包覆型纳米铁的制备及用于地下水污染修复的实验研究
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摘要
近年来,随着三氯乙烯(TCE)等卤代烃类污染物在环境中,尤其是在地下水中的不断积累,水体的卤代烃类污染已经成为了非常严重的环境问题。地下水的卤代烃污染修复也已成为全球环境污染修复的重要内容。
纳米技术的发展给污染物的处理带来了一种颇具潜力的新方法,其中纳米铁材料具有粒径小,比表面积大,表面活性高,还原能力强等特点,能够有效去除有机物、重金属和硝酸盐等多种污染物,已越来越多的被应用于土壤和地下水污染修复的研究。
但是,目前纳米铁在地下水环境修复中的应用尚存在一些问题。高活性的纳米铁暴露在空气中会发生自燃,当缓慢接触空气时会被氧化,在其表面生成氧化铁膜而损失其表面活性。在液相中处理疏水性有机物时,由于纳米铁极性与其不同,两者难于接触而使反应速率低。这些因素使得纳米铁在实际应用中受到了很大的限制。
本论文针对这些问题,结合国家自然科学基金“乳化炭载纳米铁原位修复地下水中有机氯代烃”的部分内容,制备了表面包覆型纳米铁材料,研究了包覆型纳米铁在空气中的稳定性;并考察了其对TCE的还原脱氯性能;探讨了脱氯反应的动力学和反应机理。论文的主要研究内容和结果有:
1.用乳液聚合法制备了聚甲基丙烯酸甲酯(PMMA)包覆型纳米铁材料,发现经过包覆的纳米铁表面亲油性和抗氧化性均有所提高,接触空气未发生自燃,但于空气中放置一周后仍发生了明显氧化。将纳米材料制备与微乳聚合相结合,开发出一种新型的微乳原位聚合法制备包覆型纳米铁,该方法可将纳米粒子的生成、粒径控制、抗团聚、抗氧化保护在一个体系中一次性实现,在生成的纳米粒子外层形成稳定的PMMA包覆层。用这种新型微乳液原位聚合法制备的包覆型纳米铁的抗氧化性更强,能够在空气中放置两周不被氧化。
2.用微乳液原位聚合法制备的包覆型纳米铁进行了TCE降解实验。探讨了溶液初始pH,纳米铁投加剂量,TCE初始浓度,溶解氧等因素对反应的影响。包覆型纳米铁在反应中同时发挥吸附和还原降解的作用,吸附在包覆型纳米铁表面的TCE分子溶胀、穿透PMMA包覆层到达铁表面与其发生反应,但由于包覆层的存在,这种材料的降解速率比未包覆的材料有所降低。
溶液初始pH越低,TCE去除速率越大;振荡速度的提高可加快传质过程,提高反应速率;溶液中纳米铁剂量的增加可以加快反应的进行;TCE初始浓度的越大,TCE的去除速率越慢;反应体系中有溶解氧存在时,溶解氧作为电子受体与TCE进行竞争消耗纳米铁,减慢反应速率;共存离子的存在会降低铁还原TCE的能力;周期实验显示,反应中生成的铁氧化物和氢氧化物沉积在铁的表面,逐渐将有活性的零价铁包覆,使其还原性能逐渐减弱。
柱实验研究表明,TCE溶液流速越慢,与填充铁的接触时间越长,接触越充分,柱的去除率越高。
3.研究了微乳原位聚合包覆型纳米铁去除TCE的反应动力学,探讨了其对TCE的脱氯还原机理。
通过线性回归验证纳米铁对TCE的还原脱氯较好的符合准一级反应动力学模型。分析了包覆型纳米铁与TCE反应的固-液相反应动力学模型,证明化学还原是控制该反应速率的最主要步骤。
在包覆型纳米材料还原TCE的过程中,纳米铁是主要的还原剂,纳米铁表面的电子直接转移到吸附在铁表面的氯代烃上发生还原性脱氯。还原性脱氯反应中氯原子与碳原子断开的方式是序贯氢解作用和β消去作用,其中以氢解作用为主。在TCE的去除过程中,还原脱氯占主要部分。无氧环境下包覆型纳米铁在溶液中对TCE进行还原后的最终腐蚀产物为Fe3O4。
In recent years, halogenated hydrocarbons, including chlorinated hydrocarbons such as trichloroethylene(TCE), have been accumulating in the environment, particularly in groundwaters. As a result, pollution of water by halogenated hydrocarbons has become an important environmental problem. Contaminated groundwaters represent a large portion of environmental remedial action plans throughout the world.
Due to their small particle size and high reactivity, the nanoscale zero valent iron (nZVI) has increasingly been utilized in the remediation of soils and groundwater.
nZVI has been proved to be one of the latest innovative technologies for environmental remediation. Laboratory studies have demonstrated that nZVI can effectively transform a wide array of environmental contaminants including chlorinated organic compounds, toxic metals, and nitrate. The use of nZVI in the reaction affords little environmental threat. Thus, it is desirable to be able to efficiently dechlorinate groundwater contaminates using nZVI.
However, Fe nanoparticles were easily oxidized, e.g. by air, and thereby significantly lost their main advantage of a very high surface reactivity. Freshly synthesized iron nanoparticles often ignited spontaneously upon exposure to air. When slowly exposed to air, a coating of iron oxide was formed on the surface of particles. Furthermore, it was hard for nanoiron to touch TCE in solution. The characters of this material have been serious drawbacks in practical application.
To overcome these drawbacks, the study aims to: (1) synthesize polymer coated nanoiron particles and assess their air stability; (2) research the removal efficiency of TCE by polymer coated nanoiron particles; and (3) study the kinetic and mechanisms of the TCE removal by the synthesized polymer coated nanoiron particles. The research work is a part of the project named“The In-situ Remediation of Chlorinated Hydrocarbons in Groundwater with Supported Nanoscale Iron Emulsion”, which is funded by the National Natural Science Foundation of China (NNSFC).
There were three main parts in our study:
1. nanoscale iron particles were entrapped successfully in poly(methyl methacrylate) (PMMA) by emulsion polymerization. It was found that the freshly synthesized polymer coated nanoiron particles did not ignite spontaneously when they were rapidly exposed to air. However, upon subsequent exposure in air for one week, a coating of iron oxide was formed on the surface of particles. And then, we synthesize PMMA coated nanoiron particles via a modified in-situ inverse microemulsion polymerization. The remarkable characteristic of nanoparticles in-situ synthesizing is which can synchronously bring to success in a single system for the growth of particles, granularity control, agglomeration control, high degree dispersion and long lasting stability. In this study, the polymer coated nanoiron particles produced by microemulsion polymerization have been shown to be more stable in air.
2. The polymer coated nanoiron particles were used for TCE removal from aqueous solution. The effects of some factors were discussed, such as initial pH, dispersion intensity, nanoiron particles content, initial concentration of TCE, dissolved oxygen and so on.
The batch studies showed that the reaction between the polymer coated nanoiron particles and TCE was composed of two processes: (a) TCE molecules was adsorped on the surface of particles; (b) Adsorped TCE molecules moved through the polymer membranes and participate in the redox reaction. The reaction of TCE removal by nanoiron particles was fater than that by polymer coated nanoiron particles.
The TCE removal rate was strongly dependent on intensity of dispersion. Great intensity would accelerate the reaction when a rotary shaker was used. The greater the polymer coated nanoiron particles content was, the greater the reaction rate would be. Under the same content of polymer coated nanoiron particles, reaction rate would decrease with the increase of the pH and the initial nitrate concentration. Dissolved oxygen would retard the reduction of TCE by consuming electrons released from iron. The co-exist ion could weaken the dechlorination efficiency of polymer coated nanoiron particles. The generation of OH- in the reaction would cause the precipitation of Fe2+ during the experiment.
The column studies indicated that the greater the dechlorination efficiency was, the longer the contact time in column was.
3. The kinetics and mechanisms of TCE removal by the synthesized polymer coated nanoiron particles investigated.
In this study, the experimental data could be fit to pseudo first-order kinetic model. In the solid-liquid interface reaction between polymer coated nanoiron particles and TCE, the main factors that control the reaction rate was the chemical reduction. The nanoiron is the main reducing agent in the reaction. The possible reaction pathways for TCE reduction by nanoiron were hydrogenolys and reductiveβelimination, but the hydrogenolysis was the main reaction pathway for TCE. The polymer membranes appeared to have no obvious impact on the final efficiency and products of the denitrification. In anaerobic system, Fe3O4 was the final iron corrosion product.
纳米技术的发展给污染物的处理带来了一种颇具潜力的新方法,其中纳米铁材料具有粒径小,比表面积大,表面活性高,还原能力强等特点,能够有效去除有机物、重金属和硝酸盐等多种污染物,已越来越多的被应用于土壤和地下水污染修复的研究。
但是,目前纳米铁在地下水环境修复中的应用尚存在一些问题。高活性的纳米铁暴露在空气中会发生自燃,当缓慢接触空气时会被氧化,在其表面生成氧化铁膜而损失其表面活性。在液相中处理疏水性有机物时,由于纳米铁极性与其不同,两者难于接触而使反应速率低。这些因素使得纳米铁在实际应用中受到了很大的限制。
本论文针对这些问题,结合国家自然科学基金“乳化炭载纳米铁原位修复地下水中有机氯代烃”的部分内容,制备了表面包覆型纳米铁材料,研究了包覆型纳米铁在空气中的稳定性;并考察了其对TCE的还原脱氯性能;探讨了脱氯反应的动力学和反应机理。论文的主要研究内容和结果有:
1.用乳液聚合法制备了聚甲基丙烯酸甲酯(PMMA)包覆型纳米铁材料,发现经过包覆的纳米铁表面亲油性和抗氧化性均有所提高,接触空气未发生自燃,但于空气中放置一周后仍发生了明显氧化。将纳米材料制备与微乳聚合相结合,开发出一种新型的微乳原位聚合法制备包覆型纳米铁,该方法可将纳米粒子的生成、粒径控制、抗团聚、抗氧化保护在一个体系中一次性实现,在生成的纳米粒子外层形成稳定的PMMA包覆层。用这种新型微乳液原位聚合法制备的包覆型纳米铁的抗氧化性更强,能够在空气中放置两周不被氧化。
2.用微乳液原位聚合法制备的包覆型纳米铁进行了TCE降解实验。探讨了溶液初始pH,纳米铁投加剂量,TCE初始浓度,溶解氧等因素对反应的影响。包覆型纳米铁在反应中同时发挥吸附和还原降解的作用,吸附在包覆型纳米铁表面的TCE分子溶胀、穿透PMMA包覆层到达铁表面与其发生反应,但由于包覆层的存在,这种材料的降解速率比未包覆的材料有所降低。
溶液初始pH越低,TCE去除速率越大;振荡速度的提高可加快传质过程,提高反应速率;溶液中纳米铁剂量的增加可以加快反应的进行;TCE初始浓度的越大,TCE的去除速率越慢;反应体系中有溶解氧存在时,溶解氧作为电子受体与TCE进行竞争消耗纳米铁,减慢反应速率;共存离子的存在会降低铁还原TCE的能力;周期实验显示,反应中生成的铁氧化物和氢氧化物沉积在铁的表面,逐渐将有活性的零价铁包覆,使其还原性能逐渐减弱。
柱实验研究表明,TCE溶液流速越慢,与填充铁的接触时间越长,接触越充分,柱的去除率越高。
3.研究了微乳原位聚合包覆型纳米铁去除TCE的反应动力学,探讨了其对TCE的脱氯还原机理。
通过线性回归验证纳米铁对TCE的还原脱氯较好的符合准一级反应动力学模型。分析了包覆型纳米铁与TCE反应的固-液相反应动力学模型,证明化学还原是控制该反应速率的最主要步骤。
在包覆型纳米材料还原TCE的过程中,纳米铁是主要的还原剂,纳米铁表面的电子直接转移到吸附在铁表面的氯代烃上发生还原性脱氯。还原性脱氯反应中氯原子与碳原子断开的方式是序贯氢解作用和β消去作用,其中以氢解作用为主。在TCE的去除过程中,还原脱氯占主要部分。无氧环境下包覆型纳米铁在溶液中对TCE进行还原后的最终腐蚀产物为Fe3O4。
In recent years, halogenated hydrocarbons, including chlorinated hydrocarbons such as trichloroethylene(TCE), have been accumulating in the environment, particularly in groundwaters. As a result, pollution of water by halogenated hydrocarbons has become an important environmental problem. Contaminated groundwaters represent a large portion of environmental remedial action plans throughout the world.
Due to their small particle size and high reactivity, the nanoscale zero valent iron (nZVI) has increasingly been utilized in the remediation of soils and groundwater.
nZVI has been proved to be one of the latest innovative technologies for environmental remediation. Laboratory studies have demonstrated that nZVI can effectively transform a wide array of environmental contaminants including chlorinated organic compounds, toxic metals, and nitrate. The use of nZVI in the reaction affords little environmental threat. Thus, it is desirable to be able to efficiently dechlorinate groundwater contaminates using nZVI.
However, Fe nanoparticles were easily oxidized, e.g. by air, and thereby significantly lost their main advantage of a very high surface reactivity. Freshly synthesized iron nanoparticles often ignited spontaneously upon exposure to air. When slowly exposed to air, a coating of iron oxide was formed on the surface of particles. Furthermore, it was hard for nanoiron to touch TCE in solution. The characters of this material have been serious drawbacks in practical application.
To overcome these drawbacks, the study aims to: (1) synthesize polymer coated nanoiron particles and assess their air stability; (2) research the removal efficiency of TCE by polymer coated nanoiron particles; and (3) study the kinetic and mechanisms of the TCE removal by the synthesized polymer coated nanoiron particles. The research work is a part of the project named“The In-situ Remediation of Chlorinated Hydrocarbons in Groundwater with Supported Nanoscale Iron Emulsion”, which is funded by the National Natural Science Foundation of China (NNSFC).
There were three main parts in our study:
1. nanoscale iron particles were entrapped successfully in poly(methyl methacrylate) (PMMA) by emulsion polymerization. It was found that the freshly synthesized polymer coated nanoiron particles did not ignite spontaneously when they were rapidly exposed to air. However, upon subsequent exposure in air for one week, a coating of iron oxide was formed on the surface of particles. And then, we synthesize PMMA coated nanoiron particles via a modified in-situ inverse microemulsion polymerization. The remarkable characteristic of nanoparticles in-situ synthesizing is which can synchronously bring to success in a single system for the growth of particles, granularity control, agglomeration control, high degree dispersion and long lasting stability. In this study, the polymer coated nanoiron particles produced by microemulsion polymerization have been shown to be more stable in air.
2. The polymer coated nanoiron particles were used for TCE removal from aqueous solution. The effects of some factors were discussed, such as initial pH, dispersion intensity, nanoiron particles content, initial concentration of TCE, dissolved oxygen and so on.
The batch studies showed that the reaction between the polymer coated nanoiron particles and TCE was composed of two processes: (a) TCE molecules was adsorped on the surface of particles; (b) Adsorped TCE molecules moved through the polymer membranes and participate in the redox reaction. The reaction of TCE removal by nanoiron particles was fater than that by polymer coated nanoiron particles.
The TCE removal rate was strongly dependent on intensity of dispersion. Great intensity would accelerate the reaction when a rotary shaker was used. The greater the polymer coated nanoiron particles content was, the greater the reaction rate would be. Under the same content of polymer coated nanoiron particles, reaction rate would decrease with the increase of the pH and the initial nitrate concentration. Dissolved oxygen would retard the reduction of TCE by consuming electrons released from iron. The co-exist ion could weaken the dechlorination efficiency of polymer coated nanoiron particles. The generation of OH- in the reaction would cause the precipitation of Fe2+ during the experiment.
The column studies indicated that the greater the dechlorination efficiency was, the longer the contact time in column was.
3. The kinetics and mechanisms of TCE removal by the synthesized polymer coated nanoiron particles investigated.
In this study, the experimental data could be fit to pseudo first-order kinetic model. In the solid-liquid interface reaction between polymer coated nanoiron particles and TCE, the main factors that control the reaction rate was the chemical reduction. The nanoiron is the main reducing agent in the reaction. The possible reaction pathways for TCE reduction by nanoiron were hydrogenolys and reductiveβelimination, but the hydrogenolysis was the main reaction pathway for TCE. The polymer membranes appeared to have no obvious impact on the final efficiency and products of the denitrification. In anaerobic system, Fe3O4 was the final iron corrosion product.
引文
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