零价铁还原地下水中硝基芳香化合物的效能研究
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摘要
近年来,地下水中有机污染物的治理技术取得很大发展,已涵盖物理化学、微生物等学科领域。目前采用的主要方法有原位化学氧化、微生物曝气、井内曝气、多相抽提和渗透反应隔栅等技术。其中渗透反应隔栅技术由于其价格低廉,便于维护,在欧美等发达国家得到广泛应用,已经进入到实际工程阶段,但在我国该项技术却处于起步阶段。作为隔栅的填料介质,零价铁(Zero Valent Iron)具有价格低廉,易于获得,还原效果好等优点,日益受到广泛关注,展现出较为广阔的应用前景。本论文以商用还原铁粉为还原剂,系统地研究了其对硝基芳香化合物(NACs)的还原特性与机理,分析了还原反应动力学,特别针对我国东北地区地下水中铁、锰离子含量高的特点,讨论了水中铁、锰离子和溶解氧对还原的影响,为以零价铁为介质的渗透反应隔栅技术的实际应用奠定了理论基础。
采用比表面积为3.5697m2/g的商用铁粉,考察了其对硝基苯的还原特性与机理。通过紫外扫描和气质联机,对零价铁还原硝基苯的产物进行了分析,结果表明,还原产物主要为苯胺;对还原过程中总质量的守恒进行了计算,发现在还原过程中存在硝基苯的挥发和苯胺的吸附,并由此造成了质量损失;分别选取pH值为3,5,7,9,12,考查溶液中的pH值对还原反应的影响,检测了还原过程中pH值的变化,发现pH值越低,还原反应越容易发生,还原速率越快;pH值小于7时,随着反应的进行pH值逐渐升高,而pH大于7时,反应过程中pH值变化不明显。选取不同初始浓度(0.127~3.248mmol/L)的硝基苯溶液,考查了初始浓度对还原的影响。经假一级动力学方程对硝基苯还原过程进行拟和,表明在不同pH值和初始浓度下,硝基苯的还原过程都符合假一级动力学模型,其中不同pH值下,苯胺的生成过程符合零级反应。
考虑到我国东北地区地下水中铁、锰离子含量普遍较高,研究了溶液中的铁、锰离子对还原反应的影响。以硝基苯为污染物,向零价铁还原体系中加入不同浓度的Fe2+、Mn2+,通过气质联机分析还原过程,结果表明,Fe2+的加入可以提高反应速率,但是没有改变反应途径,而Mn2+对还原反应没有显著影响。Fe2+并不是作为反应的主要还原剂,它对反应体系具有缓冲作用。单纯的Fe(OH)2沉淀物对水中的硝基苯不具备还原能力,只有溶液中同时存在Fe2+时还原反应才能发生。溶液中的溶解氧减慢还原反应速率,造成溶液的pH值升高;但是加入Fe2+后,还原速率迅速提高,导致最终硝基苯的还原率只取决于溶液中Fe2+的量。采用X射线衍射和扫描电镜分析铁腐蚀产物,表明铁表面有纤铁矿(γ-FeOOH)生成;有Fe2+存在时,铁氧化物分层,氧化物内部主要成分是磁铁矿(Fe3O4); Fe2+的存在加速Fe0将纤铁矿还原为Fe3O4的反应速率。
分别选取硝基甲苯和硝基氯苯两大类6个单取代硝基苯,采用紫外全波段扫描和液相色谱,用内标物分析法分析了NACs的还原产物,各取代硝基苯均分别还原为相应的苯胺。对不同初始浓度的NACs进行还原试验研究,发现NACs的浓度随时间延长而不断降低,由其生成的相应的苯胺浓度不断增加,还原过程遵循假一级动力学模型。以4-Cl硝基苯为参考物质,比较了各个NACs的相对速率常数krel ,发现logKrel和其单电子还原电势Eh1’(X-NB)之间存在线性关系,而且邻位取代的化合物反应更快。该现象可以用取代芳烃的邻位效应解释。为比较不同NACs在Fe0表面上的竞争,以4-Cl硝基苯为参考物质,进行了二元混合试验。结果表明,竞争现象明显存在,通过定义竞争系数Qc来量化比较,Qc大小的排列顺序基本上与其Eh1’相关,而与其在溶液中的正辛醇/水分配系数logKow无关。
Many treatment technologies for groundwater pollution caused by organic compounds have been developed, including in situ chemical oxidation, biosparging, in-well aeration, multi-phase extraction, permeable reactive barriers (PRB), etc. The PRB technology has been applied widely to engineering in the developed countries because of its lower cost and convenience for management, however, it is studied primarily in China. As a type of reactive media of permeable barriers, zero-valent iron (ZVI) has been widely used due to its low cost, availability and excellent reductive efficiency. We used commercial reductive iron powder as reductant in this study, investigated systematically the reductive characteristics and mechanisms of nitroaromatic compounds (NACs) by Fe0 system, analyzed the kinetics of reductive reaction, in view of the higher content of ferrous and manganese ions in groundwater in the north-east of China, examined the effects of ferrous and manganese ions on reductive reaction. As is helpful for the application of PRB technology using Fe0 as media.
The specific surface area of commercial iron powder is 3.5697m2/g, the reductive characteristics of nitrobenzene by Fe0 was studied in this experiment. The reductive products of reaction were determined using UV scanning and GC/MS method. The experiment results showed that the major reductive product was aniline. The total mass balance of reductive process was calculated, an d it showed that there existed volatilization of nitrobenzene and adsorption of aniline during the reductive process, which resulted in the mass loss. The effects of pH on reduction were examined at different pH value of 3.0, 5.0, 7.0, 9.0, 12.0, respectively, and the change of pH value during the reaction was also determined. The results showed that lower pH value was favorable for the reductive reaction, and the higher reductive rate was obtained at lower pH value. The pH value of solution increased over time when the pH value was lower than 7.0, however, the variation of pH was not observed apparently when the pH value was higher than 7.0. The effects of initial nitrobenzene concentration on reduction were examined at different initial concentrations (0.127~3.248mmol/L). The reduction of nitrobenzene was fitted with pseudo-first-order kinetic model, and the results indicated that the reduction of nitrobenzene was well fitted to pseudo-first-order kinetic model at different pH values and initial concentrations. The formation of aniline followed zero order reaction at different pH values.
The effects of ferrous and manganese ions on reduction were firstly studied in this paper. Nitrobenzene was selected as the pollutant, and the Fe2+ and Mn2+ ions of different concentrations were added into the Fe0 system. According to the GC/MS results, the reactive rate was enhanced due to the addition of Fe2+ ions, however, the reactive pathway was not changed, and there existed no significant influence on the reduction of nitrobenzene due to the addition of Mn2+ ions. Fe2+ ions were not the main reductant, and it had a buffering capacity in the Fe0 system. The reduction of nitrobenzene caused by ferrous hydroxide deposits was examined, the results showed that the reductive reaction only occurred when the Fe2+ ions coexisted with Fe(OH)2. The effects of dissolved oxygen (DO) on reduction were also examined, the results showed that the presence of DO in solution lowered the reactive rate, resulting in the increase of pH value. However, the reductive rate of nitrobenzene was increased after the addition of Fe2+ ions, the final reductive ratio of nitrobenzene depended on the amount of Fe2+ ions in solution. The corrosive products were determined using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods, the results showed that lepidocrocite was formed on the surface of iron powder, and the iron corrosion coating had a stratified structure under the presence of Fe2+ ions, the inner layer mainly consisted of magnetite with negligible lepidocrocite. The addition of Fe2+ ions accelerated the reductive rate of lepidocrocite to Fe3O4 by Fe0.
Six monosubstituted nitrobenzenes (NBs) were selected, according to a method based on all band ultraviolet scanning and HPLC, the reductive products of NACs were determined using internal standard gas chromatography, the results indicated that the reductive products of each monosubstituted NB were the corresponding aniline. The reduction of NACs was examined at different initial concentrations, the results showed that the NACs concentration decreased over time and the corresponding concentration of reductive products aniline increased over time, the reduction process was well fitted with pseudo-first-order kinetic model. The relative rate constant krel of each NAC was compared in the reference of 4-ClNB, the results showed that there existed a linear relationship between logKrel and Eh1’(X-NB), and the reactive rate of o-substituted compounds was the fastest, which could be explained by o-substituted effect. The competition experiments with binary mixtures of 4-ClNB and each one of the other NACs were performed, the results showed that there existed apparent competition, and the competition was quantitatively compared by definition of competition coefficient Qc. The order of Qc correlated well with its Eh1’, and there existed no correlation with logKow.
采用比表面积为3.5697m2/g的商用铁粉,考察了其对硝基苯的还原特性与机理。通过紫外扫描和气质联机,对零价铁还原硝基苯的产物进行了分析,结果表明,还原产物主要为苯胺;对还原过程中总质量的守恒进行了计算,发现在还原过程中存在硝基苯的挥发和苯胺的吸附,并由此造成了质量损失;分别选取pH值为3,5,7,9,12,考查溶液中的pH值对还原反应的影响,检测了还原过程中pH值的变化,发现pH值越低,还原反应越容易发生,还原速率越快;pH值小于7时,随着反应的进行pH值逐渐升高,而pH大于7时,反应过程中pH值变化不明显。选取不同初始浓度(0.127~3.248mmol/L)的硝基苯溶液,考查了初始浓度对还原的影响。经假一级动力学方程对硝基苯还原过程进行拟和,表明在不同pH值和初始浓度下,硝基苯的还原过程都符合假一级动力学模型,其中不同pH值下,苯胺的生成过程符合零级反应。
考虑到我国东北地区地下水中铁、锰离子含量普遍较高,研究了溶液中的铁、锰离子对还原反应的影响。以硝基苯为污染物,向零价铁还原体系中加入不同浓度的Fe2+、Mn2+,通过气质联机分析还原过程,结果表明,Fe2+的加入可以提高反应速率,但是没有改变反应途径,而Mn2+对还原反应没有显著影响。Fe2+并不是作为反应的主要还原剂,它对反应体系具有缓冲作用。单纯的Fe(OH)2沉淀物对水中的硝基苯不具备还原能力,只有溶液中同时存在Fe2+时还原反应才能发生。溶液中的溶解氧减慢还原反应速率,造成溶液的pH值升高;但是加入Fe2+后,还原速率迅速提高,导致最终硝基苯的还原率只取决于溶液中Fe2+的量。采用X射线衍射和扫描电镜分析铁腐蚀产物,表明铁表面有纤铁矿(γ-FeOOH)生成;有Fe2+存在时,铁氧化物分层,氧化物内部主要成分是磁铁矿(Fe3O4); Fe2+的存在加速Fe0将纤铁矿还原为Fe3O4的反应速率。
分别选取硝基甲苯和硝基氯苯两大类6个单取代硝基苯,采用紫外全波段扫描和液相色谱,用内标物分析法分析了NACs的还原产物,各取代硝基苯均分别还原为相应的苯胺。对不同初始浓度的NACs进行还原试验研究,发现NACs的浓度随时间延长而不断降低,由其生成的相应的苯胺浓度不断增加,还原过程遵循假一级动力学模型。以4-Cl硝基苯为参考物质,比较了各个NACs的相对速率常数krel ,发现logKrel和其单电子还原电势Eh1’(X-NB)之间存在线性关系,而且邻位取代的化合物反应更快。该现象可以用取代芳烃的邻位效应解释。为比较不同NACs在Fe0表面上的竞争,以4-Cl硝基苯为参考物质,进行了二元混合试验。结果表明,竞争现象明显存在,通过定义竞争系数Qc来量化比较,Qc大小的排列顺序基本上与其Eh1’相关,而与其在溶液中的正辛醇/水分配系数logKow无关。
Many treatment technologies for groundwater pollution caused by organic compounds have been developed, including in situ chemical oxidation, biosparging, in-well aeration, multi-phase extraction, permeable reactive barriers (PRB), etc. The PRB technology has been applied widely to engineering in the developed countries because of its lower cost and convenience for management, however, it is studied primarily in China. As a type of reactive media of permeable barriers, zero-valent iron (ZVI) has been widely used due to its low cost, availability and excellent reductive efficiency. We used commercial reductive iron powder as reductant in this study, investigated systematically the reductive characteristics and mechanisms of nitroaromatic compounds (NACs) by Fe0 system, analyzed the kinetics of reductive reaction, in view of the higher content of ferrous and manganese ions in groundwater in the north-east of China, examined the effects of ferrous and manganese ions on reductive reaction. As is helpful for the application of PRB technology using Fe0 as media.
The specific surface area of commercial iron powder is 3.5697m2/g, the reductive characteristics of nitrobenzene by Fe0 was studied in this experiment. The reductive products of reaction were determined using UV scanning and GC/MS method. The experiment results showed that the major reductive product was aniline. The total mass balance of reductive process was calculated, an d it showed that there existed volatilization of nitrobenzene and adsorption of aniline during the reductive process, which resulted in the mass loss. The effects of pH on reduction were examined at different pH value of 3.0, 5.0, 7.0, 9.0, 12.0, respectively, and the change of pH value during the reaction was also determined. The results showed that lower pH value was favorable for the reductive reaction, and the higher reductive rate was obtained at lower pH value. The pH value of solution increased over time when the pH value was lower than 7.0, however, the variation of pH was not observed apparently when the pH value was higher than 7.0. The effects of initial nitrobenzene concentration on reduction were examined at different initial concentrations (0.127~3.248mmol/L). The reduction of nitrobenzene was fitted with pseudo-first-order kinetic model, and the results indicated that the reduction of nitrobenzene was well fitted to pseudo-first-order kinetic model at different pH values and initial concentrations. The formation of aniline followed zero order reaction at different pH values.
The effects of ferrous and manganese ions on reduction were firstly studied in this paper. Nitrobenzene was selected as the pollutant, and the Fe2+ and Mn2+ ions of different concentrations were added into the Fe0 system. According to the GC/MS results, the reactive rate was enhanced due to the addition of Fe2+ ions, however, the reactive pathway was not changed, and there existed no significant influence on the reduction of nitrobenzene due to the addition of Mn2+ ions. Fe2+ ions were not the main reductant, and it had a buffering capacity in the Fe0 system. The reduction of nitrobenzene caused by ferrous hydroxide deposits was examined, the results showed that the reductive reaction only occurred when the Fe2+ ions coexisted with Fe(OH)2. The effects of dissolved oxygen (DO) on reduction were also examined, the results showed that the presence of DO in solution lowered the reactive rate, resulting in the increase of pH value. However, the reductive rate of nitrobenzene was increased after the addition of Fe2+ ions, the final reductive ratio of nitrobenzene depended on the amount of Fe2+ ions in solution. The corrosive products were determined using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods, the results showed that lepidocrocite was formed on the surface of iron powder, and the iron corrosion coating had a stratified structure under the presence of Fe2+ ions, the inner layer mainly consisted of magnetite with negligible lepidocrocite. The addition of Fe2+ ions accelerated the reductive rate of lepidocrocite to Fe3O4 by Fe0.
Six monosubstituted nitrobenzenes (NBs) were selected, according to a method based on all band ultraviolet scanning and HPLC, the reductive products of NACs were determined using internal standard gas chromatography, the results indicated that the reductive products of each monosubstituted NB were the corresponding aniline. The reduction of NACs was examined at different initial concentrations, the results showed that the NACs concentration decreased over time and the corresponding concentration of reductive products aniline increased over time, the reduction process was well fitted with pseudo-first-order kinetic model. The relative rate constant krel of each NAC was compared in the reference of 4-ClNB, the results showed that there existed a linear relationship between logKrel and Eh1’(X-NB), and the reactive rate of o-substituted compounds was the fastest, which could be explained by o-substituted effect. The competition experiments with binary mixtures of 4-ClNB and each one of the other NACs were performed, the results showed that there existed apparent competition, and the competition was quantitatively compared by definition of competition coefficient Qc. The order of Qc correlated well with its Eh1’, and there existed no correlation with logKow.
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