were evaluated. Furthermore,the performance of charge modified UF membrane and nanofiltration (NF) membraneon NOM removal and flux decline was compared.
In order to get UF membranes with better durability and anti-fouling properties,the modified polyvinylidene fluoride (PVDF) membranes were prepared andcharacterized by adding different amounts of polyethylene glycol (PEG), LiCl andTiO_2particles. The performances of different kinds of modified PVDF membranes were investigated by discussing NOM removal and flux decline in both dead-end andcross-flow filtration experiments. The effect of photocatalytic degradation onTiO_2-doped PVDF membranes was also evaluated.
Results indicated that the appropriate charge modification on the neutral RCmembrane could be an effective way for better removal of NOM and reduction of themembrane fouling due to the electrostatic interaction with the combination effect ofmembrane pore size. Charge modified RC membrane could be potentially used toreplace NF membrane on the aspect of NOM removal. The membrane charge,membrane MWCO，membrane material and NOM fractions had some importanteffects on charged UF process. Besides, the extent of flux decline and removal on thecharged RC membrane was also found to be strongly governed by solutionenvironment. Though the degrees of the effects were not the same, the trends of theeffect of solution environment on the NOM removal and fouling were same on bothneutral and negatively charged membrane. The pH value would affect the net chargeof membrane and NOM molecules through the protonation effect. The ionic strengthwould affect the physical and chemical properties of NOM molecules and theelectrostatic shielding on membrane surface. The effect of calcium concentration onNOM removal and flux decline was due to both the electrostatic interaction and thepermeability of the cake layer formed on the membrane. In the application of UFprocess for NOM removal, one has to consider not only the properties of membraneitself (including MWCO, membrane charge, hydrophobicity and material), but alsothe solution environment, to achieve better NOM removal rate and less membranefouling.
Results also indicated that the appropriate TiO_2-doped modification on PVDFmembrane could be an effective way for better removal of NOM and reduction ofmembrane fouling at the same time. The addition of TiO_2nanoparticles can improvethe hydrophilicity of PVDF membrane and increase the removal rate of testingmolecule pepsin. Compared with PVDF membrane, TiO_2-doped PVDF membraneincreases NOM removal and at the same time decreases the flux decline, which is due to smaller membrane pores, and more hydrophilic and smoother membrane surface.TiO_2-doped PVDF membrane has self-cleaning ability offered by photocatalysis. Asto TiO_2-doped PVDF membrane, an equilibrium might be reached between thefoulants deposited on the membrane surface and photocatalytic degradation of thefoulants during cross-flow UF coupled with photocatalysis. UV irradiation might be anew kind of membrane cleaning method for TiO_2photocatalytic membranes.Compared with conventional physical and chemical cleaning methods, this novelmembrane cleaning method provides advantages of energy saving, high efficiency andno second-pollution, which indicates great potential for applications.
本研究通过对再生纤维素膜（Regenerated Cellulose，RC）进行荷电改性，比较中性膜和荷电超滤膜对水中NOM的去除率和膜通量的衰减情况。考察膜改性的荷电量、截留分子量、膜材料和NOM的不同组分对荷电超滤过程的影响。此外，还研究了溶液pH值、离子强度和代表水体硬度的钙离子浓度等溶液环境因素对荷电超滤行为的影响。最后进一步比较了荷电超滤膜与纳滤膜对水中NOM的去除效果。
为了获得更加耐用、抗污染的超滤膜，本研究还通过添加聚乙二醇（Polyethylene Glycol，PEG）、氯化锂（LiCl）和二氧化钛（TiO_2）等添加剂，制备并表征了改性后的聚偏氟乙烯（Polyvinylidene Fluoride，PVDF）超滤膜。在死端过滤和错流过滤的实验条件下，研究了不同种类的改性PVDF超滤膜对水中NOM的去除率和膜通量的衰减情况。同时，重点考察了TiO_2改性后的PVDF超滤膜的光催化性能。
研究结果表明，对中性RC膜进行荷电改性，在传统筛分机理和静电相互作用力的共同作用下，可以有效提高截留率，同时减轻膜污染。对比实验结果表明，在去除水中NOM的应用环境中，荷电超滤膜具备替代纳滤膜的技术可行性。膜的截留分子量、改性后的荷电量、膜材料的性质以及NOM组分的亲疏水性对荷电超滤过程有着重要影响。此外，溶液环境因素同样影响荷电超滤膜的性能。尽管溶液环境因素对中性膜和荷电超滤膜的截留率和膜通量衰减的影响幅度不同，但趋势基本一致。水体的pH值通过质子化作用影响NOM分子和荷电膜表面的荷电量。水体的离子强度影响NOM分子的物理化学性质，改变NOM分子的形状以及膜表面的静电屏蔽作用力。代表水体硬度的钙离子浓度影响膜与NOM分子的静电相互作用力的大小以及膜表面滤饼层的致密/疏松程度。所以，在应用超滤膜去除水中天然有机物的过程中，不仅要考察膜本身的性质（如截留分子量、荷电量、膜材料的亲疏水性），还要考虑溶液环境等诸多影响因素，以便在提高截留率的同时，减轻膜污染。
在研究具有光催化性能的TiO_2改性PVDF超滤膜的制备与改性实验中，研究结果表明，将TiO_2纳米颗粒按适当比例添加到PVDF膜中，可以有效提高截留率，同时减轻膜污染。TiO_2纳米颗粒的添加可以改善PVDF膜的亲水性，同时提高截留率。TiO_2改性PVDF膜在光催化条件下还具有良好的自清洁性能。光催化条件下的TiO_2改性PVDF膜在错流过滤实验中，污染物在膜表面的沉积与污染物的光催化降解这两种过程可能会达到一种平衡状态。对于TiO_2光催化膜，UV辐照有望成为一种新的膜清洗方法。与传统的物理化学清洗方法相比，这种新型膜清洗方法具有节能环保、高效彻底以及无二次污染等优点，技术应用前景广阔。
Natural organic matter (NOM) is commonly found in surface and ground waterand considered to react with the major disinfectants to produce a host of disinfectionby-products (DBPs). Therefore, the removal of NOM effectively is of significantimportance in meeting the stringent DBPs regulations and providing safe drinkingwater. Ultrafiltration (UF) allows the removal of particle, colloids, microorganism,variety of water born viruses, and certain amount of the dissolved organic matter. Ithas proved to be one of the best alternatives replacing conventional drinking watertreatment technologies and is increasingly used in drinking water treatment. However,UF is not very effectively to remove NOM due to the comparatively larger pore sizecompared with the size of NOM. Membrane fouling is another factor which restrictsits widespread application.
In this study, the effect of charge modification of regenerated cellulose (RC)membrane was studied by discussing NOM removal and flux decline with neutral andnegatively charged version of RC membranes. Effects of the membrane charge,molecular weight cut-off (MWCO), membrane material and NOM fractions on NOMremoval and flux decline with charged UF membranes were also investigated. Inaddition, solution environment, including pH, ionic strength and calcium ionconcentration, affecting NOM removal and flux decline were evaluated. Furthermore,the performance of charge modified UF membrane and nanofiltration (NF) membraneon NOM removal and flux decline was compared.
In order to get UF membranes with better durability and anti-fouling properties,the modified polyvinylidene fluoride (PVDF) membranes were prepared andcharacterized by adding different amounts of polyethylene glycol (PEG), LiCl andTiO_2particles. The performances of different kinds of modified PVDF membranes were investigated by discussing NOM removal and flux decline in both dead-end andcross-flow filtration experiments. The effect of photocatalytic degradation onTiO_2-doped PVDF membranes was also evaluated.
Results indicated that the appropriate charge modification on the neutral RCmembrane could be an effective way for better removal of NOM and reduction of themembrane fouling due to the electrostatic interaction with the combination effect ofmembrane pore size. Charge modified RC membrane could be potentially used toreplace NF membrane on the aspect of NOM removal. The membrane charge,membrane MWCO，membrane material and NOM fractions had some importanteffects on charged UF process. Besides, the extent of flux decline and removal on thecharged RC membrane was also found to be strongly governed by solutionenvironment. Though the degrees of the effects were not the same, the trends of theeffect of solution environment on the NOM removal and fouling were same on bothneutral and negatively charged membrane. The pH value would affect the net chargeof membrane and NOM molecules through the protonation effect. The ionic strengthwould affect the physical and chemical properties of NOM molecules and theelectrostatic shielding on membrane surface. The effect of calcium concentration onNOM removal and flux decline was due to both the electrostatic interaction and thepermeability of the cake layer formed on the membrane. In the application of UFprocess for NOM removal, one has to consider not only the properties of membraneitself (including MWCO, membrane charge, hydrophobicity and material), but alsothe solution environment, to achieve better NOM removal rate and less membranefouling.
Results also indicated that the appropriate TiO_2-doped modification on PVDFmembrane could be an effective way for better removal of NOM and reduction ofmembrane fouling at the same time. The addition of TiO_2nanoparticles can improvethe hydrophilicity of PVDF membrane and increase the removal rate of testingmolecule pepsin. Compared with PVDF membrane, TiO_2-doped PVDF membraneincreases NOM removal and at the same time decreases the flux decline, which is due to smaller membrane pores, and more hydrophilic and smoother membrane surface.TiO_2-doped PVDF membrane has self-cleaning ability offered by photocatalysis. Asto TiO_2-doped PVDF membrane, an equilibrium might be reached between thefoulants deposited on the membrane surface and photocatalytic degradation of thefoulants during cross-flow UF coupled with photocatalysis. UV irradiation might be anew kind of membrane cleaning method for TiO_2photocatalytic membranes.Compared with conventional physical and chemical cleaning methods, this novelmembrane cleaning method provides advantages of energy saving, high efficiency andno second-pollution, which indicates great potential for applications.
引文
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