摘要
目前地下水中重金属和有机物环境污染问题备受人们关注。吸附法是一种简单、快速有效去除污染物的方法，其关键问题在于吸附材料。碳纳米管作为一种新型吸附剂，由于具有独特的多孔和空心结构、较大的比表面积以及与污染物间的多种相互作用，对水相中多种无机和有机污染物具有优异的吸附性能，引起学者广泛关注。
本论文根据碳纳米管孔径结构和表面性质在制备过程中具有广泛调控的特性，通过碳纳米管生长条件的控制和液相氧化、固相活化和磁性修饰等多种化学改性方法，实现碳纳米管表面物理和化学性质的控制，获得一系列新型改性碳纳米管吸附剂。本论文定性定量地系统研究改性碳纳米管的物理、化学性质与污染物吸附特性之间的内在关系。针对实际环境中普遍存在的多种污染物共存现象，结合采用X射线光电子能谱（XPS）、X射线吸收近边结构（XANES）和扩展X射线吸收精细结构光谱（EXAFS）表征手段，从微观分子水平探讨改性碳纳米管与单一污染物的吸附作用及多种污染物共存的竞争吸附机理。并设计出一种制备简单、低成本且高吸附性能的磁性碳纳米管的新方法，为碳纳米管大规模应用提供一种新思路。
本论文的主要研究结果如下：
(1)不同含氧量碳纳米管的制备及其表面含氧量对苯系物吸附的影响
通过控制次氯酸钠氧化剂的浓度，制备具有不同含氧量的多壁碳纳米管（MWCNTs），作为吸附剂研究不同含氧量对苯系物吸附特性的影响。随着改性MWCNTs表面含氧量的增加，苯系物吸附性能呈现先增加后降低的趋势。MWCNTs表面含氧量增加会提高吸附剂在水相中的亲水性和分散性，当含氧量增加到一定程度时其表面形成的水膜会阻碍苯系物与MWCNTs表面发生相互作用。水膜的抑制作用是不同含氧量MWCNTs吸附苯系物的一个主要作用机制，适当控制碳纳米管表面含氧量有利于苯系物吸附。
(2)活化MWCNTs的制备及其物理化学性质对苯系物吸附的影响
采用KOH活化法，控制KOH/MWCNTs质量比，制备具有不同比表面积的活化MWCNTs。活化MWCNTs对苯系物的吸附性能均随着KOH/MWCNTs质量比增加而显著提高。采用相关分析法定量地系统研究发现：活化MWCNTs的比表面积、介孔孔容和比表面积归一化的羟基相对含量与苯系物的吸附量、吸附系数均成良好的正线性相关，并得到介孔孔容和羟基官能团与吸附性能的回归方程，介孔填充和氢键作用是活化MWCNTs吸附苯系物的两个主要吸附机理，结果突出了碳纳米管的孔径和表面化学性质的协同作用对苯系物吸附具有重要意义。
(3)一步法制备具有高吸附性能和良好磁分离效果的磁性碳纳米管
以含纳米铁的碳纳米管原始样品（APCNTs）为原材料，采用KOH活化一步法制得具有磁分离特性的MWCNTs/FexOy复合材料(APCNTs-KOH)，将其用于水相中苯系物吸附。APCNTs-KOH吸附苯系物的能力较APCNTs显著提高，同时APCNTs所含纳米铁催化剂颗粒被转化成磁性Fe_3O_4或γ-Fe_2O_3，从而实现MWCNTs粉体在水相中快速磁分离，减小纳米粉体可能带来的二次污染。该方法大幅度降低制备经济成本，为碳纳米管的大规模应用提供新的科学指导思路。解吸附实验结果表明APCNTs-KOH对五种苯系物存在明显的滞后现象，是由于吸附质进入吸附剂的微孔或刚性区域中而不易解吸出来所导致。
(4)苯系物和重金属共吸附及其微观作用机理研究
Pb~(2+)的存在抑制苯系物（TEX）在CNTs-3.2%O上的吸附；随着TEX初始浓度的增大，Pb~(2+)对TEX吸附抑制程度有减小的趋势，Pb~(2+)对甲苯的抑制作用最明显。TEX的同时加入抑制Pb~(2+)或Cu~(2+)在CNTs-5.9%O上的吸附；不同初始浓度TEX对Pb~(2+)吸附抑制作用差异不大；随着Pb~(2+)初始浓度的增大，TEX对其抑制作用减弱。应用XPS、XANES和EXAFS先进的微观表征手段从分子层面研究苯系物、重金属及两者共存时的吸附机理，结果表明：第一，Pb~(2+)与CNTs-3.2%O含氧官能团形成O-Pb键，直接占据CNTs-3.2%O部分吸附位点；由于Pb~(2+)较强的水合作用而在其周围形成致密的水化核，可能挤压、遮蔽CNTs-3.2%O表面位点，间接与苯系物发生位点竞争，从而Pb~(2+)抑制CNTs-3.2%O对TEX吸附。第二，Cu~(2+)与CNTs-5.9%O表面的羧基或羟基形成内层配合物，Pb~(2+)与CNTs-5.9%O含氧官能团形成O-Pb键，TEX与CNTs-5.9%O表面含氧官能团存在一定的相互作用。由于TEX吸附占据CNTs-5.9%O表面吸附位点，直接与Pb~(2+)或Cu~(2+)发生位点竞争，从而TEX抑制CNTs-5.9%O对Pb~(2+)或Cu~(2+)吸附。
Groundwater contamination of organic contaminants and heavy metals has drawnwidespread attention. Adsorption is a simple, fast and efficient method to remove organiccontaminants and heavy metals, and the most critical technical problem is adsorbents.Carbon nanotubes (CNTs) have aroused widespread attention as a new type of adsorbentsdue to their outstanding ability for the removal of various inorganic and organiccontaminants. CNTs have been the focus of considerable research because of their highlyporous and hollow structure, large specific surface areas, and CNTs show stronginteractions with organic compounds.
The pore structure and surface chemical properties of CNTs can be effectivelycontrolled by adjusting the synthesis parameters and modifying by liquid phase oxidation,solid phase activation and magnetic modification, and then some new types of modifiedmulti-walled carbon nanotubes (MWCNTs) were successfully synthetized in this study.The systematic study of the relationship between physicochemical properties andadsorption characteristics of TEX onto modified MWCNTs by qualitative and quantitativeanalysis has been investigated. Both heavy metals and organic contaminants may coexist atmany contaminated sites. Furthermore, the molecular science techniques were utilized toprobe and elucidate the relevant mechanisms from adsorption sites and coordinationenvironment of adsorbates by X-ray photoelectron spectroscopy (XPS), X-ray absorptionnear edge structure (XANES) and extended X-ray absorption fine structure (EXAFS)spectroscopy. A facile one-pot method for synthesis of low-cost magnetic MWCNTs hasbeen reported, which will be of great significance for large-scale practical applications ofCNTs.
The important conclusions of this work are summarized as follows:
(1) Synthesis of MWCNTs with different oxygen contents and the influence of theirsurface oxygen content on TEX adsorption
MWCNTs with different oxygen contents were prepared by oxidization usingdifferent concentration NaClO solutions. With the increase of surface oxygen content,maximum adsorption capacities of TEX firstly increased, and then, began to decrease. Thesurface functionalization of the oxidized MWCNTs can improve their dispersibility inaqueous solutions, which consequently can be favorable for the aqueous phase adsorption.However, when oxygen content increases to a certain extent, oxygen-containing functionalgroups cause water clusters formation on the surface or tube end of MWCNTs, whichhinder the interaction between TEX and MWCNTs. The decrease indicates that theformation of water clusters plays a more important role than the better dispersion ofMWCNTs for TEX adsorption.
(2) Synthesis of MWCNTs with different specific surface area and the influence oftheir physicochemical properties on adsorption characteristics of ethylbenzene and xyleneisomers
MWCNTs with different specific surface area (SSA) by adjusting KOH/MWCNTsmass ratio were prepared using KOH activation. With the increase of KOH/MWCNTsmass ratio, adsorption capacities of ethylbenzene and xylene isomers (EX) greatlyincreased. A systematic quantitative analysis of the relationships between thephysicochemical properties of activated MWCNTs and adsorption characteristics of EXwas studied by correlation analysis. There are strong positive correlations between theadsorption affinity (or capacity) and SSA, mesopore volumes or hydroxyl groups, and theirregression equations have been obtained. Mesopore-filling and hydrogen-bond interactioncould be a predominant mechanism governing monoarmatics adsorption onto activatedMWCNTs. Results highlight the synergetic effects of porosity and surface chemistry incontrolling adsorption of monoaromatics onto MWCNTs in wastewater treatment.
(3) A facile one-pot method for synthesis of low-cost magnetic MWCNTs and theirapplication for TEX adsorption
A facile one-pot method was devised to produce magnetic MWCNTs (APCNTs-KOH)by KOH etching method using as-prepared MWCNTs (APCNTs). The adsorptioncapacities of TEX onto APCNTs-KOH are much higher than those onto APCNTs.Meanwhile, Fe nanoparticles of APCNTs were oxidized to Fe_3O_4/γ-Fe_2O_3, andAPCNTs-KOH could be effectively and immediately separated from aqueous solutions bya magnet, which reduces potential risks of CNTs as another source of environmentalpollution. Excellent magnetic materials APCNTs-KOH were prepared based on APCNTswith low cost, which is of great significance for large-scale practical applications of CNTs.Desorption of TEX showed a pronounced hysteresis for APCNTs-KOH, because someadsorbates may enter some micropores or rigid region of adsorbents.
(4) Mutual effects of heavy metals and TEX adsorption on modified MWCNTs andtheir relevant mechanisms from molecular levels
Pb~(2+)suppressed the adsorption of TEX onto CNTs-3.2%O, and the degree ofsuppression decreased with the increase of initial concentration of TEX. Among fiveadsorbates, adsorption of toluene was diminished more than others. TEX diminish theadsorption of Pb~(2+)or Cu~(2+)onto CNTs-5.9%O. The differende in initial concentrations ofTEX had little influence on the suppression of Pb~(2+). The degree of suppression decreasedwith the increase of initial concentration of Pb~(2+). The molecular environmental sciencetechniques, such as XPS, XANES and EXAFS, were utilized to probe and elucidate therelevant mechanisms from molecular levels. Pb~(2+)can form the O-Pb bond with surafaceoxygen-containing groups of CNTs-3.2%O, which may directly occupy part of the surfaceadsorption sites of CNTs-3.2%O. The large hydration sphere around surface complexes ofPb~(2+)may also intrude or shield hydrophilic sites, leading to the “crowding out” of TEXaround the metal cations-complexed sites, and thus Pb~(2+)can inhibit TEX adsorption onto CNTs-3.2%O. The results of XPS, NEXAFS and EXAFS indicate that the formation ofsurface or inner-sphere complexes of Cu~(2+)through carboxylic groups (or hydroxyl groups)and hydration of CNTs-5.9%O. Pb~(2+)can also form the O-Pb bond with oxygen-containinggroups of CNTs-5.9%O. There are some interactions between TEX and CNTs-5.9%Oindicated by the shift of bonding energy by XPS analysis, which could result in acompetition for adsorption sites between TEX and heavy metals ions. Thus, TEX directlyor indirectly inhibited Pb~(2+)or Cu~(2+)adsorption onto CNTs-5.9%O.
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