蒙脱土、高岭土和层状双金属氢氧化物对Pb~（2+）和对硝基苯酚的吸附研究
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摘要
随着工农业生产的发展,污染物的排放量日趋增多,对生态安全和人类健康造成严重威胁,其中重金属污染就是亟需解决的环境问题之一。目前,重金属污染土壤的修复及废水的处理已成为环境科学与工程领域的研究热点。重金属在固-液界面的吸附-脱附行为是决定重金属的地球化学过程和环境生态效应的根本问题,对这一基本现象的科学认识,是了解重金属污染物形态分布、迁移转化和归宿、开发污染土壤修复及废水处理技术的基础。前期虽然已对重金属在固-液界面上的吸附现象进行了大量研究,且对其吸附规律有了较全面的认识,但对吸附机理的了解并不十分清楚,这主要是由吸附体系的复杂性所致。另外,所研究的吸附剂多是带负电荷的,带正电荷的吸附剂涉及很少。
本文选择带结构负电荷的蒙脱土、基本不带结构电荷(或带微量结构负电荷)的高岭土和带结构正电荷的层状双金属氢氧化物(Layered double hydroxides,简称LDHs)为模型吸附剂,研究了对重金属铅的吸附行为,考察了多种因素的影响,以期探讨结构电荷(或由此引起的界面相微环境酸碱性)对重金属吸附的影响规律,加深对吸附机理的认识。同时,考察了煅烧层状双金属氢氧化物(CLDHs)、LDHs-EDTA纳米杂化物等对铅和对硝基苯酚的吸附,以期为高效吸附剂的开发提供信息。
主要研究内容和结论归纳如下。
一、蒙脱土和高岭土对Pb~(2+)的吸附作用及机理研究
主要研究了Pb~(2+)在蒙脱土和高岭土上的吸附性能,考察了温度、pH值、离子强度和吸附剂含量等因素对吸附的影响,并结合X射线光电子能谱(XPS)、XRD和比表面积等实验结果探讨了吸附机理。研究表明,蒙脱土和高岭土吸附Pb~(2+)的动力学曲线符合准二级动力学方程和Elovich方程,等温线符合Langmuir方程。以mg/g为单位时,蒙脱土的饱和吸附量明显高于高岭土,而以mg/m~2为单位时,二者相近。吸附量主要由黏土的比表面积决定,而吸附力由黏土的结构电荷密度决定。Pb~(2+)在蒙脱土和高岭土上的吸附机理可分为化学键合吸附(或内络合层吸附)和静电键合吸附(或外络合层吸附),其中静电键合吸附主要为结构负电荷位吸附。化学键合吸附具有强的选择性和不可逆性,不受离子强度的影响;静电键合吸附没有选择性,具有较强的可逆性,受离子强度的影响较大。化学键合吸附和静电键合吸附的相对量与pH有关;在pH小于4和大于8的范围内,化学键合吸附为主,而在pH4～8范围内静电键合吸附比例增大。pH增高,吸附量增高;温度、离子强度和吸附剂含量增大,吸附量下降。Pb~(2+)能进入蒙脱土的层间,而不能进入高岭土的层间;部分Pb~(2+)可进入黏土颗粒的微孔中被固定。EDTA可明显降低Pb~(2+)在蒙脱土上的吸附,而基本不影响在高岭土上的吸附。
二、层状双金属氢氧化物及其煅烧产物对Pb~(2+)的吸附作用
合成了Mg/Al摩尔比分别为1:1和2:1的Mg-Al-LDHs样品(MgAl-LDH和Mg_2Al-LDH)及其煅烧产物(MgAl-CLDH和Mg_2Al-CLDH),同时还合成了乙二胺四乙酸(EDTA)-LDH纳米杂化物,考察了它们对Pb~(2+)的吸附作用。结果表明,Mg-Al-LDHs和Mg-Al-CLDHs对Pb~(2+)均有很强的吸附能力,有望成为一类新型高效吸附剂;吸附动力学符合准二级动力学过程,吸附等温线符合Freundlich方程。吸附量在pH=3～10的范围内变化不大。电解质可抑制Pb~(2+)在Mg-Al-LDHs上的吸附,但基本不影响在Mg-Al-CLDHs上的吸附。吸附机理为表面络合吸附,在Mg-Al-LDHs上的吸附同时存在化学键合(内层络合)吸附和静电键合(外层络合)吸附,而在Mg-Al-CLDHs的吸附主要为化学键合吸附。
Mg-Al-CLDHs对Pb~(2+)的吸附能力明显高于相应的Mg-Al-LDHs;EDTA-LDH纳米杂化物也明显高于相应的Mg-Al-LDHs,表明EDTA的插入具有协同增效作用。
三、对硝基苯酚在Mg_2Al-LDH及其煅烧产物上的吸附
研究了对硝基苯酚在Mg_2Al-LDH和Mg_2Al-CLDH上的吸附,考察了pH、温度等因素的影响。结果表明,对硝基苯酚在Mg_2Al-LDH和Mg_2Al-CLDH上均有明显吸附,其吸附等温线均符合Freundlich等温式;在Mg_2Al-LDH上的吸附动力学符合双常数方程,而在Mg_2Al-CLDH上符合准一级动力学速率方程和Elovich方程;在Mg_2Al-CLDH上的吸附速率和吸附量明显高于Mg_2Al-LDH。初始pH在3～10范围内变化对吸附量的影响不大。温度升高,吸附量增大。CLDHs有望成为一种新型的高效酚类有机污染物处理剂。
With the development of industry and agriculture,the emission of pollutants is increasing which causes serious harm to ecological safety and human health.Heavy metal pollution is one of the environmental problems to be urgently resolved.The remediation of heavy metal contaminated soil and the treatment of waste water have become hot topics of environmental science and engineering.The adsorption/desorption behavior of heavy metal at the solid liquid interface is the fundamental problem which determines the geochemistry process of heavy metal and environmental ecological effect.The scientific knowing of the basic phenomena is the basis of understanding the speciation distribution,transport and fate of heavy metal pollutants and techonolgy on remediation of contaminated soil and waste water treatment.A great deal of studies have been done on the adsorption of heavy metal at the solid liquid interface and an overall understanding to adsorption law has been reached, however,the adsorption mechanism is not very clear due to the complexity of adsorption systems.Moreover,the adsorbents studied are usually negative charged.Rare studies have been done about positive charged heavy metal adsorbents.
We choose structurally negative charged montmorillonite,structurally no charged kaolinite(or small quantity of negative structural charge)and structurally positive charged layered double hydroxides as model adsorbents and study the adsorption behavior of Pb~(2+) on them.The influence of various factors were investigated to obtain the influence law of structural charge(or interface phase microenvironmental acidity induced by it)on heavy metal adsorption and deepen the cognition to the adsorption mechanism.Adsorption of p-nitrophenol and Pb~(2+)on MgAl-CLDHs,adsorption of Pb~(2+)on LDHs- EDTA were also discussed to supply information to the development of the high- efficiency sorbent.
The contents include the followings:
Section1.Study on adsorption behavior and adsorption mechanism of Pb~(2+)on montmorillonite and kaolinite
Sorption properties of Pb~(2+)on montmorillonite and kaolinite were studied,the influence of temperature,solution pH,ion strength and sorbent content on the sorption of Pb~(2+)were investigated,and the sorption mechanism was discussed in combination with the results of XPS,XRD and specific surface area(SSA)experiments.The sorption kinetics can be well described by the pseudo-second-order kinetics and the Elovich kinetic equation and the sorption isotherms can be described by Langmuir isotherm.The sorption amount in mg/g of Pb~(2+)on montmorillonite is obviously higher than that on kaolinite,however that in mg/m~2 on montmorillonite is very close with that on kaolinite.Adsorption amount is mainly determined by the SSA while the adsorption ability is determined by structural negative charge density of clays.The sorption mechanism of Pb~(2+)on the montmorillonite and kaolinite may be distinguished to the chemi-bonded adsorption(or inner-sphere surface complexation adsorption)and electrostatic-bond adsorption(or outer-sphere surface complexation adsorption).The electrostatic-bond adsorption is mainly negative structural charge sites adsorption.The chemi-bonded adsorption is irreversible,strong selective and the ionic strength has no effect on it.The electrostatic-bond adsorption is reversible,no selective and the ionic strength has a significant effect on it.The relative content of chemi-bonded adsorption and the electrostatic-bond adsorption is dependent of pH,and the relative content of the electrostatic-bond adsorption in the pH range of 4～8 is higher than in the pH ranges of lower than 4 and higher than 8.The increases of temperature,ion strength and sorbent content would induce the decrease of the adsorption amounts of Pb~(2+)on montmorillonite and kaolinite while the sorption amount increases with increasing pH.Pb~(2+)can be intercalated between the layers of the montmorillonite while it can not be intercalated between the layers of kaolinite.Portion of Pb~(2+)can be fixed by enterring in the micropore of clay particles.EDTA can significantly decrease the adsorption of Pb~(2+)on montmorillonite,hardly affects the adsorption of Pb~(2+)on kaolinite.
Section2.Adsorption of Pb~(2+)on MgAl Layered double hydroxides and their calcined products
Layered double hydroxides with an Mg/Al molar ratio of 1:1(MgAl-LDH),2:1 (Mg_2Al-LDH)and EDTA-LDH nanohybrids were synthesized by using a co-precipitation method and calcined LDHs(CLDHs)were obtained by calcination LDHs at 500℃.The sorption removal of Pb~(2+)by them was investigated.It was found that both Mg-Al-LDHs and Mg-Al-CLDHs show good sorption ability and they could be a new type of environmental sorbent for the removal of Pb~(2+).The sorption kinetics and the sorption isotherms of Pb~(2+)on both the Mg-Al-LDHs and the Mg-Al-CLDHs can be described by the pseudo-second order kinetics and Freundlich isotherm,respectively.The sorption amounts of Pb~(2+)are independent of the pH in the range of about 3～10.The presence of electrolyte inhibited the sorption of Pb~(2+)on the Mg-Al-LDHs while not on the Mg-Al-CLDHs.The sorption mechanism of Pb~(2+)may be contributed to the surface complexation.The adsorption of Pb~(2+)on the Mg-Al-LDHs may be contributed to both the chemi-bonded adsorption(or inner-sphere surface complexation adsorption)and the electrostatic-bond adsorption(or outer-sphere surface complexation adsorption),while that on the Mg-Al-CLDHs mainly to the chemi-bonded adsorption.
The adsorption ability of Pb~(2+)on the Mg-Al-CLDHs is higher than that on the Mg-Al-LDHs.The adsorption ability of Pb~(2+)on the EDTA-LDH nanohybrids is also higher than that on the Mg-Al-LDHs which indicates the intercalation of EDTA had synergy.
Section3.Adsorption of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH
The sorption removal of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH were investigated.The influence of pH,temperature on the adsorption was investigated.The results showed that p-nitrophenol could be adsorbed on both Mg_2Al-LDH and Mg_2Al-CLDH.Adsorption isotherms could be fitted with the Freundlich equation,the sorption kinetics of p-nitrophenol on Mg_2Al-LDH could be well described by the two-constant equation while the sorption kinetics of p-nitrophenol on Mg_2Al-CLDH could be well described by pseudo-first-order kinetics and Elovich equation.The sorption rate and sorption amount of p-nitrophenol on the Mg_2Al-CLDH was higher than that on the Mg_2Al-LDH.The sorption amounts of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH were independent of the initial pH in the range of about 3～10.The increases of temperature,the adsorption amounts decrease.CLDH was promising to be a new kind of high effective adsorbents for phenols.
本文选择带结构负电荷的蒙脱土、基本不带结构电荷(或带微量结构负电荷)的高岭土和带结构正电荷的层状双金属氢氧化物(Layered double hydroxides,简称LDHs)为模型吸附剂,研究了对重金属铅的吸附行为,考察了多种因素的影响,以期探讨结构电荷(或由此引起的界面相微环境酸碱性)对重金属吸附的影响规律,加深对吸附机理的认识。同时,考察了煅烧层状双金属氢氧化物(CLDHs)、LDHs-EDTA纳米杂化物等对铅和对硝基苯酚的吸附,以期为高效吸附剂的开发提供信息。
主要研究内容和结论归纳如下。
一、蒙脱土和高岭土对Pb~(2+)的吸附作用及机理研究
主要研究了Pb~(2+)在蒙脱土和高岭土上的吸附性能,考察了温度、pH值、离子强度和吸附剂含量等因素对吸附的影响,并结合X射线光电子能谱(XPS)、XRD和比表面积等实验结果探讨了吸附机理。研究表明,蒙脱土和高岭土吸附Pb~(2+)的动力学曲线符合准二级动力学方程和Elovich方程,等温线符合Langmuir方程。以mg/g为单位时,蒙脱土的饱和吸附量明显高于高岭土,而以mg/m~2为单位时,二者相近。吸附量主要由黏土的比表面积决定,而吸附力由黏土的结构电荷密度决定。Pb~(2+)在蒙脱土和高岭土上的吸附机理可分为化学键合吸附(或内络合层吸附)和静电键合吸附(或外络合层吸附),其中静电键合吸附主要为结构负电荷位吸附。化学键合吸附具有强的选择性和不可逆性,不受离子强度的影响;静电键合吸附没有选择性,具有较强的可逆性,受离子强度的影响较大。化学键合吸附和静电键合吸附的相对量与pH有关;在pH小于4和大于8的范围内,化学键合吸附为主,而在pH4～8范围内静电键合吸附比例增大。pH增高,吸附量增高;温度、离子强度和吸附剂含量增大,吸附量下降。Pb~(2+)能进入蒙脱土的层间,而不能进入高岭土的层间;部分Pb~(2+)可进入黏土颗粒的微孔中被固定。EDTA可明显降低Pb~(2+)在蒙脱土上的吸附,而基本不影响在高岭土上的吸附。
二、层状双金属氢氧化物及其煅烧产物对Pb~(2+)的吸附作用
合成了Mg/Al摩尔比分别为1:1和2:1的Mg-Al-LDHs样品(MgAl-LDH和Mg_2Al-LDH)及其煅烧产物(MgAl-CLDH和Mg_2Al-CLDH),同时还合成了乙二胺四乙酸(EDTA)-LDH纳米杂化物,考察了它们对Pb~(2+)的吸附作用。结果表明,Mg-Al-LDHs和Mg-Al-CLDHs对Pb~(2+)均有很强的吸附能力,有望成为一类新型高效吸附剂;吸附动力学符合准二级动力学过程,吸附等温线符合Freundlich方程。吸附量在pH=3～10的范围内变化不大。电解质可抑制Pb~(2+)在Mg-Al-LDHs上的吸附,但基本不影响在Mg-Al-CLDHs上的吸附。吸附机理为表面络合吸附,在Mg-Al-LDHs上的吸附同时存在化学键合(内层络合)吸附和静电键合(外层络合)吸附,而在Mg-Al-CLDHs的吸附主要为化学键合吸附。
Mg-Al-CLDHs对Pb~(2+)的吸附能力明显高于相应的Mg-Al-LDHs;EDTA-LDH纳米杂化物也明显高于相应的Mg-Al-LDHs,表明EDTA的插入具有协同增效作用。
三、对硝基苯酚在Mg_2Al-LDH及其煅烧产物上的吸附
研究了对硝基苯酚在Mg_2Al-LDH和Mg_2Al-CLDH上的吸附,考察了pH、温度等因素的影响。结果表明,对硝基苯酚在Mg_2Al-LDH和Mg_2Al-CLDH上均有明显吸附,其吸附等温线均符合Freundlich等温式;在Mg_2Al-LDH上的吸附动力学符合双常数方程,而在Mg_2Al-CLDH上符合准一级动力学速率方程和Elovich方程;在Mg_2Al-CLDH上的吸附速率和吸附量明显高于Mg_2Al-LDH。初始pH在3～10范围内变化对吸附量的影响不大。温度升高,吸附量增大。CLDHs有望成为一种新型的高效酚类有机污染物处理剂。
With the development of industry and agriculture,the emission of pollutants is increasing which causes serious harm to ecological safety and human health.Heavy metal pollution is one of the environmental problems to be urgently resolved.The remediation of heavy metal contaminated soil and the treatment of waste water have become hot topics of environmental science and engineering.The adsorption/desorption behavior of heavy metal at the solid liquid interface is the fundamental problem which determines the geochemistry process of heavy metal and environmental ecological effect.The scientific knowing of the basic phenomena is the basis of understanding the speciation distribution,transport and fate of heavy metal pollutants and techonolgy on remediation of contaminated soil and waste water treatment.A great deal of studies have been done on the adsorption of heavy metal at the solid liquid interface and an overall understanding to adsorption law has been reached, however,the adsorption mechanism is not very clear due to the complexity of adsorption systems.Moreover,the adsorbents studied are usually negative charged.Rare studies have been done about positive charged heavy metal adsorbents.
We choose structurally negative charged montmorillonite,structurally no charged kaolinite(or small quantity of negative structural charge)and structurally positive charged layered double hydroxides as model adsorbents and study the adsorption behavior of Pb~(2+) on them.The influence of various factors were investigated to obtain the influence law of structural charge(or interface phase microenvironmental acidity induced by it)on heavy metal adsorption and deepen the cognition to the adsorption mechanism.Adsorption of p-nitrophenol and Pb~(2+)on MgAl-CLDHs,adsorption of Pb~(2+)on LDHs- EDTA were also discussed to supply information to the development of the high- efficiency sorbent.
The contents include the followings:
Section1.Study on adsorption behavior and adsorption mechanism of Pb~(2+)on montmorillonite and kaolinite
Sorption properties of Pb~(2+)on montmorillonite and kaolinite were studied,the influence of temperature,solution pH,ion strength and sorbent content on the sorption of Pb~(2+)were investigated,and the sorption mechanism was discussed in combination with the results of XPS,XRD and specific surface area(SSA)experiments.The sorption kinetics can be well described by the pseudo-second-order kinetics and the Elovich kinetic equation and the sorption isotherms can be described by Langmuir isotherm.The sorption amount in mg/g of Pb~(2+)on montmorillonite is obviously higher than that on kaolinite,however that in mg/m~2 on montmorillonite is very close with that on kaolinite.Adsorption amount is mainly determined by the SSA while the adsorption ability is determined by structural negative charge density of clays.The sorption mechanism of Pb~(2+)on the montmorillonite and kaolinite may be distinguished to the chemi-bonded adsorption(or inner-sphere surface complexation adsorption)and electrostatic-bond adsorption(or outer-sphere surface complexation adsorption).The electrostatic-bond adsorption is mainly negative structural charge sites adsorption.The chemi-bonded adsorption is irreversible,strong selective and the ionic strength has no effect on it.The electrostatic-bond adsorption is reversible,no selective and the ionic strength has a significant effect on it.The relative content of chemi-bonded adsorption and the electrostatic-bond adsorption is dependent of pH,and the relative content of the electrostatic-bond adsorption in the pH range of 4～8 is higher than in the pH ranges of lower than 4 and higher than 8.The increases of temperature,ion strength and sorbent content would induce the decrease of the adsorption amounts of Pb~(2+)on montmorillonite and kaolinite while the sorption amount increases with increasing pH.Pb~(2+)can be intercalated between the layers of the montmorillonite while it can not be intercalated between the layers of kaolinite.Portion of Pb~(2+)can be fixed by enterring in the micropore of clay particles.EDTA can significantly decrease the adsorption of Pb~(2+)on montmorillonite,hardly affects the adsorption of Pb~(2+)on kaolinite.
Section2.Adsorption of Pb~(2+)on MgAl Layered double hydroxides and their calcined products
Layered double hydroxides with an Mg/Al molar ratio of 1:1(MgAl-LDH),2:1 (Mg_2Al-LDH)and EDTA-LDH nanohybrids were synthesized by using a co-precipitation method and calcined LDHs(CLDHs)were obtained by calcination LDHs at 500℃.The sorption removal of Pb~(2+)by them was investigated.It was found that both Mg-Al-LDHs and Mg-Al-CLDHs show good sorption ability and they could be a new type of environmental sorbent for the removal of Pb~(2+).The sorption kinetics and the sorption isotherms of Pb~(2+)on both the Mg-Al-LDHs and the Mg-Al-CLDHs can be described by the pseudo-second order kinetics and Freundlich isotherm,respectively.The sorption amounts of Pb~(2+)are independent of the pH in the range of about 3～10.The presence of electrolyte inhibited the sorption of Pb~(2+)on the Mg-Al-LDHs while not on the Mg-Al-CLDHs.The sorption mechanism of Pb~(2+)may be contributed to the surface complexation.The adsorption of Pb~(2+)on the Mg-Al-LDHs may be contributed to both the chemi-bonded adsorption(or inner-sphere surface complexation adsorption)and the electrostatic-bond adsorption(or outer-sphere surface complexation adsorption),while that on the Mg-Al-CLDHs mainly to the chemi-bonded adsorption.
The adsorption ability of Pb~(2+)on the Mg-Al-CLDHs is higher than that on the Mg-Al-LDHs.The adsorption ability of Pb~(2+)on the EDTA-LDH nanohybrids is also higher than that on the Mg-Al-LDHs which indicates the intercalation of EDTA had synergy.
Section3.Adsorption of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH
The sorption removal of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH were investigated.The influence of pH,temperature on the adsorption was investigated.The results showed that p-nitrophenol could be adsorbed on both Mg_2Al-LDH and Mg_2Al-CLDH.Adsorption isotherms could be fitted with the Freundlich equation,the sorption kinetics of p-nitrophenol on Mg_2Al-LDH could be well described by the two-constant equation while the sorption kinetics of p-nitrophenol on Mg_2Al-CLDH could be well described by pseudo-first-order kinetics and Elovich equation.The sorption rate and sorption amount of p-nitrophenol on the Mg_2Al-CLDH was higher than that on the Mg_2Al-LDH.The sorption amounts of p-nitrophenol on Mg_2Al-LDH and Mg_2Al-CLDH were independent of the initial pH in the range of about 3～10.The increases of temperature,the adsorption amounts decrease.CLDH was promising to be a new kind of high effective adsorbents for phenols.
引文
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Fig1.X-ray diffraction patterns of Mg-Al LDH(a)and EDTA-LDH(b)
Fig2.Infrared spectra of Mg-Al LDH(a)and EDTA-LDH(b)
Fig3.Adsorption isotherms of Pb~(2+)on Mg-Al LDH(a)and EDTA-LDH(b)