羧甲基纤维素钠、海藻酸钠及壳聚糖磷酸酯复合纳滤膜的研究
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摘要
本文选用具有良好成膜性的羧甲基纤维素钠（CMC）、海藻酸钠（ALG）和壳聚糖的水溶性衍生物-壳聚糖磷酸酯（PCS）为复合纳滤膜表面活性层材料，戊二醛（GA）、环氧氯丙烷（ECH）和CuSO4溶液作为交联剂，聚砜（PSF）超滤膜为支撑层，利用涂敷交联的方法，制备了五种新型荷负电复合纳滤膜。利用衰减全反射红外光谱（ATR-IR）、扫描电子电镜（SEM）和原子力显微镜(AFM)对复合膜结构形貌进行了表征。研究了复合纳滤（NF）膜的最佳制备条件及操作条件对膜截留性能的影响。在铸膜液中添加适量的有机小分子或无机盐小分子，测得其对复合NF膜截留性能的影响。
以羧甲基纤维素钠（CMC）为表面活性层材料，聚砜（PSF）超滤膜为基膜，戊二醛（GA）水溶液为交联剂，制得一种新型荷负电复合纳滤膜。其最佳制备条件为：羧甲基纤维素钠浓度为1%，戊二醛浓度为0.5%，稀硫酸催化条件下，30℃下交联2h。在室温下，复合膜接触角为57.85°，说明其表面亲水性比聚砜膜有很大提高。溶胀度为44.26%，截留分子量约为520Da。在操作压力为1MPa，料液流量为40L·h~(-1)时，对1000mg·L~(-1)K_2SO_4、Na_2SO_4、KCl、NaCl、MgSO4和MgCl_2溶液的截留率分别为98.3、98.0、62.5、59.1、54.4和24.6%，膜通量分别为10.0、10.1、15.2、15.8、13.7和16.5L·m~(-2)· h~(-1)。CMC/PSF复合膜对几种无机盐的截留顺序为：Na_2SO_4> NaCl> MgSO_4> MgCl_2。
以羧甲基纤维素钠（CMC）和海藻酸钠（ALG）共混液为表面活性层材料，聚砜（PSF）超滤膜为基膜，环氧氯丙烷（ECH）的乙醇溶液（调节pH=10）为交联剂，制得一种新型共混复合纳滤膜。其最佳制备条件为：ALG/CMC共混比为1:3，交联剂环氧氯丙烷浓度为2%，在温度50℃交联18h。在操作压力为1MPa，料液流量为30L·h~(-1)时，对1000mg·L~(-1)K_2SO_4、Na_2SO_4、KCl、NaCl、MgSO_4和MgCl_2溶液的截留率分别为97.4、97.1、58.9、55.1、51.6和24.6%，膜通量分别为17.1、17.3、16.9、17.2、16.0和16.6L·m~(-2)· h~(-1)。该纳滤膜对不同无机盐的截留性能不同，具有典型的荷负电膜截留特性，这主要决定于荷电膜与电解质离子之间的静电作用力。
通过对壳聚糖改性制备了水溶性的壳聚糖磷酸酯（PCS）。以PCS水溶液为铸膜液材料，PSF超滤膜为基膜，ECH为交联剂，用涂敷交联的方法制备了PCS/PSF复合纳滤膜，对其结构和形貌进行了表征。研究了活性层铸膜液的组成、交联剂浓度等因素对复合膜截留性能的影响。制备的PCS/PSF复合纳滤膜在操作压力为1MPa，料液流量为40L·h~(-1)时，对1000mg·L~(-1)Na_2SO_4和NaCl溶液的截留率分别为89.2、20.8%，通量分别为6.9、7.4L·m~(-2)· h~(-1)。复合膜对几种无机盐的截留顺序为：Na_2SO_4> MgSO_4> NaCl> MgCl_2。
以PCS为表面活性层材料，PSF超滤膜为基膜，GA为交联剂，制备了一种新型PCS/PSF复合纳滤膜。其最佳制备条件为：壳聚糖磷酸酯PCS溶液浓度为2%，GA浓度为0.5%，在50℃下交联1.5h。复合膜对1000mg·L~(-1)Na_2SO_4溶液的截留率和通量分别为87.6%和8.3L·m~(-2)· h~(-1)。对无机盐的截留顺序为：Na_2SO_4>MgSO_4> NaCl> MgCl_2。研究了操作条件和有机小分子添加剂对复合膜截留性能的影响。在室温下，复合膜接触角为56.20°，溶胀度为44.07%，截留分子量约为510Da。
以PCS为表面活性层材料，聚砜（PSF）为支撑层，CuSO4为螯合剂，成功制备了一种新型离子交联PCS/PSF复合纳滤膜。其最佳制备条件为：壳聚糖磷酸酯（PCS）水溶液浓度为1.5%，CuSO_4浓度为4%，在40℃下交联2h。复合膜对1000mg·L~(-1)Na_2SO_4溶液的截留率和通量分别为85.5%和7.4L·m~(-2)· h~(-1)。膜的截留分子量约为580Da，接触角为58.46°。
用戊二醛交联的壳聚糖磷酸酯（PCS）/聚砜（PSF）复合纳滤膜对某污水处理厂中水进行了深度处理应用研究，对影响纳滤过程的因素，如操作压力、工作流量和运行时间进行了考察。测定在这些条件下，其对膜通量的影响以及对CODCr等的去除率（R）。结果表明，在操作压力为1MPa，进料液流量为40L·h~(-1)时，复合膜对总磷的去除率（R）>85.0%，对CODCr、氨氮及电导率的去除率（R）分别为76.2、69.8和33.2%，对色度的去除率为100%。经过膜法深度处理之后，出水各项指标都可以达到GB18918~(-2)002一级A的排放标准。
Sodium carboxymethyl cellulose (CMC), sodium alginate (ALG) andphosphorylated chitosan (PCS) were explored as the active layer materials forcomposite nanofiltration (NF) membranes in this study. A series of negatively chargedcomposite NF membranes were prepared through coating the casting solution ontoPSF matrix, and then cross-linked with glutaraldehyde (GA), epichlorohydrin (ECH),or CuSO4, repectively. The membranes were characterized by scanning electronmicroscopy (SEM), attenuated total reflection infrared spectroscopy (ATR-IR) andatomic force microscopy (AFM). Effects of membrane making conditions,low-molecular-weight organic additives in the casting solution and operatingconditions on performance of the composite membranes were also investigated.
A negatively charged composite NF membrane was prepared using CMC assurface active layer, PSF matrix as support layer, cross-linked with GA. The resultsindicated that the composite membrane with excellent rejection performance shouldbe prepared while CMC concentration1%, GA concentration0.5%, cross-linking time2h at30℃. At room temperature, the contact angle is57.85°, degree of swelling44.26%, and its molecular weight cut-off is520Da. At1MPa and40L·h~(-1)feed flow,the rejections of the composite membrane to1000mg·L~(-1)K_2SO_4, Na_2SO_4, KCl, NaCl,MgSO4and MgCl_2were98.3,98.0,62.5,59.1,54.4and24.6%, with a flux of10.0,10.1,15.2,15.8,13.7and16.5L· m~(-2)· h~(-1), respectively. The rejection rate of themembrane to different electrolyte solutions decreased in the order of Na_2SO_4, NaCl,MgSO4and MgCl_2.
A blend composite NF membrane was prepared using CMC and ALG blend assurface active layer, PSF as support layer, cross-linked with ECH at pH=10. Thecomposite membrane with excellent rejection performance should be prepared whileALG/CMC proportion1:3, ECH concentration2%, cross-linking time18h at50℃. At1MPa and30L·h~(-1)feed flow, the rejections of the composite membrane to1000mg·L~(-1) K_2SO_4, Na_2SO_4, KCl, NaCl, MgSO4and MgCl_2were97.4,97.1,58.9,55.1,51.6and24.6%, with a flux of17.1,17.3,16.9,17.2,16.0and16.6L· m~(-2)· h~(-1), respectively. Theresults indicate that the composite NF membrane has different rejection ratio todifferent kinds of inorganic salts. Similar to other negative charged membranes, therejection performance of the composite membrane depends on the electrostatic forcebetween the charged membrane and ions of electrolyte.
The water soluble PCS with D.C. of0.78was prepared through a modified andhomogeneous method. A novel kind of composite NF membrane was prepared usingPCS as surface active layer, PSF as support layer, cross-linked with ECH. Themembrane preparation techniques on the performance of the composite membranewere investigated. The results suggest that the composite membrane with excellentrejection performance should be prepared while PCS concentration1.5%, ECHconcentration1%, cross-linking time22h at60℃. The structure and morphology ofthe resulting membrane were characterized by ATR-IR, SEM, and AFM. At1MPa and40L·h~(-1)feed flow, the rejections of the NF membrane to1000mg·L~(-1)Na_2SO_4andNaCl were89.2and20.8%, respectively. The flux were6.9and7.4L· m~(-2)· h~(-1). Therejections of the membrane to different electrolyte solutions decreased in the order ofNa_2SO_4, MgSO4, NaCl and MgCl_2.
The PCS/PSF composite NF membrane was prepared using PCS as surfaceactive layer, PSF as support layer, cross-linked with GA. The results suggest that thecomposite membrane with excellent rejection performance should be prepared whilePCS concentration2%, GA concentration0.5%, cross-linking time1.5h at50℃.At1MPa and40L·h~(-1)feed flow, the rejection and flux of the NF membrane to1000mg·L~(-1)Na_2SO_4was87.6%and8.3L· m~(-2)· h~(-1), respectively. The rejections of thiskind of membrane to the electrolyte solutions decreased in the order of Na_2SO_4,MgSO4, NaCl and MgCl_2. The preparation techniques on the performance of thecomposite membrane were investigated. At room temperature, the contact angle is56.20°, degree of swelling44.07%, and its molecular weight cut-off510Da.
A novel PCS/PSF composite membrane was prepared using PCS as surfaceactive layer, PSF as support layer, cross-linked with CuSO4. The composite membranewith excellent rejection performance should be prepared while PCS concentration1.5%, CuSO4concentration4%, cross-linking time2h at40℃. At1MPa and40L·h~(-1)feed flow, the rejection and flux of the NF membrane to1000mg·L~(-1)Na_2SO_4was85.5%and7.4L· m~(-2)· h~(-1), respectively. The contact angle is58.46°and molecular weight cut-off580Da.
The GA cross-linked PCS/PSF composite membrane was used in reclaimedwater treatment of a waste water plant. The permeate flux and the removalefficiencies in color, CODCr, TP, NH3and conductivity were investigated in relationto the driving pressure, the feed flow, and the operation time. At the pressure of1MPaand40L·h~(-1)feed flow, the removal efficiencies for color, CODCr, TP, NH3andconductivity were100,76.2,85.2,69.8and33.2%, respectively. After membraneprocess treatment, all the indexes of permeate reached A level standard ofGB18918~(-2)002.
以羧甲基纤维素钠（CMC）为表面活性层材料，聚砜（PSF）超滤膜为基膜，戊二醛（GA）水溶液为交联剂，制得一种新型荷负电复合纳滤膜。其最佳制备条件为：羧甲基纤维素钠浓度为1%，戊二醛浓度为0.5%，稀硫酸催化条件下，30℃下交联2h。在室温下，复合膜接触角为57.85°，说明其表面亲水性比聚砜膜有很大提高。溶胀度为44.26%，截留分子量约为520Da。在操作压力为1MPa，料液流量为40L·h~(-1)时，对1000mg·L~(-1)K_2SO_4、Na_2SO_4、KCl、NaCl、MgSO4和MgCl_2溶液的截留率分别为98.3、98.0、62.5、59.1、54.4和24.6%，膜通量分别为10.0、10.1、15.2、15.8、13.7和16.5L·m~(-2)· h~(-1)。CMC/PSF复合膜对几种无机盐的截留顺序为：Na_2SO_4> NaCl> MgSO_4> MgCl_2。
以羧甲基纤维素钠（CMC）和海藻酸钠（ALG）共混液为表面活性层材料，聚砜（PSF）超滤膜为基膜，环氧氯丙烷（ECH）的乙醇溶液（调节pH=10）为交联剂，制得一种新型共混复合纳滤膜。其最佳制备条件为：ALG/CMC共混比为1:3，交联剂环氧氯丙烷浓度为2%，在温度50℃交联18h。在操作压力为1MPa，料液流量为30L·h~(-1)时，对1000mg·L~(-1)K_2SO_4、Na_2SO_4、KCl、NaCl、MgSO_4和MgCl_2溶液的截留率分别为97.4、97.1、58.9、55.1、51.6和24.6%，膜通量分别为17.1、17.3、16.9、17.2、16.0和16.6L·m~(-2)· h~(-1)。该纳滤膜对不同无机盐的截留性能不同，具有典型的荷负电膜截留特性，这主要决定于荷电膜与电解质离子之间的静电作用力。
通过对壳聚糖改性制备了水溶性的壳聚糖磷酸酯（PCS）。以PCS水溶液为铸膜液材料，PSF超滤膜为基膜，ECH为交联剂，用涂敷交联的方法制备了PCS/PSF复合纳滤膜，对其结构和形貌进行了表征。研究了活性层铸膜液的组成、交联剂浓度等因素对复合膜截留性能的影响。制备的PCS/PSF复合纳滤膜在操作压力为1MPa，料液流量为40L·h~(-1)时，对1000mg·L~(-1)Na_2SO_4和NaCl溶液的截留率分别为89.2、20.8%，通量分别为6.9、7.4L·m~(-2)· h~(-1)。复合膜对几种无机盐的截留顺序为：Na_2SO_4> MgSO_4> NaCl> MgCl_2。
以PCS为表面活性层材料，PSF超滤膜为基膜，GA为交联剂，制备了一种新型PCS/PSF复合纳滤膜。其最佳制备条件为：壳聚糖磷酸酯PCS溶液浓度为2%，GA浓度为0.5%，在50℃下交联1.5h。复合膜对1000mg·L~(-1)Na_2SO_4溶液的截留率和通量分别为87.6%和8.3L·m~(-2)· h~(-1)。对无机盐的截留顺序为：Na_2SO_4>MgSO_4> NaCl> MgCl_2。研究了操作条件和有机小分子添加剂对复合膜截留性能的影响。在室温下，复合膜接触角为56.20°，溶胀度为44.07%，截留分子量约为510Da。
以PCS为表面活性层材料，聚砜（PSF）为支撑层，CuSO4为螯合剂，成功制备了一种新型离子交联PCS/PSF复合纳滤膜。其最佳制备条件为：壳聚糖磷酸酯（PCS）水溶液浓度为1.5%，CuSO_4浓度为4%，在40℃下交联2h。复合膜对1000mg·L~(-1)Na_2SO_4溶液的截留率和通量分别为85.5%和7.4L·m~(-2)· h~(-1)。膜的截留分子量约为580Da，接触角为58.46°。
用戊二醛交联的壳聚糖磷酸酯（PCS）/聚砜（PSF）复合纳滤膜对某污水处理厂中水进行了深度处理应用研究，对影响纳滤过程的因素，如操作压力、工作流量和运行时间进行了考察。测定在这些条件下，其对膜通量的影响以及对CODCr等的去除率（R）。结果表明，在操作压力为1MPa，进料液流量为40L·h~(-1)时，复合膜对总磷的去除率（R）>85.0%，对CODCr、氨氮及电导率的去除率（R）分别为76.2、69.8和33.2%，对色度的去除率为100%。经过膜法深度处理之后，出水各项指标都可以达到GB18918~(-2)002一级A的排放标准。
Sodium carboxymethyl cellulose (CMC), sodium alginate (ALG) andphosphorylated chitosan (PCS) were explored as the active layer materials forcomposite nanofiltration (NF) membranes in this study. A series of negatively chargedcomposite NF membranes were prepared through coating the casting solution ontoPSF matrix, and then cross-linked with glutaraldehyde (GA), epichlorohydrin (ECH),or CuSO4, repectively. The membranes were characterized by scanning electronmicroscopy (SEM), attenuated total reflection infrared spectroscopy (ATR-IR) andatomic force microscopy (AFM). Effects of membrane making conditions,low-molecular-weight organic additives in the casting solution and operatingconditions on performance of the composite membranes were also investigated.
A negatively charged composite NF membrane was prepared using CMC assurface active layer, PSF matrix as support layer, cross-linked with GA. The resultsindicated that the composite membrane with excellent rejection performance shouldbe prepared while CMC concentration1%, GA concentration0.5%, cross-linking time2h at30℃. At room temperature, the contact angle is57.85°, degree of swelling44.26%, and its molecular weight cut-off is520Da. At1MPa and40L·h~(-1)feed flow,the rejections of the composite membrane to1000mg·L~(-1)K_2SO_4, Na_2SO_4, KCl, NaCl,MgSO4and MgCl_2were98.3,98.0,62.5,59.1,54.4and24.6%, with a flux of10.0,10.1,15.2,15.8,13.7and16.5L· m~(-2)· h~(-1), respectively. The rejection rate of themembrane to different electrolyte solutions decreased in the order of Na_2SO_4, NaCl,MgSO4and MgCl_2.
A blend composite NF membrane was prepared using CMC and ALG blend assurface active layer, PSF as support layer, cross-linked with ECH at pH=10. Thecomposite membrane with excellent rejection performance should be prepared whileALG/CMC proportion1:3, ECH concentration2%, cross-linking time18h at50℃. At1MPa and30L·h~(-1)feed flow, the rejections of the composite membrane to1000mg·L~(-1) K_2SO_4, Na_2SO_4, KCl, NaCl, MgSO4and MgCl_2were97.4,97.1,58.9,55.1,51.6and24.6%, with a flux of17.1,17.3,16.9,17.2,16.0and16.6L· m~(-2)· h~(-1), respectively. Theresults indicate that the composite NF membrane has different rejection ratio todifferent kinds of inorganic salts. Similar to other negative charged membranes, therejection performance of the composite membrane depends on the electrostatic forcebetween the charged membrane and ions of electrolyte.
The water soluble PCS with D.C. of0.78was prepared through a modified andhomogeneous method. A novel kind of composite NF membrane was prepared usingPCS as surface active layer, PSF as support layer, cross-linked with ECH. Themembrane preparation techniques on the performance of the composite membranewere investigated. The results suggest that the composite membrane with excellentrejection performance should be prepared while PCS concentration1.5%, ECHconcentration1%, cross-linking time22h at60℃. The structure and morphology ofthe resulting membrane were characterized by ATR-IR, SEM, and AFM. At1MPa and40L·h~(-1)feed flow, the rejections of the NF membrane to1000mg·L~(-1)Na_2SO_4andNaCl were89.2and20.8%, respectively. The flux were6.9and7.4L· m~(-2)· h~(-1). Therejections of the membrane to different electrolyte solutions decreased in the order ofNa_2SO_4, MgSO4, NaCl and MgCl_2.
The PCS/PSF composite NF membrane was prepared using PCS as surfaceactive layer, PSF as support layer, cross-linked with GA. The results suggest that thecomposite membrane with excellent rejection performance should be prepared whilePCS concentration2%, GA concentration0.5%, cross-linking time1.5h at50℃.At1MPa and40L·h~(-1)feed flow, the rejection and flux of the NF membrane to1000mg·L~(-1)Na_2SO_4was87.6%and8.3L· m~(-2)· h~(-1), respectively. The rejections of thiskind of membrane to the electrolyte solutions decreased in the order of Na_2SO_4,MgSO4, NaCl and MgCl_2. The preparation techniques on the performance of thecomposite membrane were investigated. At room temperature, the contact angle is56.20°, degree of swelling44.07%, and its molecular weight cut-off510Da.
A novel PCS/PSF composite membrane was prepared using PCS as surfaceactive layer, PSF as support layer, cross-linked with CuSO4. The composite membranewith excellent rejection performance should be prepared while PCS concentration1.5%, CuSO4concentration4%, cross-linking time2h at40℃. At1MPa and40L·h~(-1)feed flow, the rejection and flux of the NF membrane to1000mg·L~(-1)Na_2SO_4was85.5%and7.4L· m~(-2)· h~(-1), respectively. The contact angle is58.46°and molecular weight cut-off580Da.
The GA cross-linked PCS/PSF composite membrane was used in reclaimedwater treatment of a waste water plant. The permeate flux and the removalefficiencies in color, CODCr, TP, NH3and conductivity were investigated in relationto the driving pressure, the feed flow, and the operation time. At the pressure of1MPaand40L·h~(-1)feed flow, the removal efficiencies for color, CODCr, TP, NH3andconductivity were100,76.2,85.2,69.8and33.2%, respectively. After membraneprocess treatment, all the indexes of permeate reached A level standard ofGB18918~(-2)002.
引文
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