磁性纳米复合材料的制备及其去除水体污染物的研究
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摘要
本文围绕纳米材料治理水体重金属污染物而展开。基于吸附法和纳米材料的优点，制备了一系列磁性纳米复合吸附剂，同时将纳米材料的独特性能运用到微生物固定化技术中，用于高效治理水体重金属污染物。论文以磁性纳米复合材料去除水体中的铜、锌、镉重金属离子、磁性纳米颗粒选择性的去除Cr(VI)、磁性纳米粒子从铅锌二元金属溶液中选择性去除他们以及碳纳米管作为固定化材料来固定铜绿假单胞菌还原Cr(VI)为主要研究内容而进行，具体如下。
（1）首先通过分散聚合法合成了磁性多孔纳米复合物，然后借助化学法将聚乙烯亚胺共价修饰到粒子表面，制备了磁性纳米复合吸附剂，用于水体中铜、锌和镉的去除。用SEM和FTIR表征了它的外部形貌和内部结构。该吸附剂对铜、锌和镉的吸附随着pH的升高而升高，且吸附速度快，几乎在10min内达到吸附平衡。动力学拟合表明：该吸附过程符合准二级动力学方程；基于Langmuir吸附等温式的最大吸附容量分别是Cu~(2+)157.81mg/g，Zn~(2+)138.84mg/g，Cd~(2+)105.26mg/g。该磁性纳米复合物吸附剂对重金属的吸附表现出不同的亲和性，同样条件下，对铜的吸附优先于锌和镉。该吸附剂稳定性好，分离简单，且可以反复利用，为水体重金属污染治理提供了一个技术选择，通过修饰不同的功能性物质，可以制备其他高效的纳米吸附剂用于水体污染物的去除（第二章）。
（2）以水体中高毒性的Cr(Ⅵ)为治理对象，制备稳定性提高的磁性纳米吸附剂来选择性的去除它。首先通过煅烧Fe_3O_4形成具有核壳结构的Fe_3O_4@γ-Fe_2O_3磁性纳米粒子，然后将含有大量亚胺基团的聚合物修饰到颗粒表面，制备了磁性纳米吸附剂。该吸附剂为直径100nm的球体，等电点为pH=11.4，水分散性好，对盐酸或者氢氧化钠的耐受浓度可达1mol/L。在pH=2-3的范围，由于修饰的亚胺基团导致吸附剂表面的质子化，对Cr(Ⅵ)的去除效果非常的好。当用于吸附Cr(Ⅵ)的时候，能在15min内达到吸附饱和，数据拟合表明：吸附符合准二级动力学过程。对热力学参数(ΔG，ΔH和ΔS)的分析表明：该吸附剂对Cr(Ⅵ)的吸附为自发的放热过程，吸附容量随着温度的升高而有所降低，在35-15℃范围内的最大吸附量为74.07-83.33mg/g。溶液中共存的离子K~+、Na~+、Ca~(2+)和Cu~(2+)以及Cl~-和NO_3~-不会对Cr(Ⅵ)吸附造成影响。负载有Cr(Ⅵ)的吸附剂可以用0.02mol/L的氢氧化钠进行有效的再生。连续使用5次后对Cr(Ⅵ)的去除效率比最初只下降了9%。该研究的结果表明，基于磁性纳米颗粒的吸附剂可以选择性的去除废水中的Cr(Ⅵ)，且具有实际的应用前景（第三章）。
（3）制备了一种磁性纳米吸附剂来选择性的去除二元金属废水中的铅和锌。该吸附剂是通过嫁接亚胺基团到磁性纳米颗粒上而制备。可调节的选择性吸附是通过改变溶液的pH值和加入EDTA试剂来实现的。调查发现：当二元金属溶液条件为：pH=6，[EDTA]/[M~(2+)]=0.7时候，锌主要以二价锌离子的形式存在，而铅是以PbEDTA~(2-)的阴离子复合物存在，在该条件下通过鳌合作用选择性的去除锌，而对铅不产生吸附作用；当溶液条件为pH=2，[EDTA]/[M~(2+)]=0.7的时候，金属铅主要以PbEDTA~(2-)和PbHEDTA~-阴离子金属复合物的形式存在，而锌则主要以二价锌离子的形式稳定于溶液中，在强酸性条件下，该吸附剂借助静电作用选择性的去除二元金属溶液中铅。被吸附铅和锌分别经过碱（0.04mol/L的氢氧化钠）和酸（0.05mol/L的盐酸）洗脱后，而浓缩富集。此外，经过再生的吸附剂仍然保持了较高的吸附容量（第四章）。
（4）将多壁碳纳米管聚乙烯醇和海藻酸钠同时用于固定铜绿假单胞菌来还原Cr(Ⅵ)为Cr(Ⅲ)。使用4%的海藻酸钠、6%的聚乙烯醇、以及0.2-0.5%的MCNTs作为基质的时候，可以在交联剂4%的硝酸钙溶液中形成直径为3mm的小球体。经过冷冻解冻处理后的微生物小球的机械强度显著提高。多壁碳纳米管在基质中对Cr(Ⅵ)还原酶的固定起到了积极作用。和游离的菌相比，固定的菌体对Cr(Ⅵ)的耐受浓度提高到了80mg/L。可以反复利用且从液相中分离简单。该技术方法为处理Cr(Ⅵ)废水提供了新的方法选择，且可以用于固定其他微生物来治理环境污染物（第五章）。
（5）磁性纳米催化剂在环境污染物治理中的前景巨大。合成了磁性介孔硅，其孔径范围在5-7nm左右，且分布比较均匀，BET比表面积为536.5m~2/g，BJH吸附脱附孔容为1.08cm~3/g。欲将其用于固定金属钴，催化过硫酸盐产生高氧化性能的过硫酸根来降解水体中的偶氮化合物（第六章）。
Environmental pollution has become a serious global problem. Based on the advantages of adsorption method and nanaomaterials, a serial of nanocompounds are prepared to remedy the heavy metals contaminated water. The key contents include:preparation of magnetic nanocompound for the effective adsorption of Cu Zn and Cd in effluent; selective removal of Cr(VI) by stability-enhanced magnetic nanoparticles; selective adsorption of Pb and Zn from binary-metal solution; using of carbon nanotubes as immobilization materials to immobilize Pseudomonas aeruginosa for the reduction of Cr(VI). They are briefly as follows:
(1) Magnetic porous compound was synthesized by dispersion polymerization method, and then polyethylenimine was modified onto its surface to obtain the adsorbent. The adsorbent was used to remove Cu, Zn and Cd in effluent. SEM and FTIR were applied to characterize its morphology and structure. Adsorption of heavy metal increased with the increasing of solution pH, and achieved adsorption equilibrium within10min. Kinetics study showed that the adsorption process was well fitted with pseudo-second-order model. The maximum adsorption capacity was Cu2+157.81mg/g, Zn2+138.84mg/g, Cd2+105.26mg/g based on Langmuir adsorption isotherms. The magnetic adsorbent showed different adsorption affinity towards heavy metal, which was Cu2+> Zn2+> Cd2+. Besides, the adsorbent had good stability, easy separation and could be used repeatedly, which provided an alternative for heavy metal wastewater remediation. What is more, other effective nanoadsorbent could be developed by modification of different functional composite onto magnetic porous powder (in chapter2).
(2) The stability enhanced magnetic nanoparticle was prepared to selectively remove toxical Cr(VI). The Fe3O4was calcined to form magnetic nanoparticle with core-shell structure of Fe3O4@γ-Fe2O3, and then imine groups was grafted onto its surface to develop magnetic adsorbent. The adsorbent had a spheric shape with average diameter of100nm, its zero point of zeta potential was pH=11.4, dispersed in water evenly and could resist HCl and NaOH solution as high as1mol/L. The adsorbent was able to effectively remove anionic Cr(Ⅵ) in the pH range of2to3due to the large amount of protonated imine groups on its surface, and could be magnetically separated from liquid quickly. Adsorption equilibrium was reached within15min and independent of initial Cr(Ⅵ) concentration. The Cr(Ⅵ) maximum sorption capacity at a temperature range of35to15℃was74.07to83.33mg/g, which was obtained using the Langmuir adsorption isotherm. The calculated thermodynamic parameters (ΔG, ΔH, and ΔS) indicated that adsorption of Cr(Ⅵ) was spontaneous and exothermic in nature. Competition from coexisting ions (K+, Na+, Ca2+, Cu2+, Cl-, and NO3-) was found insignificant. The adsorbent had satisfying acid-alkali stability and could be regenerated by0.02mol/L NaOH solution. The results suggested the potential application of the PEI-modified magnetic nanoparticles in selective removal of Cr(Ⅵ) from wastewater (in chapter3).
(3) A magnetic nanoadsorbent was prepared to selectively remove Pb and Zn from binary-metal ions. The nanoadsorbent was prepared by introducing imine groups onto the surface of stability enhanced magnetic nanoparticles and then characterized by TEM and FTIR. The tunable selectivity was achieved by adjusting the solution pH and adding EDTA chelator. It was found that when the solution condition was [EDTA]/[M2+]=0.7with pH of6, zinc was existed with the form Zn2+and lead was PbEDTA2-compound, the zinc was selectively removed by chelate interaction. When the solution condition was [EDTA]/[M2+]=0.7and pH of2, PbEDTA2-and PbHEDTA-was existed in binary metal solution, zinc existed stablely with the form of Zn2+, under this solution condition, the adsorbent selectively removed lead by electrostatic interaction. The lead and zinc loaded adsorbent could be regenerated by0.04mol/L NaOH and0.05mol/L HCl, respectively, and still possessed high adsorption capacity. The recovered metal ions could be concentrated and reused (in chapter4).
(4) An immobilization technology based on polyvinyl alcohol (PVA), sodium alginate and multiwalled carbon nanotubes (MCNTs) was developed to immobilize Pseudomonas aeruginosa (Pa) for reduction of Cr(Ⅵ) to soluble Cr(Ⅲ). It was found that6%PVA,4%sodium alginate and0.4%MCNTs with4%Ca(NO3)2cross-linking agent (w/w) was the best option for forming beads with the average diameter of3mm. The immobilized Pa was subjected to freezing-thawing treatment to enhance its mechanical strength. MCNTs played a positive role in immobilization of chromium reductase. Compared with free cells, the immobilized Pa bead was able to resist higher toxicity of80mg/L Cr(VI), was convenient to operate for consecutive reduction of Cr(VI). The microbe immobilization technology provided an alternative for Cr(VI) wastewater treatment, and could be extended for other microorganism immobilization (in chapter5).
(5) Magnetic nanocatalyst has immense potential in remediation contaminated environment. Therefore, magnetic mesoporous silica was developed. Its pore size was in the range of5-7nm with a narrow particle size distribution. The BET surface area was536.2m2/g and BJH pore volume was1.08cm3/g. The magnetic mesoporous silica was planned to immobilize Co to activate PMS to generate sulfate radical to remove dyes in water (in chapter6).
（1）首先通过分散聚合法合成了磁性多孔纳米复合物，然后借助化学法将聚乙烯亚胺共价修饰到粒子表面，制备了磁性纳米复合吸附剂，用于水体中铜、锌和镉的去除。用SEM和FTIR表征了它的外部形貌和内部结构。该吸附剂对铜、锌和镉的吸附随着pH的升高而升高，且吸附速度快，几乎在10min内达到吸附平衡。动力学拟合表明：该吸附过程符合准二级动力学方程；基于Langmuir吸附等温式的最大吸附容量分别是Cu~(2+)157.81mg/g，Zn~(2+)138.84mg/g，Cd~(2+)105.26mg/g。该磁性纳米复合物吸附剂对重金属的吸附表现出不同的亲和性，同样条件下，对铜的吸附优先于锌和镉。该吸附剂稳定性好，分离简单，且可以反复利用，为水体重金属污染治理提供了一个技术选择，通过修饰不同的功能性物质，可以制备其他高效的纳米吸附剂用于水体污染物的去除（第二章）。
（2）以水体中高毒性的Cr(Ⅵ)为治理对象，制备稳定性提高的磁性纳米吸附剂来选择性的去除它。首先通过煅烧Fe_3O_4形成具有核壳结构的Fe_3O_4@γ-Fe_2O_3磁性纳米粒子，然后将含有大量亚胺基团的聚合物修饰到颗粒表面，制备了磁性纳米吸附剂。该吸附剂为直径100nm的球体，等电点为pH=11.4，水分散性好，对盐酸或者氢氧化钠的耐受浓度可达1mol/L。在pH=2-3的范围，由于修饰的亚胺基团导致吸附剂表面的质子化，对Cr(Ⅵ)的去除效果非常的好。当用于吸附Cr(Ⅵ)的时候，能在15min内达到吸附饱和，数据拟合表明：吸附符合准二级动力学过程。对热力学参数(ΔG，ΔH和ΔS)的分析表明：该吸附剂对Cr(Ⅵ)的吸附为自发的放热过程，吸附容量随着温度的升高而有所降低，在35-15℃范围内的最大吸附量为74.07-83.33mg/g。溶液中共存的离子K~+、Na~+、Ca~(2+)和Cu~(2+)以及Cl~-和NO_3~-不会对Cr(Ⅵ)吸附造成影响。负载有Cr(Ⅵ)的吸附剂可以用0.02mol/L的氢氧化钠进行有效的再生。连续使用5次后对Cr(Ⅵ)的去除效率比最初只下降了9%。该研究的结果表明，基于磁性纳米颗粒的吸附剂可以选择性的去除废水中的Cr(Ⅵ)，且具有实际的应用前景（第三章）。
（3）制备了一种磁性纳米吸附剂来选择性的去除二元金属废水中的铅和锌。该吸附剂是通过嫁接亚胺基团到磁性纳米颗粒上而制备。可调节的选择性吸附是通过改变溶液的pH值和加入EDTA试剂来实现的。调查发现：当二元金属溶液条件为：pH=6，[EDTA]/[M~(2+)]=0.7时候，锌主要以二价锌离子的形式存在，而铅是以PbEDTA~(2-)的阴离子复合物存在，在该条件下通过鳌合作用选择性的去除锌，而对铅不产生吸附作用；当溶液条件为pH=2，[EDTA]/[M~(2+)]=0.7的时候，金属铅主要以PbEDTA~(2-)和PbHEDTA~-阴离子金属复合物的形式存在，而锌则主要以二价锌离子的形式稳定于溶液中，在强酸性条件下，该吸附剂借助静电作用选择性的去除二元金属溶液中铅。被吸附铅和锌分别经过碱（0.04mol/L的氢氧化钠）和酸（0.05mol/L的盐酸）洗脱后，而浓缩富集。此外，经过再生的吸附剂仍然保持了较高的吸附容量（第四章）。
（4）将多壁碳纳米管聚乙烯醇和海藻酸钠同时用于固定铜绿假单胞菌来还原Cr(Ⅵ)为Cr(Ⅲ)。使用4%的海藻酸钠、6%的聚乙烯醇、以及0.2-0.5%的MCNTs作为基质的时候，可以在交联剂4%的硝酸钙溶液中形成直径为3mm的小球体。经过冷冻解冻处理后的微生物小球的机械强度显著提高。多壁碳纳米管在基质中对Cr(Ⅵ)还原酶的固定起到了积极作用。和游离的菌相比，固定的菌体对Cr(Ⅵ)的耐受浓度提高到了80mg/L。可以反复利用且从液相中分离简单。该技术方法为处理Cr(Ⅵ)废水提供了新的方法选择，且可以用于固定其他微生物来治理环境污染物（第五章）。
（5）磁性纳米催化剂在环境污染物治理中的前景巨大。合成了磁性介孔硅，其孔径范围在5-7nm左右，且分布比较均匀，BET比表面积为536.5m~2/g，BJH吸附脱附孔容为1.08cm~3/g。欲将其用于固定金属钴，催化过硫酸盐产生高氧化性能的过硫酸根来降解水体中的偶氮化合物（第六章）。
Environmental pollution has become a serious global problem. Based on the advantages of adsorption method and nanaomaterials, a serial of nanocompounds are prepared to remedy the heavy metals contaminated water. The key contents include:preparation of magnetic nanocompound for the effective adsorption of Cu Zn and Cd in effluent; selective removal of Cr(VI) by stability-enhanced magnetic nanoparticles; selective adsorption of Pb and Zn from binary-metal solution; using of carbon nanotubes as immobilization materials to immobilize Pseudomonas aeruginosa for the reduction of Cr(VI). They are briefly as follows:
(1) Magnetic porous compound was synthesized by dispersion polymerization method, and then polyethylenimine was modified onto its surface to obtain the adsorbent. The adsorbent was used to remove Cu, Zn and Cd in effluent. SEM and FTIR were applied to characterize its morphology and structure. Adsorption of heavy metal increased with the increasing of solution pH, and achieved adsorption equilibrium within10min. Kinetics study showed that the adsorption process was well fitted with pseudo-second-order model. The maximum adsorption capacity was Cu2+157.81mg/g, Zn2+138.84mg/g, Cd2+105.26mg/g based on Langmuir adsorption isotherms. The magnetic adsorbent showed different adsorption affinity towards heavy metal, which was Cu2+> Zn2+> Cd2+. Besides, the adsorbent had good stability, easy separation and could be used repeatedly, which provided an alternative for heavy metal wastewater remediation. What is more, other effective nanoadsorbent could be developed by modification of different functional composite onto magnetic porous powder (in chapter2).
(2) The stability enhanced magnetic nanoparticle was prepared to selectively remove toxical Cr(VI). The Fe3O4was calcined to form magnetic nanoparticle with core-shell structure of Fe3O4@γ-Fe2O3, and then imine groups was grafted onto its surface to develop magnetic adsorbent. The adsorbent had a spheric shape with average diameter of100nm, its zero point of zeta potential was pH=11.4, dispersed in water evenly and could resist HCl and NaOH solution as high as1mol/L. The adsorbent was able to effectively remove anionic Cr(Ⅵ) in the pH range of2to3due to the large amount of protonated imine groups on its surface, and could be magnetically separated from liquid quickly. Adsorption equilibrium was reached within15min and independent of initial Cr(Ⅵ) concentration. The Cr(Ⅵ) maximum sorption capacity at a temperature range of35to15℃was74.07to83.33mg/g, which was obtained using the Langmuir adsorption isotherm. The calculated thermodynamic parameters (ΔG, ΔH, and ΔS) indicated that adsorption of Cr(Ⅵ) was spontaneous and exothermic in nature. Competition from coexisting ions (K+, Na+, Ca2+, Cu2+, Cl-, and NO3-) was found insignificant. The adsorbent had satisfying acid-alkali stability and could be regenerated by0.02mol/L NaOH solution. The results suggested the potential application of the PEI-modified magnetic nanoparticles in selective removal of Cr(Ⅵ) from wastewater (in chapter3).
(3) A magnetic nanoadsorbent was prepared to selectively remove Pb and Zn from binary-metal ions. The nanoadsorbent was prepared by introducing imine groups onto the surface of stability enhanced magnetic nanoparticles and then characterized by TEM and FTIR. The tunable selectivity was achieved by adjusting the solution pH and adding EDTA chelator. It was found that when the solution condition was [EDTA]/[M2+]=0.7with pH of6, zinc was existed with the form Zn2+and lead was PbEDTA2-compound, the zinc was selectively removed by chelate interaction. When the solution condition was [EDTA]/[M2+]=0.7and pH of2, PbEDTA2-and PbHEDTA-was existed in binary metal solution, zinc existed stablely with the form of Zn2+, under this solution condition, the adsorbent selectively removed lead by electrostatic interaction. The lead and zinc loaded adsorbent could be regenerated by0.04mol/L NaOH and0.05mol/L HCl, respectively, and still possessed high adsorption capacity. The recovered metal ions could be concentrated and reused (in chapter4).
(4) An immobilization technology based on polyvinyl alcohol (PVA), sodium alginate and multiwalled carbon nanotubes (MCNTs) was developed to immobilize Pseudomonas aeruginosa (Pa) for reduction of Cr(Ⅵ) to soluble Cr(Ⅲ). It was found that6%PVA,4%sodium alginate and0.4%MCNTs with4%Ca(NO3)2cross-linking agent (w/w) was the best option for forming beads with the average diameter of3mm. The immobilized Pa was subjected to freezing-thawing treatment to enhance its mechanical strength. MCNTs played a positive role in immobilization of chromium reductase. Compared with free cells, the immobilized Pa bead was able to resist higher toxicity of80mg/L Cr(VI), was convenient to operate for consecutive reduction of Cr(VI). The microbe immobilization technology provided an alternative for Cr(VI) wastewater treatment, and could be extended for other microorganism immobilization (in chapter5).
(5) Magnetic nanocatalyst has immense potential in remediation contaminated environment. Therefore, magnetic mesoporous silica was developed. Its pore size was in the range of5-7nm with a narrow particle size distribution. The BET surface area was536.2m2/g and BJH pore volume was1.08cm3/g. The magnetic mesoporous silica was planned to immobilize Co to activate PMS to generate sulfate radical to remove dyes in water (in chapter6).
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