厌氧条件下纳米铁还原水中六价铀的反应动力学和机理研究
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摘要
由于人类对铀矿的开采和提炼,以及铀在核武器和核能源方面的广泛应用,造成了环境中大规模的铀污染,这使得了解铀在环境介质中的迁移转化过程十分必要。在自然环境中,铀可以以多种价态存在,包括零价、三价、四价、五价和六价。其中六价铀易溶于水,易于在水环境中传输并且容易被生物吸收；而四价铀难溶于水,通常以二氧化铀固体的形式存在,因此其在水环境中的活动性有限。由于水环境中铀的活动性在很大程度上取决于其化学价态,因此以还原六价铀为基础的修复技术被提出来治理地下水中的铀污染。近几年来,纳米铁作为新一代环境修复材料,已广泛应用于环境中有机污染物(如三氯乙烯和多氯联苯)的修复研究中；然而有关纳米铁还原固定水中铀的研究很少见报道。在本论文中,笔者详细研究了厌氧条件下纳米铁还原水中铀的反应动力学特征和反应机理。
本研究采用理论模拟和实验监测相结合的研究思路,利用批式实验和光谱分析的方法,系统研究了纳米铁去除和还原水中铀的主要影响因素,探讨了二价铁和三价铁在反应体系中的作用,研究了温度对反应的影响,利用X射线光电子能谱法鉴定了反应产物并研究了其可氧化性,最后比较了实验合成纳米铁和两种商业纳米铁的应用效果。通过对不同水化学条件下反应动力学数据的模拟和反应热力学参数的理论计算,对纳米铁还原固定水中的六价铀的反应机理进行了探讨。
本论文共分六章：
第一章简要介绍了问题的来源,研究的目的和意义,研究任务,以及论文的组织结构。
第二章共分三节：第一节介绍了铀的水环境地球化学特征,包括铀在水中存在的化学形态,水中铀的吸附,以及铀的化学还原和生物还原；第二节总结了纳米铁的特征和性质,然后回顾了其在环境修复中的应用,包括修复有机污染物和有毒重金属及放射性核素两个方面；第三节介绍了零价铁和铀反应的研究现状。
第三章详细研究了不同水化学条件下实验合成纳米铁去除和还原水中铀的反应动力学特征和反应机理。实验结果表明纳米铁能够快速去除水中的铀,水中铀的去除由吸附和还原所引起。研究证实铀的去除和还原速率随着pH值的升高而降低,水中的碳酸根和钙离子对纳米铁去除和还原水中铀具有明显的抑制作用,因为它们能与六价铀形成非常稳定的络合物。和其它还原剂(如普通铁粉、硫化氢、硫化铁和还原细菌)相比,纳米铁去除和还原水中铀的效果最好,并且水中碳酸根和钙离子的抑制作用相对较小。利用Scientist软件进行的反应动力学模拟结果表明,纳米铁还原水中铀分两步完成,即水中铀首先吸附到纳米铁的表面,随后六价铀被还原为四价。其反应过程如下：
第一步：(?)(吸附和解吸反应)
第二步(?)(还原反应)此外,X射线光电子能谱的实验结果(见第五章)也证实铀被还原为四价。
第四章采用螯合法研究了二价铁和三价铁在反应体系中的作用。两种铁的络合剂即1,10-邻菲罗琳(1,10-phenanthroline)和三乙醇胺(triethanolamine)分别用来络合反应体系中的二价铁和三价铁,实验表明当体系中的二价铁和三价铁被络合时,纳米铁还原水中的铀的反应速率明显降低,这表明反应体系中的二价铁和三价铁对还原水中的铀具有促进作用。此外,实验还证实吸附在纳米铁表面的二价铁能够快速还原水中的铀。根据实验的监测结果和固体-水界面化学理论,二价铁和三价铁在反应体系中的作用可以用下面的反应式表示：≡UO22++Fe→UO2+Fe2+ (3)≡UO22++2≡Fe2+→UO2+2Fe3+ (4) Fe3++Fe→2≡Fe2+ (5)首先吸附在纳米铁表面的铀将零价纳米铁氧化成二价铁(反应3),纳米铁表面的二价铁随后和铀反应生成三价铁(反应4),生成的三价铁和零价纳米铁反应生成二价铁(反应5),生成的二价铁再和铀反应生成三价铁(反应4),最后形成一个循环的氧化还原反应过程。
第五章研究了铀的还原产物及其可氧化性,监测了温度对反应的影响,还比较了实验合成和两种商业纳米铁的应用效果。X射线光电子能谱的实验结果表明六价铀已经被还原为四价,而零价纳米铁则被氧化为复杂的含二价和三价铁的(含水)氧化物,空气氧化实验表明厌氧条件下被纳米铁还原的铀可以被空气中的氧所氧化,但氧化速率要明显低于其还原速率；实验结果证实铀的去除和还原速率随着温度的升高而加快,并且水中碳酸根离子的存在,能加大温度对反应的影响,通过阿雷利乌斯公式和艾琳公式所计算出的反应的活化能(activation energy)、活化焓(enthalpy of activation)和活化熵(entropy of activation)的结果表明整个过程受表面反应控制而不是受扩散控制；三种纳米铁的对比实验研究表明,实验合成和经过表面钝化处理的纳米铁均能很好的去除和还原水中的铀,而镀碳的纳米铁的去除和还原铀的效果则相对较差。
第六章总结了前面的研究结果,并对今后进一步的研究方向进行了展望。
通过本论文的研究,主要获得了以下几个方面的成果：
1、纳米铁在厌氧条件下能够很快去除水中的铀,水中铀的去除由吸附和还原所引起,其反应过程是水中铀先吸附到纳米铁表面,随后被还原为四价铀；
2、水中的铀的去除和还原速率随着pH值的升高,碳酸根和钙离子浓度的增加而减慢,但与其它还原剂相比,这些抑制作用相对较弱；
3、二价和三价铁在纳米铁还原六价铀的过程中扮演着重要的角色,它们与零价铁一起形成一个氧化还原反应循环使得铀从六价还原为四价；
4、水温的升高能够加快纳米铁去除和还原水中的铀,并且水中碳酸根离子的存在加大了温度对反应的影响,相关的热力学参数表明整个过程受表面反应控制；
5、表面钝化技术既能保证纳米铁的环境稳定性,又不影响其使用效果；而表面镀碳技术则明显影响纳米铁的应用效果。
这些成果均表明纳米铁具有修复地下水中铀污染的潜力,但由于目前的研究尚处于实验室探索阶段,如需将其应用于野外修复实践中,还需进一步多角度多手段来研究纳米铁和铀的反应过程。
The extraction and processing of uranium for use in the nuclear weapons and in commercial nuclear energy production have led to extensive uranium contamination in the environment. This makes it imperative to understand the processes that affect the environmental mobility of uranium. The hexavalent oxidation state of uranium is mobile, and thus mostly susceptible to environmental transport and biological uptake. On the other hand, the reduced state uranium as U(IV) is sparely soluble, and hence its mobility, is limited. Since the mobility of uranium is largely determined by its valence, reduction-based technologies have been proposed to remediate the uranium contamination in the subsurface. Recently, nanoscale zerovalent iron (nano Fe0) particles have been proposed as a new generation of materials for environmental remediation. The material has been widely studied for the cleanup of organic contaminants such as TCE and PCBs. However, the potential application of nano Fe0 for uranium immobilization in the aquatic environment has not been well studied. The research described in this dissertation seeks to examine the kinetics and mechanism of the reactions between U(Ⅵ) and nano Fe0 in the subsurface setting.
The aqueous environmental geochemistry of uranium and the application of nano Fe0 for site remediation are briefly reviewed in Chapter 2.The research presented in Chapters 3 through 5 monitors the reaction kinetics between U(Ⅵ) and nano Fe0, investigates the roles of Fe(Ⅱ) and Fe(Ⅲ) in the U(Ⅵ) reduction reactions, examines the temperature effect, identifies the reaction products, evaluates the extent of U(Ⅳ) reoxidation, proposes the reaction scheme, and compares the efficiencies of three types of nano Fe0 on U(Ⅵ) removal and reduction. The research presented in this thesis collectively used several approaches including batch reactions, kinetics modeling and spectroscopic technique to investigate the interaction between nano Fe0 and uranium contaminant under anoxic conditions in order to identify the controlling factors and reaction pathways in the contaminated subsurface.
The results of this research reveal that bicarbonate and Ca have notable impacts on uranium removal and reduction through formation of binary uranyl-carbonato complexes and ternary uranyl-calcium-carbonato complexes, which stabilized U(VI) in aqueous phase and decreased both the rates of U(VI) removal and reduction. The observed variability of reaction rate constants in the presence of Fe(II)/Fe(III) complexing agents also indicate the roles of Fe(II) and Fe(III) in U(VI) reduction. Fe0, Fe(Ⅱ) and Fe(Ⅲ) can mediate electron cycling and thus catalyze the redox process. The XPS analysis confirms U(Ⅵ) is reduced to U(Ⅳ) by nano Fe0 under anoxic conditions, while the reduced U(Ⅳ) can be reoxidized by air. In addition, the temperature and iron types also affect the rates of U(Ⅵ) removal and reduction by nano Fe0 under anoxic conditions. This research clearly demonstrates that the reductive immobilization of U(Ⅵ) by nano Fe0 in the groundwater is closely linked to geochemical conditions controlling uranium speciation as well as the anaerobic/aerobic conditions and iron types.
In summary, the research presented in this dissertation evaluated and quantified the impacts of major controlling factors such as solution chemical components, temperature and iron types on uranium immobilization by nano Fe0. The study advanced our knowledge to use nano Fe0 for the remediation of uranium contamination in the complex subsurface environment.
本研究采用理论模拟和实验监测相结合的研究思路,利用批式实验和光谱分析的方法,系统研究了纳米铁去除和还原水中铀的主要影响因素,探讨了二价铁和三价铁在反应体系中的作用,研究了温度对反应的影响,利用X射线光电子能谱法鉴定了反应产物并研究了其可氧化性,最后比较了实验合成纳米铁和两种商业纳米铁的应用效果。通过对不同水化学条件下反应动力学数据的模拟和反应热力学参数的理论计算,对纳米铁还原固定水中的六价铀的反应机理进行了探讨。
本论文共分六章：
第一章简要介绍了问题的来源,研究的目的和意义,研究任务,以及论文的组织结构。
第二章共分三节：第一节介绍了铀的水环境地球化学特征,包括铀在水中存在的化学形态,水中铀的吸附,以及铀的化学还原和生物还原；第二节总结了纳米铁的特征和性质,然后回顾了其在环境修复中的应用,包括修复有机污染物和有毒重金属及放射性核素两个方面；第三节介绍了零价铁和铀反应的研究现状。
第三章详细研究了不同水化学条件下实验合成纳米铁去除和还原水中铀的反应动力学特征和反应机理。实验结果表明纳米铁能够快速去除水中的铀,水中铀的去除由吸附和还原所引起。研究证实铀的去除和还原速率随着pH值的升高而降低,水中的碳酸根和钙离子对纳米铁去除和还原水中铀具有明显的抑制作用,因为它们能与六价铀形成非常稳定的络合物。和其它还原剂(如普通铁粉、硫化氢、硫化铁和还原细菌)相比,纳米铁去除和还原水中铀的效果最好,并且水中碳酸根和钙离子的抑制作用相对较小。利用Scientist软件进行的反应动力学模拟结果表明,纳米铁还原水中铀分两步完成,即水中铀首先吸附到纳米铁的表面,随后六价铀被还原为四价。其反应过程如下：
第一步：(?)(吸附和解吸反应)
第二步(?)(还原反应)此外,X射线光电子能谱的实验结果(见第五章)也证实铀被还原为四价。
第四章采用螯合法研究了二价铁和三价铁在反应体系中的作用。两种铁的络合剂即1,10-邻菲罗琳(1,10-phenanthroline)和三乙醇胺(triethanolamine)分别用来络合反应体系中的二价铁和三价铁,实验表明当体系中的二价铁和三价铁被络合时,纳米铁还原水中的铀的反应速率明显降低,这表明反应体系中的二价铁和三价铁对还原水中的铀具有促进作用。此外,实验还证实吸附在纳米铁表面的二价铁能够快速还原水中的铀。根据实验的监测结果和固体-水界面化学理论,二价铁和三价铁在反应体系中的作用可以用下面的反应式表示：≡UO22++Fe→UO2+Fe2+ (3)≡UO22++2≡Fe2+→UO2+2Fe3+ (4) Fe3++Fe→2≡Fe2+ (5)首先吸附在纳米铁表面的铀将零价纳米铁氧化成二价铁(反应3),纳米铁表面的二价铁随后和铀反应生成三价铁(反应4),生成的三价铁和零价纳米铁反应生成二价铁(反应5),生成的二价铁再和铀反应生成三价铁(反应4),最后形成一个循环的氧化还原反应过程。
第五章研究了铀的还原产物及其可氧化性,监测了温度对反应的影响,还比较了实验合成和两种商业纳米铁的应用效果。X射线光电子能谱的实验结果表明六价铀已经被还原为四价,而零价纳米铁则被氧化为复杂的含二价和三价铁的(含水)氧化物,空气氧化实验表明厌氧条件下被纳米铁还原的铀可以被空气中的氧所氧化,但氧化速率要明显低于其还原速率；实验结果证实铀的去除和还原速率随着温度的升高而加快,并且水中碳酸根离子的存在,能加大温度对反应的影响,通过阿雷利乌斯公式和艾琳公式所计算出的反应的活化能(activation energy)、活化焓(enthalpy of activation)和活化熵(entropy of activation)的结果表明整个过程受表面反应控制而不是受扩散控制；三种纳米铁的对比实验研究表明,实验合成和经过表面钝化处理的纳米铁均能很好的去除和还原水中的铀,而镀碳的纳米铁的去除和还原铀的效果则相对较差。
第六章总结了前面的研究结果,并对今后进一步的研究方向进行了展望。
通过本论文的研究,主要获得了以下几个方面的成果：
1、纳米铁在厌氧条件下能够很快去除水中的铀,水中铀的去除由吸附和还原所引起,其反应过程是水中铀先吸附到纳米铁表面,随后被还原为四价铀；
2、水中的铀的去除和还原速率随着pH值的升高,碳酸根和钙离子浓度的增加而减慢,但与其它还原剂相比,这些抑制作用相对较弱；
3、二价和三价铁在纳米铁还原六价铀的过程中扮演着重要的角色,它们与零价铁一起形成一个氧化还原反应循环使得铀从六价还原为四价；
4、水温的升高能够加快纳米铁去除和还原水中的铀,并且水中碳酸根离子的存在加大了温度对反应的影响,相关的热力学参数表明整个过程受表面反应控制；
5、表面钝化技术既能保证纳米铁的环境稳定性,又不影响其使用效果；而表面镀碳技术则明显影响纳米铁的应用效果。
这些成果均表明纳米铁具有修复地下水中铀污染的潜力,但由于目前的研究尚处于实验室探索阶段,如需将其应用于野外修复实践中,还需进一步多角度多手段来研究纳米铁和铀的反应过程。
The extraction and processing of uranium for use in the nuclear weapons and in commercial nuclear energy production have led to extensive uranium contamination in the environment. This makes it imperative to understand the processes that affect the environmental mobility of uranium. The hexavalent oxidation state of uranium is mobile, and thus mostly susceptible to environmental transport and biological uptake. On the other hand, the reduced state uranium as U(IV) is sparely soluble, and hence its mobility, is limited. Since the mobility of uranium is largely determined by its valence, reduction-based technologies have been proposed to remediate the uranium contamination in the subsurface. Recently, nanoscale zerovalent iron (nano Fe0) particles have been proposed as a new generation of materials for environmental remediation. The material has been widely studied for the cleanup of organic contaminants such as TCE and PCBs. However, the potential application of nano Fe0 for uranium immobilization in the aquatic environment has not been well studied. The research described in this dissertation seeks to examine the kinetics and mechanism of the reactions between U(Ⅵ) and nano Fe0 in the subsurface setting.
The aqueous environmental geochemistry of uranium and the application of nano Fe0 for site remediation are briefly reviewed in Chapter 2.The research presented in Chapters 3 through 5 monitors the reaction kinetics between U(Ⅵ) and nano Fe0, investigates the roles of Fe(Ⅱ) and Fe(Ⅲ) in the U(Ⅵ) reduction reactions, examines the temperature effect, identifies the reaction products, evaluates the extent of U(Ⅳ) reoxidation, proposes the reaction scheme, and compares the efficiencies of three types of nano Fe0 on U(Ⅵ) removal and reduction. The research presented in this thesis collectively used several approaches including batch reactions, kinetics modeling and spectroscopic technique to investigate the interaction between nano Fe0 and uranium contaminant under anoxic conditions in order to identify the controlling factors and reaction pathways in the contaminated subsurface.
The results of this research reveal that bicarbonate and Ca have notable impacts on uranium removal and reduction through formation of binary uranyl-carbonato complexes and ternary uranyl-calcium-carbonato complexes, which stabilized U(VI) in aqueous phase and decreased both the rates of U(VI) removal and reduction. The observed variability of reaction rate constants in the presence of Fe(II)/Fe(III) complexing agents also indicate the roles of Fe(II) and Fe(III) in U(VI) reduction. Fe0, Fe(Ⅱ) and Fe(Ⅲ) can mediate electron cycling and thus catalyze the redox process. The XPS analysis confirms U(Ⅵ) is reduced to U(Ⅳ) by nano Fe0 under anoxic conditions, while the reduced U(Ⅳ) can be reoxidized by air. In addition, the temperature and iron types also affect the rates of U(Ⅵ) removal and reduction by nano Fe0 under anoxic conditions. This research clearly demonstrates that the reductive immobilization of U(Ⅵ) by nano Fe0 in the groundwater is closely linked to geochemical conditions controlling uranium speciation as well as the anaerobic/aerobic conditions and iron types.
In summary, the research presented in this dissertation evaluated and quantified the impacts of major controlling factors such as solution chemical components, temperature and iron types on uranium immobilization by nano Fe0. The study advanced our knowledge to use nano Fe0 for the remediation of uranium contamination in the complex subsurface environment.
引文
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