纳米铁系金属复合材料去除地下水中硝酸盐污染的研究
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摘要
近年来随工农业的快速发展,地下水中硝酸盐的污染已成为一个相当重要的环境问题,且污染具有日益恶化的趋势,目前已引起人们的普遍关注。结合纳米技术对环境污染进行修复是当今世界一个新的发展方向。纳米材料具有粒径小,比表面积大以及表面活性高等特点,并可直接注入地下对污染区域实现原位修复,因此合成新型高效的纳米材料去除地下水中硝酸盐污染已成为环境中的一个研究热点课题。
目前应用于地下水中硝酸盐去除的技术主要有生物反硝化、离子交换技术、膜分离法和化学还原修复等技术;其中生物处理法具有高效低耗的特点,但会导致出水中含有细菌和残留有机物,必须进行后续处理;离子交换和膜分离等物理化学处理技术只是将硝酸盐污染物进行了浓缩或转移,并没有对其进行彻底去除,同时产生高浓度再生废液同样需要处理;而在化学还原反硝化中,应用负载型催化剂可将大部分硝酸盐转化为N2,但催化还原过程中需要以H2作为还原剂,而H2容易爆炸,不便于工程施用;纳米Fe0可快速还原地下水中的硝酸盐,但其产物主要为NH4+-N,只有很小部分硝酸盐可能被转化为N2。
针对以上问题,本文采用液相还原法制备了纳米级Fe/Ni、Fe/Cu、Fe/Pd和Fe/Pd/Cu金属复合材料,并首次将纳米Fe/Ni和纳米Fe/Pd/Cu颗粒应用于地下水中硝酸盐污染物的去除,采用TEM-EDS、SEM、XRD、BET等分析手段对纳米材料的结构、组成进行了表征,系统的研究了不同催化剂金属对硝酸盐还原中间产物和最终产物的影响,同时对纳米颗粒还原NO3-的反应机理进行了探讨。与普通铁屑相比,纳米Fe0具有很高的反应活性,金属催化剂Ni、Cu、Pd的引入进一步提高了NO3-的去除速率,且不同催化剂种类对还原速率及还原产物具有不同的影响。
对比普通铁屑与纳米零价铁去除NO3-的反应,溶液pH是影响铁屑反应速率的主要影响因素,酸性条件有利于铁屑还原去除NO3-,而纳米Fe0即使在中性初始pH条件下也具有较高的反应活性;将铁屑与纳米Fe0分别应用于地浸采铀实际地下水,普通铁屑反应5 h,硝酸盐去除率为93% ,而纳米Fe0 15分钟即可将硝酸盐污染物完全去除,但约96%的NO3-被转化为NH4+-N。
在纳米Fe/Ni去除硝酸盐的研究中,当Ni负载量为5.0%时,且在中性pH条件下,纳米颗粒具有最高的反应活性;新鲜制备的Fe/Ni纳米双金属颗粒,在空气中缓慢氧化22h后可稳定存在于空气中,但其反应活性降为原来的十分之一,与纳米Fe0反应活性相当,继续老化44 h对纳米Fe/Ni的反应活性影响不大;反应中有少量NO2-作为中间副产物被检出,但最终与NO3-一起被同时去除,NH4+转化率在84.6%~90.6%范围内,改变Ni负载量、溶液初始pH值、初始浓度等实验条件对改善产物选择性的贡献很小;认为硝酸盐的脱硝反应经历了NO3-→NO2-→NH4+两个转化步骤,为连续分步反应,其中NO3-→NO2-为整个反应的速度控制步骤。
以Cu为催化剂催化还原硝酸盐,当Cu负载量为5.0%时,纳米Fe/Cu与硝酸盐反应具有最快的去除速率,30min可将硝酸盐完全去除;反应过程中有30%的NO3-可被还原为中间副产物NO2-,提高nano-Fe/Cu的反应活性,有利于NO2-在溶液中的积累,但NO2-可进一步被转化为NH4+或N2,NH4+最终转化率为79.4%~82.8%;纳米Fe/Cu复合材料还原NO3-的反应历程与纳米Fe/Ni相似,为连续分步反应,与nano-Fe/Ni反应体系不同的是,金属Cu催化剂对NO2-具有较高的选择性, NO3-→NO2-转化速率较快,而NO2-→NH4+的转化速率较慢。
本文同时合成了纳米Fe/Pd以及纳米Fe/Pd/Cu复合材料,并对其催化还原硝酸盐的反应进行了初步探讨。实验结果表明,以Fe0为还原剂,分别以Ni、Cu、Pd不同金属为催化剂去除地下水中的硝酸盐,具有不同的还原效果,其中纳米Fe/Cu反应体系的反应活性最高,对中间产物NO2-的选择性最大,且对NH4+具有较小的选择性,在硝酸盐污染物的环境修复中具有很好的发展前景。
Recently, with the development of industry and agriculture, nitrate pollution in ground water has been an importantly environmental problem and with the tendency of gradually deterioration. Nowadays, it has been prevalently considered by people. Using nanotechnology to remediate environmental pollution is a new direction of environmental remediation in the world. Nanoscale materials have the characteristic of small diameter, high specific surface area to mass ratios and great surface reactivity. In addition, nanoparticles could be injected directly to contaminated field and realize in situ remediation of ground water. So synthesizing new and high efficiency nanoscale materials to reduce nitrate has become the focus of water research.
Technologies applied to remove nitrate in ground water include biological denitrification, ion exchange, membrane separation and chemical reduction. Nitrate removal with biological approach may obtain high efficiency and low cost, but it may lead to the existence of bacteria and organic compounds in water, it request further treatment. For physico-chemical approaches, nitrate is only shift to another form, and not removed completely, on the other hand, it may bring large volumes of waste solution with high concentration which also needs to be treated. Application of loading catalyst could transform mostly nitrate to N2, but during the catalytic process, H2 is used as reductant which is easy to blast and difficult to construction. Nitrate could be rapidly reduced by nanoscale Fe0 particles, but the main product is NH4+-N, only a little nitrate may be transformed to N2.
To overcome these drawbacks, liquid-phase synthesized method was applied to prepare nanoscale Fe/Ni、Fe/Cu、Fe/Pd and Fe/Pd/Cu compound materials. In the nanoscale materials, nano-Fe/Ni and nano-Fe/Pd/Cu particles were firstly used to reduce nitrate contamination in groundwater. Nanoparticles were characterized by TEM-EDS, SEM, XRD and BET techniques. Nitrate reduction with different nanoscale materials was investigated systemically. At the same time, the reduction mechanism with nanoparticle was discussed in our work. Nanosized Fe0 behaved high reactivity during the denitrification of nitrate compared with common iron powder. The introduction of Ni, Cu and Pd further enhance the removal rate, and different catalyst makes differently degree effects on reduction rate and product.
For iron powder, solution pH is an important parameter influencing nitrate reduction and low pH is favorable for the denitrification of nitrate. Different from iron powder, nanosized Fe0 performed large reaction rate even under the condition of neutral solution pH. Using iron powder and nano-Fe0 to treat in-situ uranium leaching groundwater, under laboratory conditions, nitrate removal rate was 93% in 5 h by iron powder but nitrate was removed completely by nanosized Fe0 within 15 min. About 96% nitrate was reduced to NH4+-N.
In nano-Fe/Ni reaction system, when Ni loading was 5.0%, nanoparticles showed the highest reactivity under neutral initial solution pH. After slowly ageing 22 h, the reactivity of freshly prepared nanoscale Fe/Ni particles decreased about 10 times, but with the followed 44 h ageing, little decreasing of reactivity was observed which is equivalent to freshly synthesized nano-Fe0. Nitrite was detected as the intermediate product during the reduce process and disappeared companied with nitrate vanishing. NH4+-N transformation rate was at the range of 84.6%~90.6%. Little improve of selectivity to N2 was obtained through changing Ni contents, initial solution pH and nitrate concentration et al. experimental conditions. According to the analysis of product, it was considered that nitrate reduction by Ni/Fe nanoparticles undergo two steps: (1) NO3- was reduced to NO2- with the tendency of increasing at first and disappeared from solution at last; (2) NO2- was then reduced to NH4+. The first transformation process was the control step.
Using Cu as catalyst catalytic reduce nitrate contaminant, when Cu content was 5.0% nano-Fe/Cu bimetallic particles showed the rapidest removal rate, and nitrate was removed entirely within 30 min. During the process of nitrate reduction, about 30% nitrate was transformed to intermediate product NO2-. Increasing the reactivity of nanoscale Fe/Cu particles was favorable to the accumulation of NO2- in the solution. At the end of reaction, NO2- was reduced to NH4- N or N2 and NH4- N transformation rate was at the range of 79.4%~82.8%. For nano-Fe/Cu bimetallic material, the reaction course of nitrate reduction was similar to nano-Fe/Ni system, and it also suffers two steps. But the difference between Fe/Ni and Fe/Cu nano-material was that metallic catalyst Cu has better selectivity to NO2- than Ni. Further more, the transformation process from NO3- to NO2- was quick, reversely, the transformation from NO2- to NH4+ was slow.
Nano-Fe/Pd and nanoscale Fe/Pd/Cu compound materials were also synthesized in our work, the denitrification of nitrate with these nanosized particles were discussed preliminarily. The results showed that using Fe0 as reductant, different reduction results could be obtained with the different catalyst Ni、Cu and Pd. For Fe0 systemic nanoscale particles prepared in our laboratory, nano-Fe/Cu has the highest reactivity and selectivity to NO2-, but the lowest selectivity to NH4+. So it is a promising remediation technology for nitrate contamination.
目前应用于地下水中硝酸盐去除的技术主要有生物反硝化、离子交换技术、膜分离法和化学还原修复等技术;其中生物处理法具有高效低耗的特点,但会导致出水中含有细菌和残留有机物,必须进行后续处理;离子交换和膜分离等物理化学处理技术只是将硝酸盐污染物进行了浓缩或转移,并没有对其进行彻底去除,同时产生高浓度再生废液同样需要处理;而在化学还原反硝化中,应用负载型催化剂可将大部分硝酸盐转化为N2,但催化还原过程中需要以H2作为还原剂,而H2容易爆炸,不便于工程施用;纳米Fe0可快速还原地下水中的硝酸盐,但其产物主要为NH4+-N,只有很小部分硝酸盐可能被转化为N2。
针对以上问题,本文采用液相还原法制备了纳米级Fe/Ni、Fe/Cu、Fe/Pd和Fe/Pd/Cu金属复合材料,并首次将纳米Fe/Ni和纳米Fe/Pd/Cu颗粒应用于地下水中硝酸盐污染物的去除,采用TEM-EDS、SEM、XRD、BET等分析手段对纳米材料的结构、组成进行了表征,系统的研究了不同催化剂金属对硝酸盐还原中间产物和最终产物的影响,同时对纳米颗粒还原NO3-的反应机理进行了探讨。与普通铁屑相比,纳米Fe0具有很高的反应活性,金属催化剂Ni、Cu、Pd的引入进一步提高了NO3-的去除速率,且不同催化剂种类对还原速率及还原产物具有不同的影响。
对比普通铁屑与纳米零价铁去除NO3-的反应,溶液pH是影响铁屑反应速率的主要影响因素,酸性条件有利于铁屑还原去除NO3-,而纳米Fe0即使在中性初始pH条件下也具有较高的反应活性;将铁屑与纳米Fe0分别应用于地浸采铀实际地下水,普通铁屑反应5 h,硝酸盐去除率为93% ,而纳米Fe0 15分钟即可将硝酸盐污染物完全去除,但约96%的NO3-被转化为NH4+-N。
在纳米Fe/Ni去除硝酸盐的研究中,当Ni负载量为5.0%时,且在中性pH条件下,纳米颗粒具有最高的反应活性;新鲜制备的Fe/Ni纳米双金属颗粒,在空气中缓慢氧化22h后可稳定存在于空气中,但其反应活性降为原来的十分之一,与纳米Fe0反应活性相当,继续老化44 h对纳米Fe/Ni的反应活性影响不大;反应中有少量NO2-作为中间副产物被检出,但最终与NO3-一起被同时去除,NH4+转化率在84.6%~90.6%范围内,改变Ni负载量、溶液初始pH值、初始浓度等实验条件对改善产物选择性的贡献很小;认为硝酸盐的脱硝反应经历了NO3-→NO2-→NH4+两个转化步骤,为连续分步反应,其中NO3-→NO2-为整个反应的速度控制步骤。
以Cu为催化剂催化还原硝酸盐,当Cu负载量为5.0%时,纳米Fe/Cu与硝酸盐反应具有最快的去除速率,30min可将硝酸盐完全去除;反应过程中有30%的NO3-可被还原为中间副产物NO2-,提高nano-Fe/Cu的反应活性,有利于NO2-在溶液中的积累,但NO2-可进一步被转化为NH4+或N2,NH4+最终转化率为79.4%~82.8%;纳米Fe/Cu复合材料还原NO3-的反应历程与纳米Fe/Ni相似,为连续分步反应,与nano-Fe/Ni反应体系不同的是,金属Cu催化剂对NO2-具有较高的选择性, NO3-→NO2-转化速率较快,而NO2-→NH4+的转化速率较慢。
本文同时合成了纳米Fe/Pd以及纳米Fe/Pd/Cu复合材料,并对其催化还原硝酸盐的反应进行了初步探讨。实验结果表明,以Fe0为还原剂,分别以Ni、Cu、Pd不同金属为催化剂去除地下水中的硝酸盐,具有不同的还原效果,其中纳米Fe/Cu反应体系的反应活性最高,对中间产物NO2-的选择性最大,且对NH4+具有较小的选择性,在硝酸盐污染物的环境修复中具有很好的发展前景。
Recently, with the development of industry and agriculture, nitrate pollution in ground water has been an importantly environmental problem and with the tendency of gradually deterioration. Nowadays, it has been prevalently considered by people. Using nanotechnology to remediate environmental pollution is a new direction of environmental remediation in the world. Nanoscale materials have the characteristic of small diameter, high specific surface area to mass ratios and great surface reactivity. In addition, nanoparticles could be injected directly to contaminated field and realize in situ remediation of ground water. So synthesizing new and high efficiency nanoscale materials to reduce nitrate has become the focus of water research.
Technologies applied to remove nitrate in ground water include biological denitrification, ion exchange, membrane separation and chemical reduction. Nitrate removal with biological approach may obtain high efficiency and low cost, but it may lead to the existence of bacteria and organic compounds in water, it request further treatment. For physico-chemical approaches, nitrate is only shift to another form, and not removed completely, on the other hand, it may bring large volumes of waste solution with high concentration which also needs to be treated. Application of loading catalyst could transform mostly nitrate to N2, but during the catalytic process, H2 is used as reductant which is easy to blast and difficult to construction. Nitrate could be rapidly reduced by nanoscale Fe0 particles, but the main product is NH4+-N, only a little nitrate may be transformed to N2.
To overcome these drawbacks, liquid-phase synthesized method was applied to prepare nanoscale Fe/Ni、Fe/Cu、Fe/Pd and Fe/Pd/Cu compound materials. In the nanoscale materials, nano-Fe/Ni and nano-Fe/Pd/Cu particles were firstly used to reduce nitrate contamination in groundwater. Nanoparticles were characterized by TEM-EDS, SEM, XRD and BET techniques. Nitrate reduction with different nanoscale materials was investigated systemically. At the same time, the reduction mechanism with nanoparticle was discussed in our work. Nanosized Fe0 behaved high reactivity during the denitrification of nitrate compared with common iron powder. The introduction of Ni, Cu and Pd further enhance the removal rate, and different catalyst makes differently degree effects on reduction rate and product.
For iron powder, solution pH is an important parameter influencing nitrate reduction and low pH is favorable for the denitrification of nitrate. Different from iron powder, nanosized Fe0 performed large reaction rate even under the condition of neutral solution pH. Using iron powder and nano-Fe0 to treat in-situ uranium leaching groundwater, under laboratory conditions, nitrate removal rate was 93% in 5 h by iron powder but nitrate was removed completely by nanosized Fe0 within 15 min. About 96% nitrate was reduced to NH4+-N.
In nano-Fe/Ni reaction system, when Ni loading was 5.0%, nanoparticles showed the highest reactivity under neutral initial solution pH. After slowly ageing 22 h, the reactivity of freshly prepared nanoscale Fe/Ni particles decreased about 10 times, but with the followed 44 h ageing, little decreasing of reactivity was observed which is equivalent to freshly synthesized nano-Fe0. Nitrite was detected as the intermediate product during the reduce process and disappeared companied with nitrate vanishing. NH4+-N transformation rate was at the range of 84.6%~90.6%. Little improve of selectivity to N2 was obtained through changing Ni contents, initial solution pH and nitrate concentration et al. experimental conditions. According to the analysis of product, it was considered that nitrate reduction by Ni/Fe nanoparticles undergo two steps: (1) NO3- was reduced to NO2- with the tendency of increasing at first and disappeared from solution at last; (2) NO2- was then reduced to NH4+. The first transformation process was the control step.
Using Cu as catalyst catalytic reduce nitrate contaminant, when Cu content was 5.0% nano-Fe/Cu bimetallic particles showed the rapidest removal rate, and nitrate was removed entirely within 30 min. During the process of nitrate reduction, about 30% nitrate was transformed to intermediate product NO2-. Increasing the reactivity of nanoscale Fe/Cu particles was favorable to the accumulation of NO2- in the solution. At the end of reaction, NO2- was reduced to NH4- N or N2 and NH4- N transformation rate was at the range of 79.4%~82.8%. For nano-Fe/Cu bimetallic material, the reaction course of nitrate reduction was similar to nano-Fe/Ni system, and it also suffers two steps. But the difference between Fe/Ni and Fe/Cu nano-material was that metallic catalyst Cu has better selectivity to NO2- than Ni. Further more, the transformation process from NO3- to NO2- was quick, reversely, the transformation from NO2- to NH4+ was slow.
Nano-Fe/Pd and nanoscale Fe/Pd/Cu compound materials were also synthesized in our work, the denitrification of nitrate with these nanosized particles were discussed preliminarily. The results showed that using Fe0 as reductant, different reduction results could be obtained with the different catalyst Ni、Cu and Pd. For Fe0 systemic nanoscale particles prepared in our laboratory, nano-Fe/Cu has the highest reactivity and selectivity to NO2-, but the lowest selectivity to NH4+. So it is a promising remediation technology for nitrate contamination.
引文
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