聚合物基新型复合吸附材料的制备及对水体中重金属污染物的吸附性能研究

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英文题名：Preparation of Novel Composite Adsorbents Based on Polymer Matrix and the Research on the Adsorption of Heavy Metals in Aqueous Solutions 作者：李晓丽 论文级别：博士 学科专业名称：环境科学 中文关键词：聚合物 ; 重金属去除 ; 废水处理 ; 静态吸附 ; 动态吸附 英文关键词：Polymer ; Heavy metal removal ; Wastewater treatment ; Static adsorption ; Dynamic adsorption 学位年度：2013 导师：李彦锋 学科代码：083001 学位授予单位：兰州大学 论文提交日期：2013-05-01

摘要

本学位论文综述了重金属水污染的现状与危害,重金属废水的处理技术与方法的国内外研究及进展,吸附法处理重金属废水的研究进展及复合型吸附材料的设计,开发与应用。人类的生产和生活活动产生的含有重金属的废水由于某些原因未经处理或处理未达标就排向自然环境,由此导致的重金属水污染已经对生态环境,公众健康和社会经济的可持续发展造成严重威胁。各种有效去除水体中的重金属的处理技术与方法受到了世界各国政府和研究者们的极大关注。采用吸附技术来处理含重金属的废水是一种非常有效和具有发展前景的方法之一。因此,设计,研究和开发具有特殊或优异性能的吸附材料,是该领域最前沿和最引人注目的研究热点之一。正是基于吸附技术的高效和易操作性,设计并合成了一系列吸附量大,去除效率高,吸附速率快,对某种金属离子具有特殊选择性识别,易于分离,重复利用率高,价格低廉,制备简单,对环境无污染的聚合物基新型复合吸附材料。并运用电镜扫描,X-射线衍射,傅立叶红外光谱等手段对新型吸附剂的物理化学性质进行表征。在静态吸附模式下,考察了不同的操作条件对聚合物基新型复合型吸附材料吸附净化水溶液中重金属效果的影响,以获得新型吸附剂吸附重金属的最佳条件和最佳效果。并在此基础上,运用各种等温线模型,动力学模型和热力学模型对吸附平衡进行分析,研究吸附过程的性质,控速步骤及热力学行为。同时借助傅立叶红外光谱和光电子能谱对吸附净化机理进行探讨。再次,对吸附剂的解吸,再生及重复使用性能进行了研究。考察不同的解吸剂及浓度对解吸效果的影响,优化解吸操作,使新型吸附剂的吸附-解吸-再吸附操作能够持续进行。最后采用动态固定床工艺研究了新型吸附剂吸附净化重金属的效果与流速和进水金属浓度之间的关系,并采用动态数学模型对穿透曲线进行分析,为新型吸附剂的实际运用提供理论依据。本学位论文取得的主要研究结果如下：
     1.以CaCO3为发泡剂联合冻融循环方法制备了聚乙烯醇／壳聚糖(PVA/CS)复合型泡沫,通过批吸附实验研究了PVA/CS泡沫对水溶液中的Cu2+离子的吸附性能。研究结果显示,CS的引入不仅增强了PVA/CS泡沫的机械,化学和热力学稳定性,还提高了吸附能力,而且PVA, CaCO3和CS的不同配比对PVA/CS泡沫的吸附性能也产生了明显影响。PVA/CS泡沫对Cu2+的最大吸附量可达193.39mg/g,对含低浓度的Cu2+溶液去除效率高,吸附平衡符合Langmuir等温线模型,并且吸附是一种自发和吸热的过程。PVA/CS泡沫对Cu2+离子具有快的吸附速率,其吸附动力学遵循准二级化学反应模型,粒子内扩散是限速步骤,吸附过程同时涉及到化学吸附和物理吸附,这与PVA/CS泡沫的大网络结构和存在大量氨基和羟基有关。最后,考察了各种解吸剂的解吸效率,6个吸附-解吸循环对吸附剂的可重用性进行了评估。
     2.以CaCO3为开孔剂,以硼酸为交联剂制备了PVA/CS大孔复合球,通过批吸附实验研究了PVA/CS大孔球对Cu2+,Pb2+,Zn2+和Cd2+离子的去除性能。研究显示,PVA/CS复合球具有大孔三维网络状结构。在吸附过程中,PVA和CS呈现出一种协同增强效应。该复合球吸附四种金属离子的能力为：Cu2+＞Pb2+＞Cd2+>Zn2+,动力学显示Pb2+和Cd2十的吸附速率要快于Cu2+和Zn2+。PVA/CS球呈现出明显的选择性,可从混合金属溶液中选择性去除Cu2+。为了拓宽PVA/CS大孔复合球的使用范围,同时制备了有机P掺杂的PVA/CS/ATMPZ大孔复合球明显增强了对Pb2+的吸附容量和选择性,加快了吸附速率,使pH的适用范围更宽广。在此基础上,采用Langmuir, Freundlich, Tempkin和D-R等温线；准一级反应,准二级反应和粒子内扩散方程来研究PVA/CS球和PVA/CS/ATMPZ球吸附过程的性质与限速步骤。对新型吸附剂的解吸与重复使用性能进行了评估。最后考察了动态实验条件下,PVA/CS/ATMPZ大孔复合球实际去除Pb2+的能力。
     3.首先制备了-]NH2功能化的ZrO2(ZrN),耳将其包埋在PVA中形成大孔球状PVA/ZrN来增强复合材料的使用性能。采用批吸附模式研究了ZrN和PVA/ZrN对水溶液中金属离子的吸附性能。结果发现,氨基的引入明显增强了对Hg2+,Ag+,Cu2+离子的吸附能力。ZrN和PVA/ZrN对Hg2+,Ag+,Cu2+离子的最大吸附容量要高于很多其他类型的吸附剂,可以更好地去除废水中的重金属离子。ZrN吸附三种金属离子的平衡数据最符合Langmuir等温线模型,而PVA/ZrN则复合Freundlich等温线。同时,ZrN和PVA/ZrN的吸附动力学可以用准二级动力学来解释,吸附过程是一个复杂的过程,涉及到表面吸附,孔内扩散和化学反应过程。FTIR和XPS分析显示,羟基和金属表面羟基中的O原子和氨基中的N原子与重金属离子之间发生了螯合和／或离子交换。
     4.合成了包含大量功能团如氨基,羟基,羧酸盐基的新型PVA/CNTs-NC大孔复合球,并通过批吸附和柱吸附实验考察了PVA/CNTs-NC去除净化水溶液中Pb2+和Cu2+的性能。研究发现,氨基和羧酸盐功能团的引入极大地增强了CNTs-NC对Pb2+和Cu2+的吸附性能,呈现出高的去除率,快的吸附速率和宽的pH适用性。PVA/CNTs-NC的吸附量稍低于CNTs-NC,但是球形吸附剂的使用性能更强,易于分离和重复使用。CNTs-NC和PVA/CNTs-NC吸附Pb2+和Cu2+的平衡数据符合Langmuir单分子层吸附等温线。PVA/CNTs-NC对Pb2+的吸附速率明显快于Cu2+,表面吸附和粒子内扩散是两个主要的吸附机制。FTIR和XPS分析显示Pb2+和Cu2+离子与氨基的N和羧酸盐基团的O之间发生了络合反应。在动态吸附操作中,降低流速和进水金属浓度可以获得更高的吸附量和去除效率。另外,PVA/CNTs-NC的解吸-再生-再吸附操作呈现出高的重复使用效率。
     5.制备了一种新型磁性Zr(Ⅳ)交联海藻酸盐聚合物凝胶球(Fe3O4@SA-Zr),并考察了其对水中Pb2+的去除性能。合成的Fe3O4@SA-Zr具有大孔球形结构,良好的稳定性,还易于磁分离。实验结果表明,当初始Pb2+浓度低于200mg/L时,Fe3O4@SA-Zr几乎可以去除废水中100%的Pb2+。在Cu2+,Zn2+,Cd2+,Hg2+存在下,Fe3O4@SA-Zr可以选择性去除Pb2+。Fe3O4@SA-Zr对Pb2+的吸附非常符合Langmuir等温线模型,最大吸附量可达333.33mg/g。Pb2+的吸附动力学最符合准二级反应动力学模型。动态工艺研究发现,流速和进水金属浓度严重影响了穿透曲线的形状,较大的流速和较高的金属浓度将会使床层穿透和饱和加快。10个吸附-解吸循环之后,Fe3O4@SA-Zr对Pb2+吸附量仍可达到92%。
     6.首先以Zr(IV)与多乙烯多胺(EDA/DETA/TETA)反应制备了无机基聚合物Zr-(EDA/DETA/TETA),将其包埋在TA和SA-Ca形成的有机聚合物网络中形成有机/无机离子交联聚合物凝胶球,并以其作为新型吸附剂通过批吸附和柱吸附模式来考察对水溶液中的Pb(Ⅱ),Hg(Ⅱ),Cr(Ⅵ)离子的去除能力。对比实验结果显示,以Zr-DETA/TA/SA-Ca的吸附效率最高,对Pb(Ⅱ),Hg(Ⅱ)和Cr(Ⅵ)离子的最大吸附容量分别为379.75,421.15和131.15mg/g。三种重金属离子的吸附平衡最符合Langmuir等温线方程,吸附动力学显示,Pb(Ⅱ)和Hg(Ⅱ)离子的吸附速率要明显快于Cr(Ⅵ)离子,三种离子的动力学数据均符合准二级动力学模型,说明化学吸附是限速步骤。同时考察了Zr-DETA/TA/SA-Ca处理实际电镀含铬废水的效率,结果显示,废水中的Cr(Ⅵ)的去除率高达97%以上,出水中Cr(Ⅵ)的浓度≤0.5mg/L,符合废水排放标准,说明Zr-DETA/TA/SA-Ca具有非常好的实际应用的潜力。
The wastewater containing heavy metals produced from various human activities was discharged into the natural environment and caused soil, surface water and groundwater pollution, which has become the serious threat to the ecological environment, public health and the sustainable development of social economy. How to effectively remove the heavy metals in aqueous solution, various treatment technologies and methods have been attracted great attention by researchers and the governments around the world. Adsorption is one of the most effective and promising technologies used to remove heavy metals due to its simplicity, high efficiency, easy handing and no sludge generation. In recent years, various efforts have been focused on the research and development of novel adsorption materials with excellent properties such as large adsorption capacity and high selectivity, fast adsorption rate, easy separation and reusability, low cost, simple preparation, no secondary pollution.
     This paper summarized the present situation and the harm of heavy metals pollution, the development of technologies and methods for treatment of heavy metals at home and abroad, the development of adsorption technology for removal of heavy metals from aqueous solutions, and the preparation and application of novel composite adsorption materials. Based on the excellent properties of polymer, poly(vinyl alcohol) and sodium alginate were chosen as the supporter. Seven different kinds of polymer-based composite adsorbents were prepared including PVA/CS foam, PVA/CS beads, PVA/CS/ATMPZ beads, PVA/ZrN beads, PVA/CNTs-NC beads, Fe3O4@SA-Zr beads and Zr-DETA/TA/SA-Ca beads. These new adsorbents were characterized by FTIR, XRD, SEM, TGA, XPS, and so on. Tests were then conducted to study their adsorption performance for heavy metal ions and the effects of experimental parameters such as solution pH, initial metal concentration, contact time, temperature, ionic strength, humic acid and competitive ions on the removal of heavy metal ions were investigated in batch systems. Isotherms, kinetic and thermodynamic models were used to fit the experimental data to understand the adsorption mechanisms and the rate-limiting step. FTIR and XPS were used to analyze the mechanisms involved in the adsorption of heavy metals. Desorption efficiency and regeneration potential of novel adsorbents were studied by using various desorbing agents and several adsorption-desorption cycles were repeated to evaluate the reusability. The ability of novel adsorbents to remove heavy metal ions was further conducted by using the fixed-bed continuous column and breakthrough curves were analyzed at different flow rates and influent metal concentrations. Thomas model was used to analyze the dynamics of the adsorption column.
     1. A novel composite foam of PVA and CS was prepared by using CaCO3as forming agent and cryogenic-thawed treatment. Batch adsorption experiments were carried out to study the ability of PVA/CS foam to remove heavy metal ions from aqueous solution. The results showed that the introduction of CS not only enhanced mechanical strength, chemical and thermodynamic stability, but also improved the adsorption capacity. Different mass rations of PVA/CaCO3/CS had a significant effect on the adsorption of PVA/CS foam. The maximum adsorption capacity of PVA/CS foam was193.39mg/g, and removal efficiency of Cu2+was higher at lower metal concentration. Equilibrium data of Cu2+onto PVA/CS foam was best described by Langmuir isotherm and adsorption was a spontaneous and endothermic process. PVA/CS foam exhibited rapid adsorption rate, kinetic data was followed the pseudo-second order model, intraparticle diffusion was the rate limiting step and chemical and physical adsorption were involved in the adsorption process, which may be due to the network structure and many functional groups such as amine and hydroxyl groups. Finally, desorption efficiency and reusability of PVA/CS foam were assessed based on six consecutive adsorption-desorption cycles.
     2. Novel macroporous PVA/CS beads were prepared by using CaCO3as pore-forming agent and boric acid as cross-linking agent. Batch adsorption experiments were carried out to study the ability of PVA/CS beads for the removal of heavy metal ions from aqueous solution. The results showed that PVA/CS beads had the macroporous and three-dimensional network structure. PVA and CS exhibited a synergistic effect on removal of heavy metal ions. PVA/CS beads adsorbed heavy metals in the following order:Cu2+>Pb2+>Cd2+>Zn2+and showed faster kinetics for Pb2+and Cd2+than for Cu2+and Zn2+. PVA/CS beads could selectively remove Cu2+ions from the mixed-metal solution. In order to broaden the scope of application of PVA/CS beads, organic P doped PVA/CS/ATMPZ macroporous beads were prepared. PVA/CS/ATMPZ beads significantly enhanced the adsorption capacity and selectivity towards Pb2+ions, improved the adsorption rate and the efficiency in a wide range of pH. Various isotherm models (Langmuir, Freundlich, Tempkin and D-R), kinetic model (pseudo-first order, pseudo-second order and intraparticle diffusion) and thermodynamic models were used to study the mechanism and the rate-limiting step. The desorption efficiency and reusability of the adsorbents were assessed based on the consecutive adsorption-desorption cycles. Finally, dynamic experiments were conducted by using the fixed-bed continuous-flow column to further evaluate the potential of PVA/CS/ATMPZ for Pb2+removal.
     3. Amine functionalized ZrO2(ZrN) was prepared and was then embedded into PVA to form spherical macroporous adsorbent (PVA/ZrN). The adsorption performances of ZrN和PVA/ZrN for heavy metal ions in aqueous solution were studied in batch mode. It was found that the introduction of amine significantly improved the adsorption capacities for Hg2+, Ag+, Cu2+ions. The maximum adsorption capacities of PVA/ZrN beads for Hg2+, Ag+. Cu2+were higher than several adsorbents reported in the literature. The adsorption data of Hg2+, Ag+, Cu2+onto ZrN was best fitted the Langmuir isotherm while those onto PVA/ZrN followed the Freundlich isotherm. The kinetics was found to follow the pseudo-second order kinetic model. Surface adsorption, intraparticle diffusion and chemical reaction were involved in the adsorption process. From FTIR and XPS results, new complexes were formed between metal ions and nitrogen in amine groups and oxygen in hydroxyl groups through chelation and/or ion exchange.
     4. This work evaluated the macroporous PVA/CNTs-NC beads containing hydroxyl, carboxylate and amine groups for removing target pollutants Pb2+and Cu2+from aqueous solutions in batch and column modes. CNTs-NC exhibited higher adsorption capacities and efficiencies, rapid adsorption rate and wide application of pH for Pb2+and Cu2+ions. While adsorption capacities of PVA/CNTs-NC for Pb2+and Cu2+were lower than those of CNTs-NC. However, the spherical adsorbents were very easily separated from the solution and reused, which was especially important for continuous flow operations. The adsorption of Pb2+and Cu2+onto CNTs-NC and PVA/CNTs-NC was well described by Langmuir isotherm, indicating a monolayer adsorption. it was found that the adsorption rate of Pb2+was faster than that of Cu2+, surface adsorption and intraparticle diffusion were involved in Pb2+and Cu2+adsorption. FTIR and XPS indicated that nitrogen in amine groups and oxygen in carboxylate groups were the main active sites for metal ions binding. In column studies, PVA/CNTs-NC exhibited excellent performances in the removal of Pb2+, higher adsorption capacity and efficiency were obtained at low influent metal concentration and flow rate. Moreover, adsorption-desorption operations showed that PVA/CNTs-NC was a good reusable adsorption material.
     5. A novel magnetic sodium alginate-zirconium(IV) composite beads (Fe3O4@SA-Zr) were prepared by using Zr(IV) as the crosslinking ions and used as an adsorbent for the selective removal of Pb2+from aqueous solution by batch and fixed-bed column systems. The prepared Fe3O4@SA-Zr had the spherical and macroreticular structure, good stability and magnetic separation. Almost100%of Pb2+was removed by Fe3O4@SA-Zr when the initial metal concentration was lower than200mg/L. The competitive adsorption showed that Fe3O4@SA-Zr beads had good adsorption selectivity for Pb2+with the coexistence of Cu2+, Zn2+, Cd2+, Hg2+. Langmuir isotherm fitted the experimental data well and the maximum adsorption capacity was333.33mg/g. The kinetics was found to follow the pseudo-second-order model and the adsorption rate was controlled by a chemical sorption process. In the column study, flow rate and influent metal concentration significantly affected the shape of breakthrough curves, higher flow rate and influent metal concentration resulted in the earlier breakthrough time and exhaustion time. The dynamic adsorption of Pb2+by Fe3O4@SA-Zr followed the Thomas model. The adsorption capacity of Fe3O4@SA-Zr for Pb2+ions was maintained92%after10successive adsorption-desorption cycles.
     6. A novel polymer based on inorganic hybrid, Zr-(EDA/DETA/TETA), was prepared through the reaction Zr(Ⅳ) with three types of amine (EDA/DETA/TETA), which was then embedded into TA and SA-Ca organic polymer network and formed organic/inorganic ionically crosslinked polymer gel beads. The adsorption properties of Zr-(EDA/DETA/TETA)/TA/SA-Ca for Pb(Ⅱ), Hg(Ⅱ),Cr(Ⅵ) ions were studied by using the batch and column operations. Zr-DETA/TA/SA-Ca had the highest adsorption efficiencies for Pb(Ⅱ), Hg(Ⅱ) and Cr(VI) among all the beads prepared and the maximum adsorption capacities were reached to379.75,421.15和131.15mg/g, respectively. The equilibrium data of Pb(Ⅱ), Hg(Ⅱ) and Cr(Ⅵ) ions was fitted the Langmuir isotherm, indicating a monolayer adsorption. From kinetic studies, it was found that the adsorption rate of Pb(Ⅱ) and Hg(Ⅱ) was faster than that of Cr(VI) ions and reached the equilibrium around120,120and780min, respectively. For all the metal ions studied, chemical reaction may be the rate-controlling step and the pseudo-second-order kinetic model provided the best correlation of the experimental data. Importantly, Zr-DETA/TA/SA-Ca was able to remove97%of Cr(Ⅵ) in actual electroplating wastewater containing Cr(Ⅵ). Cr(Ⅵ) concentration in the effluent was0.5mg/L or less which was lower than the wastewater discharge standard, indicating that Zr-DETA/TA/SA-Ca had the very good potential in practical application.

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