基于纳米材料和含氟单体纳滤膜制备及其应用研究
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摘要
纳滤技术已经广泛应用于生物化学、制药、食品及染料等领域,如何提高膜的渗透性能已经成为纳滤膜研究的热点之一。本文采用界面聚合的方法制备复合纳滤膜,通过在聚合单体溶液中添加无机或有机材料,选择新型含氟单体等方法对膜的渗透性能进行优化,并将其用于染料废水处理及反渗透浓水软化等方面。本文研究结果如下：
首先,以聚醚砜(PES)超滤膜为基膜,利用界面聚合的方法制备了SiO2-聚哌嗪酰胺纳滤膜,研究了水相中添加硅溶胶的含量、单体浓度、反应时间等纳滤膜的制备条件及其对不同无机盐的截留性能；通过全反射红外(ATR-IR)研究膜表面的化学结构,利用扫描电镜(SEM)及原子力显微镜(AFM)观察膜表面的形态；在适宜的制膜条件下制备的聚哌嗪酰胺纳滤膜性能如下：操作压力0.6MPa,Na2SO4截留率97.4%,纯水通量46.8L·m-2·h-1；通过水相中添加硅溶胶,纳滤膜Na2SO4截留率变化不大,纯水通量增加了21.1%；根据纳滤膜对聚乙二醇(PEG)的截留测试,纳滤膜的截留分子量(MWCO)在600Da以下；在水相和有机相中分别添加SiO2、TiO2和Al2O3三种纳米颗粒,在相同的纳米颗粒与单体的比例下,有机相中添加纳米颗粒比水相中添加纳米颗粒表现出更好的性能；在水相中添加亲水性高分子聚合物聚乙烯苯磺酸钠(PSSS),膜的截留性能变化不大,渗透通量得到提高。
其次,以2,2-二(1-羟基-1-三氟甲基-2,2,2-三氟乙基)-4,4-亚甲基双苯胺(BHTTM)为水相单体,均苯三甲酰氯(TMC)为有机相单体,通过界面聚合的方法制备复合纳滤膜,研究了纳滤膜的制备条件并对纳滤膜的性能进行评估,采用ATR-IR、SEM及AFM等对膜进行了表征；当水相中含有1%(w/v)的BHTTM,有机相中含有0.15%(w/v)的TMC,将水相和有机相单体聚合10s,然后将其放入80℃下热处理5min制备含氟纳滤膜,操作压力0.6MPa,纳滤膜Na2SO4截留率85.3%,纯水通量10.1L·m~(-2)·h~(-1)；经过5000mg·L-1(ppm)(?)舌性氯处理1h后,纳滤膜Na2SO4截留率和纯水通量分别达到94.5%和94.8L·m~(-2)·h~(-1),处理前后纳滤膜对不同无机盐的截留率为Na2SO4>MgSO4> MgCl2>NaCl,该纳滤膜为荷负电纳滤膜。
在研究纳滤膜中添加硅溶胶及选择新型聚合单体后,为了进一步提高纳滤膜的渗透性能,实验以BHTTM为水相单体,TMC为有机相单体,通过水相中添加硅溶胶制备SiO_(2-)含氟纳滤膜；研究了纳滤膜制膜工艺条件并对其进行优化,在优化条件下,操作压力0.6MPa,纳滤膜对Na2SO4的截留率为85.0%,纯水通量为15.2L·m-2·h-1,相比于不添加纳米颗粒,膜的渗透性能有一定的提高；经过5000ppm活性氯处理1h后,纳滤膜Na2SO4截留率94.0%,纯水通量105L·m~(-2)·h~(-1)(17.5L·m-2·h-1·bar-1),相比于大多数纳滤膜的纯水通量(5-10L·m~(-2)·h~(-1)·bar~(-1)得到了很大的提升。
随后,以聚氯乙烯(PVC)中空纤维超滤为基膜,哌嗪(PIP)为水相单体,TMC为有机相单体,通过向有机相溶液中添加Si02纳米颗粒制备PVC-SiO2-聚哌嗪酰胺中空纤维纳滤膜,随着SiO2含量的增加,纳滤膜的渗透通量增大,截留率下降：随着聚合时间的增加,膜的分离性能提高,截留率增大,但是膜的渗透通量降低：以聚偏氟乙烯(PVDF)中空纤维超滤膜为基膜,将1%(w/v)的BHTTM水相单体和0.30%(w/v)的TMC有机相单体通过界面聚合制备了PVDF-含氟单体中空纤维纳滤膜,新制备的中空纤维纳滤膜在活性氯含量为500ppm的水溶液中进行氧化处理,纳滤膜有着较好的截留效果,当继续增加活性氯含量到3000ppm时,纳滤膜的截留性能和处理前差不多,但是渗透通量增加非常明显：以聚砜(PSf)中空纤维超滤膜为基膜,通过向水相单体溶液中添加硅溶胶成功制备了PSf-SiO2-聚哌嗪酰胺中空纤维纳滤膜。
最后,采用自制的Si02-聚哌嗪酰胺纳滤膜处理活性艳蓝X-BR染料废水,研究了不同操作条件下纳滤膜对染料废水处理效果：随着压力的升高,膜的渗透通量一直增大,而染料的截留率基本都在99.5%以上：随着染料浓度的增大,纳滤膜的渗透通量下降,但是染料的截留率随着染料浓度的增加而增大；在长时间处理染料过程中,纳滤膜稳定性能较好：此外,采用PSSS-聚哌嗪酰胺纳滤膜对模拟的反渗透浓水进行处理,研究了不同操作压力、温度及反渗透浓水的浓度对纳滤膜处理反渗透浓水效果的影响,在不同浓度的浓水中,三种离子的截留顺序为SO42->Mg2+>Ca2+:25℃时,Ca2+、Mg2+和SO_4~(2-)的截留率比40℃时Ca~(2+)、Mg~(2+)和SO_4~(2-)的截留率高,但是25℃纳滤膜的渗透通量明显低于40℃纳滤膜的渗透通量；随着模拟反渗透浓水的浓度增加,膜的渗透通量减小,截留率下降。
Nanofiltration technology has been widely used in biochemical, pharmaceutical, food and dye areas. How to improve the permeability of the NF membrane has become one of the hottest topics. In this paper, composite NF membranes were prepared by interfacial polymerization. In the preparation process of the NF membrane, the permeability of NF membranes had been optimization by added inorganic or organic materials in the polymerizable monomer solution or selected a new polymerization monomer. The optimization NF membranes were used in the dye wastewater treatment and reverse osmosis concentrated water softening. The conclusions were as follows:
Firstly, silica-polypiperazine-amide nanofiltration (NF) membranes were prepared by interfacial polymerization on polyethersulfone (PES) supporting membrane. Different preparation conditions and NF membrane performances were discussed, including silica concentrations, monomer concentrations, reaction time and salt rejections. The chemical structure characterizations of polyamide composite membrane were carried out by attenuated total reflectance infrared (ATR-IR). The surface images and cross sections were observed by scanning electron microscope (SEM) and atomic force microscopy (AFM). The results showed that polypiperazine-amide NF membrane prepared under the optimum conditions exhibited Na2SO4rejection of97.4%and water flux of46.8L·m-2·h-1. After added silica sol in the aqueous phase, the rejection of the resulting membrane changed slightly, but the water flux increased21.1%than polypiperazine-amide NF membrane. According to the rejection of polyethylene glycols (PEGs), the molecular weigh cut-off (MWCO) of the resulting membrane was under600Da. When the nanoparticles of SiO2, TiO2and Al2O3added in aqueous phase and organic phase respectively, the nanoparticles added in organic phase exhibited better performance than in aqueous phase. When the hydrophilic polymer compound of Poly(styrene sulfonic acid) sodium salt (PSSS) in the aqueous phase, the water flux was increased but the salt rejection was changed slightly.
Secondly, a novel composite nanofiltration (NF) membrane was prepared by interfacial polymerization of2,2'-bis(1-hydroxyl-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4'-methylene-dianiline (BHTTM) and trimesoyl chloride (TMC). Different preparation conditions and NF membrane performances were discussed. The membrane structures of composite NF membranes were characterized by ATR-IR, SEM and AFM. The BHTTM-TMC composite NF membrane was prepared under the condition:1%(w/v) BHTTM in the aqueous phase;0.15%TMC in the organic phase; reaction time for10s and curing temperature at80℃for5min. The optimum condition exhibited Na2SO4rejection of85.3%and the water flux of10.1L·m-2·h-1under0.6MPa. The NF membrane was treated by5000ppm chlorine solution for1h. The salt rejection and water flux of the treated membrane reached to94.5%and94.8L·m-2·h-1. The rejection of two NF membranes for inorganic electrolyte solutions decreased in the order of Na2SO4, MgSO4, MgCl2, NaCl, which were typical characteristics of negatively charged membranes.
The main objective of the research was to investigate the possibility of obtaining a membrane with high water flux. The composite polyamide NF membranes were prepared by interfacial polymerization of BHTTM and TMC with adding silica sol in aqueous phase. The performances of NF membranes were optimized by studying the preparation conditions. The results showed that the NF mrnbrane prepared under the optimum condition exhibited Na2SO4rejection of85.0%and the water flux of15.2L·m-2h-1under0.6MPa. Compared with the membrane not added nanoparticle in the aqueous phase, the permeability of silica-BHTTM-TMC NF membrane has improved. The NF membrane was treated by5000ppm chlorine solution for1h. The salt rejection and water flux of the treated membrane reached to94.0%and105L·m-2·h-1under0.6MPa (17.5L·m-2·h-1·bar-1). Compared to most other NF membrane water flux (5-10L·m-2·h-1·bar-1), the pure water flux has been greatly improved.
Then, the hollow fiber NF membranes were prepared according to the preparation conditions of the flat NF membranes. PVC-silica-polypiperazine-amide NF membranes were prepared by interfacial polymerization of PIP and TMC with adding silica nanoparticle in organic phase. The salt rejection decreased whereas water flux increased with the increased of silica concentration. As the reaction time increased, the water flux decreased and the rejection increased. On the basis of the fluoride flat NF Membrane, the fluoride hollow fiber NF membranes were prepared by interfacial polymerization of1%(w/v) BHTTM in the aqueous phase;0.30%TMC in the organic phase on PVDF hollow fiber ultrafiltration membrane. The hollow fiber NF membrane had a good rejection after treated by500ppm chlorine solution for1h. When the concentration of chlorine solution increased to3000ppm, the rejiection of NF membrane changed slightly, but the permeate flux increased very obviously. PSf-silica-polypiperazine-amide hollow fiber NF membranes were successfully prepared by added silica sol into the aqueous solution.
Finally, the reactive brilliant blue X-BR dye wastewater was treated by silica-polypiperazine-amide NF membranes, different operation conditions were discussed. With the increase of operation pressure, the permeate flux increased and the rejection of dye was above99.5%. When the feed dye concentration increased, the permeate flux decreased, but the rejection kept slightly increased. The NF membranes maintain permeability and selectivity after over10days of test, which showed excellent stability during the testing period. In addition, the RO concentrated water was treated by PSSS-polypiperazine-amide NF membranes. Different operation conditions and NF membrane performances were discussed, including operation pressure, temperature and salt concentrations. In different RO concentrated water concentration, the rejection of three kinds of ions decreased as per the order of SO42-, Mg2+and Ca2+. The salt rejection of Ca2+, Mg2+and SO42-kept on decreasing when the feed temperature was increased from25℃to40℃, while the permeate flux was increased. The salt rejection and permeate flux decreased with the increased of RO concentrated water concentration. Generally speaking, the NF membranes had a better treatment effect of dye wastewater and RO concentrated water.
首先,以聚醚砜(PES)超滤膜为基膜,利用界面聚合的方法制备了SiO2-聚哌嗪酰胺纳滤膜,研究了水相中添加硅溶胶的含量、单体浓度、反应时间等纳滤膜的制备条件及其对不同无机盐的截留性能；通过全反射红外(ATR-IR)研究膜表面的化学结构,利用扫描电镜(SEM)及原子力显微镜(AFM)观察膜表面的形态；在适宜的制膜条件下制备的聚哌嗪酰胺纳滤膜性能如下：操作压力0.6MPa,Na2SO4截留率97.4%,纯水通量46.8L·m-2·h-1；通过水相中添加硅溶胶,纳滤膜Na2SO4截留率变化不大,纯水通量增加了21.1%；根据纳滤膜对聚乙二醇(PEG)的截留测试,纳滤膜的截留分子量(MWCO)在600Da以下；在水相和有机相中分别添加SiO2、TiO2和Al2O3三种纳米颗粒,在相同的纳米颗粒与单体的比例下,有机相中添加纳米颗粒比水相中添加纳米颗粒表现出更好的性能；在水相中添加亲水性高分子聚合物聚乙烯苯磺酸钠(PSSS),膜的截留性能变化不大,渗透通量得到提高。
其次,以2,2-二(1-羟基-1-三氟甲基-2,2,2-三氟乙基)-4,4-亚甲基双苯胺(BHTTM)为水相单体,均苯三甲酰氯(TMC)为有机相单体,通过界面聚合的方法制备复合纳滤膜,研究了纳滤膜的制备条件并对纳滤膜的性能进行评估,采用ATR-IR、SEM及AFM等对膜进行了表征；当水相中含有1%(w/v)的BHTTM,有机相中含有0.15%(w/v)的TMC,将水相和有机相单体聚合10s,然后将其放入80℃下热处理5min制备含氟纳滤膜,操作压力0.6MPa,纳滤膜Na2SO4截留率85.3%,纯水通量10.1L·m~(-2)·h~(-1)；经过5000mg·L-1(ppm)(?)舌性氯处理1h后,纳滤膜Na2SO4截留率和纯水通量分别达到94.5%和94.8L·m~(-2)·h~(-1),处理前后纳滤膜对不同无机盐的截留率为Na2SO4>MgSO4> MgCl2>NaCl,该纳滤膜为荷负电纳滤膜。
在研究纳滤膜中添加硅溶胶及选择新型聚合单体后,为了进一步提高纳滤膜的渗透性能,实验以BHTTM为水相单体,TMC为有机相单体,通过水相中添加硅溶胶制备SiO_(2-)含氟纳滤膜；研究了纳滤膜制膜工艺条件并对其进行优化,在优化条件下,操作压力0.6MPa,纳滤膜对Na2SO4的截留率为85.0%,纯水通量为15.2L·m-2·h-1,相比于不添加纳米颗粒,膜的渗透性能有一定的提高；经过5000ppm活性氯处理1h后,纳滤膜Na2SO4截留率94.0%,纯水通量105L·m~(-2)·h~(-1)(17.5L·m-2·h-1·bar-1),相比于大多数纳滤膜的纯水通量(5-10L·m~(-2)·h~(-1)·bar~(-1)得到了很大的提升。
随后,以聚氯乙烯(PVC)中空纤维超滤为基膜,哌嗪(PIP)为水相单体,TMC为有机相单体,通过向有机相溶液中添加Si02纳米颗粒制备PVC-SiO2-聚哌嗪酰胺中空纤维纳滤膜,随着SiO2含量的增加,纳滤膜的渗透通量增大,截留率下降：随着聚合时间的增加,膜的分离性能提高,截留率增大,但是膜的渗透通量降低：以聚偏氟乙烯(PVDF)中空纤维超滤膜为基膜,将1%(w/v)的BHTTM水相单体和0.30%(w/v)的TMC有机相单体通过界面聚合制备了PVDF-含氟单体中空纤维纳滤膜,新制备的中空纤维纳滤膜在活性氯含量为500ppm的水溶液中进行氧化处理,纳滤膜有着较好的截留效果,当继续增加活性氯含量到3000ppm时,纳滤膜的截留性能和处理前差不多,但是渗透通量增加非常明显：以聚砜(PSf)中空纤维超滤膜为基膜,通过向水相单体溶液中添加硅溶胶成功制备了PSf-SiO2-聚哌嗪酰胺中空纤维纳滤膜。
最后,采用自制的Si02-聚哌嗪酰胺纳滤膜处理活性艳蓝X-BR染料废水,研究了不同操作条件下纳滤膜对染料废水处理效果：随着压力的升高,膜的渗透通量一直增大,而染料的截留率基本都在99.5%以上：随着染料浓度的增大,纳滤膜的渗透通量下降,但是染料的截留率随着染料浓度的增加而增大；在长时间处理染料过程中,纳滤膜稳定性能较好：此外,采用PSSS-聚哌嗪酰胺纳滤膜对模拟的反渗透浓水进行处理,研究了不同操作压力、温度及反渗透浓水的浓度对纳滤膜处理反渗透浓水效果的影响,在不同浓度的浓水中,三种离子的截留顺序为SO42->Mg2+>Ca2+:25℃时,Ca2+、Mg2+和SO_4~(2-)的截留率比40℃时Ca~(2+)、Mg~(2+)和SO_4~(2-)的截留率高,但是25℃纳滤膜的渗透通量明显低于40℃纳滤膜的渗透通量；随着模拟反渗透浓水的浓度增加,膜的渗透通量减小,截留率下降。
Nanofiltration technology has been widely used in biochemical, pharmaceutical, food and dye areas. How to improve the permeability of the NF membrane has become one of the hottest topics. In this paper, composite NF membranes were prepared by interfacial polymerization. In the preparation process of the NF membrane, the permeability of NF membranes had been optimization by added inorganic or organic materials in the polymerizable monomer solution or selected a new polymerization monomer. The optimization NF membranes were used in the dye wastewater treatment and reverse osmosis concentrated water softening. The conclusions were as follows:
Firstly, silica-polypiperazine-amide nanofiltration (NF) membranes were prepared by interfacial polymerization on polyethersulfone (PES) supporting membrane. Different preparation conditions and NF membrane performances were discussed, including silica concentrations, monomer concentrations, reaction time and salt rejections. The chemical structure characterizations of polyamide composite membrane were carried out by attenuated total reflectance infrared (ATR-IR). The surface images and cross sections were observed by scanning electron microscope (SEM) and atomic force microscopy (AFM). The results showed that polypiperazine-amide NF membrane prepared under the optimum conditions exhibited Na2SO4rejection of97.4%and water flux of46.8L·m-2·h-1. After added silica sol in the aqueous phase, the rejection of the resulting membrane changed slightly, but the water flux increased21.1%than polypiperazine-amide NF membrane. According to the rejection of polyethylene glycols (PEGs), the molecular weigh cut-off (MWCO) of the resulting membrane was under600Da. When the nanoparticles of SiO2, TiO2and Al2O3added in aqueous phase and organic phase respectively, the nanoparticles added in organic phase exhibited better performance than in aqueous phase. When the hydrophilic polymer compound of Poly(styrene sulfonic acid) sodium salt (PSSS) in the aqueous phase, the water flux was increased but the salt rejection was changed slightly.
Secondly, a novel composite nanofiltration (NF) membrane was prepared by interfacial polymerization of2,2'-bis(1-hydroxyl-1-trifluoromethyl-2,2,2-trifluoroethyl)-4,4'-methylene-dianiline (BHTTM) and trimesoyl chloride (TMC). Different preparation conditions and NF membrane performances were discussed. The membrane structures of composite NF membranes were characterized by ATR-IR, SEM and AFM. The BHTTM-TMC composite NF membrane was prepared under the condition:1%(w/v) BHTTM in the aqueous phase;0.15%TMC in the organic phase; reaction time for10s and curing temperature at80℃for5min. The optimum condition exhibited Na2SO4rejection of85.3%and the water flux of10.1L·m-2·h-1under0.6MPa. The NF membrane was treated by5000ppm chlorine solution for1h. The salt rejection and water flux of the treated membrane reached to94.5%and94.8L·m-2·h-1. The rejection of two NF membranes for inorganic electrolyte solutions decreased in the order of Na2SO4, MgSO4, MgCl2, NaCl, which were typical characteristics of negatively charged membranes.
The main objective of the research was to investigate the possibility of obtaining a membrane with high water flux. The composite polyamide NF membranes were prepared by interfacial polymerization of BHTTM and TMC with adding silica sol in aqueous phase. The performances of NF membranes were optimized by studying the preparation conditions. The results showed that the NF mrnbrane prepared under the optimum condition exhibited Na2SO4rejection of85.0%and the water flux of15.2L·m-2h-1under0.6MPa. Compared with the membrane not added nanoparticle in the aqueous phase, the permeability of silica-BHTTM-TMC NF membrane has improved. The NF membrane was treated by5000ppm chlorine solution for1h. The salt rejection and water flux of the treated membrane reached to94.0%and105L·m-2·h-1under0.6MPa (17.5L·m-2·h-1·bar-1). Compared to most other NF membrane water flux (5-10L·m-2·h-1·bar-1), the pure water flux has been greatly improved.
Then, the hollow fiber NF membranes were prepared according to the preparation conditions of the flat NF membranes. PVC-silica-polypiperazine-amide NF membranes were prepared by interfacial polymerization of PIP and TMC with adding silica nanoparticle in organic phase. The salt rejection decreased whereas water flux increased with the increased of silica concentration. As the reaction time increased, the water flux decreased and the rejection increased. On the basis of the fluoride flat NF Membrane, the fluoride hollow fiber NF membranes were prepared by interfacial polymerization of1%(w/v) BHTTM in the aqueous phase;0.30%TMC in the organic phase on PVDF hollow fiber ultrafiltration membrane. The hollow fiber NF membrane had a good rejection after treated by500ppm chlorine solution for1h. When the concentration of chlorine solution increased to3000ppm, the rejiection of NF membrane changed slightly, but the permeate flux increased very obviously. PSf-silica-polypiperazine-amide hollow fiber NF membranes were successfully prepared by added silica sol into the aqueous solution.
Finally, the reactive brilliant blue X-BR dye wastewater was treated by silica-polypiperazine-amide NF membranes, different operation conditions were discussed. With the increase of operation pressure, the permeate flux increased and the rejection of dye was above99.5%. When the feed dye concentration increased, the permeate flux decreased, but the rejection kept slightly increased. The NF membranes maintain permeability and selectivity after over10days of test, which showed excellent stability during the testing period. In addition, the RO concentrated water was treated by PSSS-polypiperazine-amide NF membranes. Different operation conditions and NF membrane performances were discussed, including operation pressure, temperature and salt concentrations. In different RO concentrated water concentration, the rejection of three kinds of ions decreased as per the order of SO42-, Mg2+and Ca2+. The salt rejection of Ca2+, Mg2+and SO42-kept on decreasing when the feed temperature was increased from25℃to40℃, while the permeate flux was increased. The salt rejection and permeate flux decreased with the increased of RO concentrated water concentration. Generally speaking, the NF membranes had a better treatment effect of dye wastewater and RO concentrated water.
引文
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