多功能介孔硅基吸附剂的制备及其对重金属废水的处理研究
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摘要
水体重金属污染所引起的环境问题已严重危及社会经济的可持续发展与民众身体健康，其处理技术研究受到了国内外学者的广泛关注。吸附法是一种常用的重金属离子污染物处理技术之一，因其吸附材料价廉易得、不需要复杂装置和添加额外化学物质等特点而被越来越多地应用。因此，寻求各种具有特殊或优异性能如具有特殊选择性、重复利用率高、成本低廉、制备简单和去除效率高的吸附剂，是该领域最引人注目的研究热之一。
本学位论文综述了水环境中重金属污染的危害与处理技术的国内外研究进展。同时，基于有序介孔硅基材料具有均一可调的中孔孔径、稳定的骨架结构、大比表面积及可修饰的内表面的优点，设计并合成了一系列去除效率高的新型介孔吸附材料，并借助红外光谱、扫描电镜等方法对所得各种吸附剂进行了表征研究；利用批实验方法进行了所得吸附剂对水体中金属离子吸附实验，考察了各种影响因素如温度、溶液pH值、金属离子初始浓度、接触时间、竞争离子和离子强度等对吸附剂性能的影响，并应用各种动力学、吸附等温线和热力学模型对实验数据进行了拟合和讨论；以新的视角开发吸附剂的循环利用的技术，实现材料的多功能化。本学位论文的主要结果如下：
1.采用后嫁接法和共缩聚法利制备了水杨醛Schiff base功能化介孔硅基吸附材料SA-SBA-15，前者合成的SA-SBA-15和后者合成的SA-SBA~(-1)5对Cu~(2+)的饱和吸附量分别为60.0mg g~(-1)和20.4mg g~(-1)，最佳溶液pH值为5。动力学研究表明，两种改性方法合成的SA-SBA-15对Cu~(2+)的吸附非常快，在40min均达到平衡。吸附动力学过程可以用拟二级动力学和粒子扩散方程解释。用等温线模型对平衡吸附数据进行拟合，发现平衡数据比较符合Langmuir等温线模型。SA-SBA-15具有良好的循环使用能力，EDTA解吸5次后吸附剂依然可以重复使用。SA-SBA-15吸附Cu~(2+)后形成的Cu-SA-SBA-15具有良好的杀菌性能，对大肠杆菌的最小抑菌浓度为160μg mL~(-1)，对金黄色葡萄球菌的最小抑菌浓度为120μg mL~(-1)。
2.采用后嫁接法得到8-羟基喹啉Schiff base功能化介孔硅基吸附剂S-SBA-15，结果发现S-SBA-15与很多其他廉价和商业化的吸附剂相比，可以更好地选择性去除废水中的Cu~(2+)。最大吸附容量为46.45mg g~(-1)，最佳溶液pH值为5.5。动力学研究表明S-SBA-15吸附反应较快，在30min吸附均达到平衡，平衡数据比较符合Langmuir等温模型。同时，吸附剂对Cu~(~(2+))的的吸附动力学符合拟二级反应模型和粒子扩散模型。虽然其它离子的存在，如Zn~(2+)，Co~(2+)，但是S-SBA-15表现出从多元金属离子溶液中对Cu~(~(2+))具有良好的选择性吸附性能。S-SBA-15吸附Cu~(2+)后形成的Cu-S-SBA-15最小抑菌浓度实验结果表明对大肠杆菌和金黄色葡萄球菌均有优秀的抗菌性能，其最小抑菌浓度小于40μg mL~(-1)，属于广谱抗菌剂。
3.通过后嫁接法，成功制备用于去除Pb~(2+)的有序介孔硅材料EDTA-SBA-15。EDTA有效接枝在SBA~(-1)5孔道表面，羧基含量为0.908m mol g~(-1)。对Pb (II)表现出优秀的吸附能力，EDTA-SBA-15对Pb (II)的吸附机理涉及了Na和Pb的离子交换以及表面络合作用。根据Langmuir模型计算，最大吸附容量为273.2mg g~(-1)，最佳溶液pH值为5。EDTA-SBA-15对Pb (II)的吸附在20min既能达到平衡，动力学数据能很好的用拟二级动力学模型进行描述，孔扩散过程在吸附过程中也扮演了重要角色，这主要归因于合成的吸附剂具有多孔结构。此外，吸附剂有非常好的重复使用性。对金属离子的多组分吸附结果表明，EDTA-SBA~(-1)5对Pb (II)有良好的吸附选择性，可从Pb~(2+)/Cd~(2+)，Pb~(2+)/Hg~(2+)或Pb~(2+)/Hg~(2+)/Cd~(2+)的金属离子混合液中选择性吸附Pb~(2+)。
4.通过后嫁接法成功制备一种多功能介孔吸附剂RBHS-SBA-15，材料结构是荧光介孔（罗丹明B感受器在孔道里），在环境保护领域的应用是检测，吸附，去除水溶液中的Hg~(2+)。制备的介孔材料表现出很好的荧光敏感性和在多种金属离子（Na+, Mg~(2+), Mn~(2+), Co~(2+), Ni~(2+), Zn~(2+), Cd~(2+), Ag+, Pb~(2+)和Cu~(~(2+))）对Hg~(2+)选择的选择性。在加入Hg~(2+)之后，观察到明显的发射改变，Hg~(2+)检测限是1ppb。微球对Hg~(2+)的吸附过程可以很好的用Langmuir描述，吸附容量为34.2mg g~(-1)。吸附能在30分钟之内达到平衡，动力学数据符合拟二级动力学模型和粒子扩散模型。
研制的功能化SBA-15吸附剂在重金属废水深度处理中具有极大的应用潜力。
Heavy metal as one of the important pollutants in water becomes a severepublic health concern because of its persistent nature and negative effect on theenvironment. They are difficultto remove from aqueous waste streams with tracequantities using conventional methods such aschemical precipitation. The process ofsorption/ion exchange appears to be one of the few alternatives available for suchsituations. To explore the availability of different kinds of adsorbents associated withconvenient procedures for obtaining high efficiency has been a hot topic recently.
This paper discussed the hazardous effect of heavy metal ions in aqueoussolution and the development of treatment technologies for heavy metal removal.Based on the viewpoints of speciation of heavy metals in waters, the distribution ofdifferent species of heavy metals and the binding mechanism with adsorbents wereinvestigated. To develop new efficient solid adsorbents by chemical modification,four different kinds of solid extractants were prepared including SA-SBA-15, S-SBA-15,EDTA-SBA-15and RBHS-SBA-15. Then these new adsorbents were characterized withFTIR, TEM and XRD. Furthermore, adsorption experiments in a batch method werecarried out to examine the adsorption performance for some heavy metal ions. Manymodels such as kinetic, thermodynamic, equilibrium models were used to fit theexperiment data to understand the adsorption mechanisms. This thesis contains thefollowing five sections:
1. Salicylidene Schiff base-functionalized SBA-15mesoporous silica is prepared,characterized and used as an adsorbent for heavy metal ion, Cu (II). By two modifiedmethods(post-grafting and co-condesnsation), the organic-inorganic hybridmesoporous materials have been synthesized by tetraethoxysilane (TEOS) with3-aminopropyltrimethoxy-silane (APTES) and salicylaldehyde in sequence. Thefunctionalized mesoporous materials are characterized by means of XRD, FT-IR, TEMand N2adsorption-desorption analysis. The result indicates that, after sequentchemical modifications of aminopropyl and schiff base, the primary hexagonallyordered mesoporous structure of SBA-15is not affected, exhibits the excellent adsorption capacity. The removal rate of Cu~(~(2+)) in aqueous media is high and theadsorbent can be regenerated by EDTA treatments without changing its properties.Meanwhile，Cu-SBA-15antibacterial agent was shown to be an effective bactericideagainst Bacillus coli and Staphylococcus aureus，indicating that it has goodantibacterial effect．
2.8-hydroxyquinoline Schiff base-functionalized SBA-15mesoporous silica wasprepared and S-SBA-15was found to be a better adsorbent for selective removal ofCu~(2+) from polluted water. The maximum adsorption capacity of Cu~(2+)(46.45mg g-1)onto S-SBA-15was obtained at pH5.5. From kinetic studies, it was found that theadsorption of Cu~(2+) was fast and it reached equilibrium around approximately30min.Langmuir models fitted the experimental data well. The kinetics of adsorption usingS-SBA-15was explained by the second-order kinetic model and theintraparticlediffusion model. Although the presence of other ions such as Zn~(2+), Co~(2+) werefound to have effect on Pb(II) adsorption, S-SBA-15show a good selective removal ofPb(II)from multi-metal ions solution. Meanwhile，Cu-S-SBA-15antibacterial agentwas shown to be an effective bactericide against Bacillus coli and Staphylococcusaureus even with the minimal inhibitory concentration (MIC) of40μg mL~(-1)，indicating that it has good antibacterial effect．
3. An organic-inorganic hybrid mesoporous silica material was synthesized bytwo-step post-grafting method of SBA-15with3-aminopropyltrimethoxy-silane(APTES) and thionyl dichloride (SOCl2) activated ethylenediaminetetraacetic acid(EDTA) in sequence and measured by means of Fourier transform infraredspectroscopy (FT-IR), X-ray diffraction (XRD), elemental analysis (EA), transmissionelectron microscopy (TEM), nitrogen (N2) adsorption-desorption analysis and backtitration. The material was found having the beneficial properties of mesoporoussilica SBA-15and EDTA. Adsorption potential of the material for Pb(II) removal fromaqueous solution was investigated by varying experimental conditions such as pH,contact time and initial metal concentration. The removal efficiency of Pb~(2+) was highunder the studied experimental conditions. The adsorption equilibrium could bereached within20minutes and the kinetic data were fitted well by pseudo-second-order and intraparticle diffusion model. The adsorbent exhibited afavorable performance and its maximum adsorption capacity calculated by Langmuirmodel was273.2mg g?1. Recycling experiments showed the adsorbent could beregenerated by acid treatment without altering its properties. The chemical states ofthe elements involved in the adsorption were analyzed by X-ray photoelectronspectroscopy (XPS). The results demonstrated that the adsorption mechanism of thematerial involved Na Pb ion-exchange and carboxyl group dominated surfacecomplexation.
4. A novel,‘‘all-in-one’’, multifunctional microsphere with a fluorescentmesoporous silica (Rhodamine B coordinate receptor inside) has been successfullyfabricated using a sol–gel method and small molecular (CTAB) surfactants asstructure-directing agents. At the same time, they were examined for environmentalprotection applications to detect, adsorb and remove Hg~(2+) in aqueous solution. Theprepared mesoporous materials were fluorescent and mesoporous. Thesemultifuctional microspheres showed excellent fluorescence sensitivity and selectivitytowards Hg~(2+) over other metal ions (Na+, Mg~(2+), Mn~(2+), Co~(2+),Ni~(2+), Zn~(2+), Cd~(2+), Ag+,Pb~(2+) and Cu~(2+)). Upon the addition of Hg~(2+), an overall emission change of16-foldwas observed, and the detection limit of Hg~(2+) was as low as1ppb. The adsorptionprocess of Hg~(2+) on the RBHS-SBA-15was well described by the Langmuir equation.The equilibrium can be established within30minutes and the adsorption capacitywas34.2mg g-1. These results suggest that these ‘‘all-in-one’’ multifunctionalmesoporous scilica are potentially useful materials for simultaneously rapidlydetecting and recovering dangerous pollutants in aqueous solution.
Chemical modified SBA-15developed in this paper have great potential for theadvanced treatment of wastewater containing heavy metals.
本学位论文综述了水环境中重金属污染的危害与处理技术的国内外研究进展。同时，基于有序介孔硅基材料具有均一可调的中孔孔径、稳定的骨架结构、大比表面积及可修饰的内表面的优点，设计并合成了一系列去除效率高的新型介孔吸附材料，并借助红外光谱、扫描电镜等方法对所得各种吸附剂进行了表征研究；利用批实验方法进行了所得吸附剂对水体中金属离子吸附实验，考察了各种影响因素如温度、溶液pH值、金属离子初始浓度、接触时间、竞争离子和离子强度等对吸附剂性能的影响，并应用各种动力学、吸附等温线和热力学模型对实验数据进行了拟合和讨论；以新的视角开发吸附剂的循环利用的技术，实现材料的多功能化。本学位论文的主要结果如下：
1.采用后嫁接法和共缩聚法利制备了水杨醛Schiff base功能化介孔硅基吸附材料SA-SBA-15，前者合成的SA-SBA-15和后者合成的SA-SBA~(-1)5对Cu~(2+)的饱和吸附量分别为60.0mg g~(-1)和20.4mg g~(-1)，最佳溶液pH值为5。动力学研究表明，两种改性方法合成的SA-SBA-15对Cu~(2+)的吸附非常快，在40min均达到平衡。吸附动力学过程可以用拟二级动力学和粒子扩散方程解释。用等温线模型对平衡吸附数据进行拟合，发现平衡数据比较符合Langmuir等温线模型。SA-SBA-15具有良好的循环使用能力，EDTA解吸5次后吸附剂依然可以重复使用。SA-SBA-15吸附Cu~(2+)后形成的Cu-SA-SBA-15具有良好的杀菌性能，对大肠杆菌的最小抑菌浓度为160μg mL~(-1)，对金黄色葡萄球菌的最小抑菌浓度为120μg mL~(-1)。
2.采用后嫁接法得到8-羟基喹啉Schiff base功能化介孔硅基吸附剂S-SBA-15，结果发现S-SBA-15与很多其他廉价和商业化的吸附剂相比，可以更好地选择性去除废水中的Cu~(2+)。最大吸附容量为46.45mg g~(-1)，最佳溶液pH值为5.5。动力学研究表明S-SBA-15吸附反应较快，在30min吸附均达到平衡，平衡数据比较符合Langmuir等温模型。同时，吸附剂对Cu~(~(2+))的的吸附动力学符合拟二级反应模型和粒子扩散模型。虽然其它离子的存在，如Zn~(2+)，Co~(2+)，但是S-SBA-15表现出从多元金属离子溶液中对Cu~(~(2+))具有良好的选择性吸附性能。S-SBA-15吸附Cu~(2+)后形成的Cu-S-SBA-15最小抑菌浓度实验结果表明对大肠杆菌和金黄色葡萄球菌均有优秀的抗菌性能，其最小抑菌浓度小于40μg mL~(-1)，属于广谱抗菌剂。
3.通过后嫁接法，成功制备用于去除Pb~(2+)的有序介孔硅材料EDTA-SBA-15。EDTA有效接枝在SBA~(-1)5孔道表面，羧基含量为0.908m mol g~(-1)。对Pb (II)表现出优秀的吸附能力，EDTA-SBA-15对Pb (II)的吸附机理涉及了Na和Pb的离子交换以及表面络合作用。根据Langmuir模型计算，最大吸附容量为273.2mg g~(-1)，最佳溶液pH值为5。EDTA-SBA-15对Pb (II)的吸附在20min既能达到平衡，动力学数据能很好的用拟二级动力学模型进行描述，孔扩散过程在吸附过程中也扮演了重要角色，这主要归因于合成的吸附剂具有多孔结构。此外，吸附剂有非常好的重复使用性。对金属离子的多组分吸附结果表明，EDTA-SBA~(-1)5对Pb (II)有良好的吸附选择性，可从Pb~(2+)/Cd~(2+)，Pb~(2+)/Hg~(2+)或Pb~(2+)/Hg~(2+)/Cd~(2+)的金属离子混合液中选择性吸附Pb~(2+)。
4.通过后嫁接法成功制备一种多功能介孔吸附剂RBHS-SBA-15，材料结构是荧光介孔（罗丹明B感受器在孔道里），在环境保护领域的应用是检测，吸附，去除水溶液中的Hg~(2+)。制备的介孔材料表现出很好的荧光敏感性和在多种金属离子（Na+, Mg~(2+), Mn~(2+), Co~(2+), Ni~(2+), Zn~(2+), Cd~(2+), Ag+, Pb~(2+)和Cu~(~(2+))）对Hg~(2+)选择的选择性。在加入Hg~(2+)之后，观察到明显的发射改变，Hg~(2+)检测限是1ppb。微球对Hg~(2+)的吸附过程可以很好的用Langmuir描述，吸附容量为34.2mg g~(-1)。吸附能在30分钟之内达到平衡，动力学数据符合拟二级动力学模型和粒子扩散模型。
研制的功能化SBA-15吸附剂在重金属废水深度处理中具有极大的应用潜力。
Heavy metal as one of the important pollutants in water becomes a severepublic health concern because of its persistent nature and negative effect on theenvironment. They are difficultto remove from aqueous waste streams with tracequantities using conventional methods such aschemical precipitation. The process ofsorption/ion exchange appears to be one of the few alternatives available for suchsituations. To explore the availability of different kinds of adsorbents associated withconvenient procedures for obtaining high efficiency has been a hot topic recently.
This paper discussed the hazardous effect of heavy metal ions in aqueoussolution and the development of treatment technologies for heavy metal removal.Based on the viewpoints of speciation of heavy metals in waters, the distribution ofdifferent species of heavy metals and the binding mechanism with adsorbents wereinvestigated. To develop new efficient solid adsorbents by chemical modification,four different kinds of solid extractants were prepared including SA-SBA-15, S-SBA-15,EDTA-SBA-15and RBHS-SBA-15. Then these new adsorbents were characterized withFTIR, TEM and XRD. Furthermore, adsorption experiments in a batch method werecarried out to examine the adsorption performance for some heavy metal ions. Manymodels such as kinetic, thermodynamic, equilibrium models were used to fit theexperiment data to understand the adsorption mechanisms. This thesis contains thefollowing five sections:
1. Salicylidene Schiff base-functionalized SBA-15mesoporous silica is prepared,characterized and used as an adsorbent for heavy metal ion, Cu (II). By two modifiedmethods(post-grafting and co-condesnsation), the organic-inorganic hybridmesoporous materials have been synthesized by tetraethoxysilane (TEOS) with3-aminopropyltrimethoxy-silane (APTES) and salicylaldehyde in sequence. Thefunctionalized mesoporous materials are characterized by means of XRD, FT-IR, TEMand N2adsorption-desorption analysis. The result indicates that, after sequentchemical modifications of aminopropyl and schiff base, the primary hexagonallyordered mesoporous structure of SBA-15is not affected, exhibits the excellent adsorption capacity. The removal rate of Cu~(~(2+)) in aqueous media is high and theadsorbent can be regenerated by EDTA treatments without changing its properties.Meanwhile，Cu-SBA-15antibacterial agent was shown to be an effective bactericideagainst Bacillus coli and Staphylococcus aureus，indicating that it has goodantibacterial effect．
2.8-hydroxyquinoline Schiff base-functionalized SBA-15mesoporous silica wasprepared and S-SBA-15was found to be a better adsorbent for selective removal ofCu~(2+) from polluted water. The maximum adsorption capacity of Cu~(2+)(46.45mg g-1)onto S-SBA-15was obtained at pH5.5. From kinetic studies, it was found that theadsorption of Cu~(2+) was fast and it reached equilibrium around approximately30min.Langmuir models fitted the experimental data well. The kinetics of adsorption usingS-SBA-15was explained by the second-order kinetic model and theintraparticlediffusion model. Although the presence of other ions such as Zn~(2+), Co~(2+) werefound to have effect on Pb(II) adsorption, S-SBA-15show a good selective removal ofPb(II)from multi-metal ions solution. Meanwhile，Cu-S-SBA-15antibacterial agentwas shown to be an effective bactericide against Bacillus coli and Staphylococcusaureus even with the minimal inhibitory concentration (MIC) of40μg mL~(-1)，indicating that it has good antibacterial effect．
3. An organic-inorganic hybrid mesoporous silica material was synthesized bytwo-step post-grafting method of SBA-15with3-aminopropyltrimethoxy-silane(APTES) and thionyl dichloride (SOCl2) activated ethylenediaminetetraacetic acid(EDTA) in sequence and measured by means of Fourier transform infraredspectroscopy (FT-IR), X-ray diffraction (XRD), elemental analysis (EA), transmissionelectron microscopy (TEM), nitrogen (N2) adsorption-desorption analysis and backtitration. The material was found having the beneficial properties of mesoporoussilica SBA-15and EDTA. Adsorption potential of the material for Pb(II) removal fromaqueous solution was investigated by varying experimental conditions such as pH,contact time and initial metal concentration. The removal efficiency of Pb~(2+) was highunder the studied experimental conditions. The adsorption equilibrium could bereached within20minutes and the kinetic data were fitted well by pseudo-second-order and intraparticle diffusion model. The adsorbent exhibited afavorable performance and its maximum adsorption capacity calculated by Langmuirmodel was273.2mg g?1. Recycling experiments showed the adsorbent could beregenerated by acid treatment without altering its properties. The chemical states ofthe elements involved in the adsorption were analyzed by X-ray photoelectronspectroscopy (XPS). The results demonstrated that the adsorption mechanism of thematerial involved Na Pb ion-exchange and carboxyl group dominated surfacecomplexation.
4. A novel,‘‘all-in-one’’, multifunctional microsphere with a fluorescentmesoporous silica (Rhodamine B coordinate receptor inside) has been successfullyfabricated using a sol–gel method and small molecular (CTAB) surfactants asstructure-directing agents. At the same time, they were examined for environmentalprotection applications to detect, adsorb and remove Hg~(2+) in aqueous solution. Theprepared mesoporous materials were fluorescent and mesoporous. Thesemultifuctional microspheres showed excellent fluorescence sensitivity and selectivitytowards Hg~(2+) over other metal ions (Na+, Mg~(2+), Mn~(2+), Co~(2+),Ni~(2+), Zn~(2+), Cd~(2+), Ag+,Pb~(2+) and Cu~(2+)). Upon the addition of Hg~(2+), an overall emission change of16-foldwas observed, and the detection limit of Hg~(2+) was as low as1ppb. The adsorptionprocess of Hg~(2+) on the RBHS-SBA-15was well described by the Langmuir equation.The equilibrium can be established within30minutes and the adsorption capacitywas34.2mg g-1. These results suggest that these ‘‘all-in-one’’ multifunctionalmesoporous scilica are potentially useful materials for simultaneously rapidlydetecting and recovering dangerous pollutants in aqueous solution.
Chemical modified SBA-15developed in this paper have great potential for theadvanced treatment of wastewater containing heavy metals.
引文
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