选矿尾砂重金属污染化学修复技术研究
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摘要
湖南是著名的“有色金属之乡”。长期有色金属采选产生了大量的选矿尾砂。尾砂多是利用山谷筑坝堆置,尾砂库一般无防渗措施。由于尾砂中含有大量的重金属污染物,这给区域生态环境造成了严重的胁迫。本文以该环境问题为研究对象,对湖南省10个大型矿山尾矿库进行了全面的重金属污染现状调查与评价,并以调查结论为基础,展开化学萃取修复技术、小规模土壤柱实验和化学改良技术的研究。研究成果可望为区域的尾矿库重金属治理和管理提供技术和理论支撑。研究结果表明：
被调查的10个有色金属矿山尾矿的重金属含量都严重超标,主要的重金属污染物有铅、锌、铜和镉。其中,铜山岭、冷水江与黄沙坪三处样品中Zn含量均严重超标,分别为10475.63mg/kg、151500.00mg/kg和12922.50mg/kg；永州铅锌矿、宝山铜矿、冷水江铅锌矿和黄沙坪铅锌矿的Pb含量特别高,分别为5846.42mg/kg、4742.30mg/kg、6470.00mg/kg和6850.17mg/kg。从重金属的存在形态分析上来看,各种重金属在尾矿中的主要存在形态各异：Pb主要以Fe/Mn氧化物结合态和残留态形式存在,可交换态与碳酸盐结合态的Pb含量极少,但永州铅锌矿尾矿中可交换态的Pb高达69%,这对周边环境有着极大影响；Cd主要以残留态存在,其它形态没有呈现明显的规律性；大部分的Cu主要以硫化物和有机物结合态存在,其次是残留态；Zn的主要存在形态是硫化物和有机物结合态与残留态。根据尾砂样的PI值和DI值分析,建议尽快进行治理与恢复的矿区是：永州铅锌矿、宝山铜矿、湘潭锰矿和冷水江铅锌矿。
应用化学萃取剂对尾矿的重金属污染进行修复的机理非常复杂,其中涉及沉淀/溶解、配合/离解、吸附/解析等一系列复杂的物理化学过程。萃取剂本身的物理化学性质、用量、pH值、萃取时间、尾矿的矿物种类及性质、重金属种类、重金属的存在形态等等都将对萃取效率产生影响。EDTA是一种优质的化学萃取剂,其对于不同的尾矿显示出了良好的适应性和高效性。其萃取效率受重金属的存在形态、萃取系统的pH值、碱金属离子的浓度、铁锰离子浓度等因素的制约。本研究所采用的4种萃取剂中,永州铅锌矿尾矿的最佳萃取剂为EDTA;湘潭锰矿尾矿的萃取剂除了乙二酸不适合外,最佳萃取剂需要进一步论证；车江铜矿尾矿的萃取剂除了柠檬酸不适合外,最佳萃取剂需要进一步论证。萃取剂的选择是化学萃取技术是否成功的前提条件,通常说来,EDTA是一种不错的选择,但是,若重金属污染物以可还原态为主,可以考虑使用还原性的萃取剂,如草酸；若重金属污染物以可氧化态为主,可以考虑氧化性的萃取剂,如硝酸,高锰酸钾等；若重金属污染物以酸可提取态为主,可以考虑EDTA或者无机酸,如盐酸,硝酸和硫酸等。鼠李糖脂可以提高萃取效率,但是就技术应用上来讲,权衡修复成本,建议不予考虑。腐殖质可以影响修复效率,这种影响可能是正面的也有可能是负面的。永州铅锌矿尾矿EDTA化学萃取修复的最佳条件为：EDTA浓度0.05mol/L,pH值5.0,固液比(m/v)为1：20,萃取时间大于12h。柠檬酸对于湘潭锰矿尾矿中的锰、铅和镉均表现较好的萃取效果,相对于盐酸和EDTA,其是湘潭锰矿尾矿的最佳萃取剂,柠檬酸对于锰的萃取效率随萃取时间、萃取剂的用量的增加而增加,但是对于铅的去除,EDTA效果更佳。
土壤柱实验中,三种萃取剂的萃取效率依次为：EDTA>HNO3>CaCl2,EDTA对Pb、Zn、Cu和Cd均表现出较好的萃取效果；EDTA对于4种金属萃取效率的高低顺序为：Cd>Zn>Cu>Pb。萃取时,由于萃取液中的重金属污染物容易被土壤颗粒重吸附,尾砂中的Pb、Cu和Cd含量随着尾砂深度的增加而增加,使得萃取效率随土壤柱深度的增加而降低,尤其Cu表现明显。Zn的萃取效果则与土壤柱深度不呈现出相关性。重金属的存在形态对萃取效率有很大的影响,但并不是活性较强的形态就能被萃取剂完全萃取,惰性的形态就不能被萃取剂萃取,研究结果显示4种金属的4个形态,均能被萃取剂萃取,而且HNO3和CaCl2萃取后酸可提取态重金属含量反而上升了。萃取后,随着土壤柱深度的增加,金属的各形态浓度均有所增加,尤其表现在酸可提取态。土壤柱实验中,任意单元的土壤截面的重金属含量是一个随萃取时间和土壤柱深度变化的三维变量,其含量的变化趋势为先逐渐上升,达到最大值后逐渐慢慢下降的过程。土壤柱实验的最适宜的修复时间为12小时左右。
腐殖酸可以用来改良重金属污染土壤。研究者发现腐殖酸的添加对土壤中不同的重金属元素有不同的影响。两组土样中Pb和Cd的形态分布受腐殖酸的影响比较大,腐殖酸的添加有望降低土壤中Pb和Cd的生物活性。Cu和Zn受腐殖酸的影响比较小,形态分布变化并无规律性。
Hunan province is a famous "town of non-ferrous metals", and the long-term non-ferrous metal mining has produced a large number of non-ferrous mineral tailings. Tailings were usually disposed by damming at the valley. Tailings contain a large number of heavy metal pollutants, which have significant impacts on the regional ecological environment because of lack of tailings seepage treatment. In this paper, this environmental problem was systematically studied. A comprehensive survey of heavy metal contamination and evaluation of10large-scale mine tailings reservoirs in Hunan province was conducted, then the mechanism of chemical extraction techniques, small-scale soil column experiments and chemical modification techniques were carried out. The results were expected to offer technical and theoretical references for the development of tailings treatment and management. The results show that:
The heavy metal contents of the10non-ferrous metal mine tailings surveyed in this study all exceeded the standard. The main heavy metal pollutants were lead, zinc, copper and cadmium. The contents of Zn in samples from Tongshanling, Lengshuijiang and Huangshaping were particularly high (10475.63mg/kg,151500.00mg/kg and12922.50mg/kg, respectively). In Yongzhou, Baoshan, Lengshuijiang and Huangshaping, the Pb contents were particularly high (5846.42mg/kg,4742.30mg/kg,6470.00mg/kg and6850.17mg/kg, respectively). For the speciation analysis of heavy metal, there were a variety of main different forms of heavy metals in the tailings:Pb was mainly in the form of Fe/Mn oxide bound and residual state, and Pb content existed in the form of exchangeable and carbonate bound was very few. However, the Pb content of exchangeable bound in Yongzhou samples was as high as69%. Cd mainly existed in residual state, and there was no obviously regularity of the other forms. Most of Cu was in the sulfide/organic bound, followed by the residual state. Zn was in the main existing forms of sulfide and organic matter bound and residual state. According to the analysis of PI values and DI values of soil samples, the mining sites which needed treatment and remediation as soon as possible were:Yongzhou, Baoshan, Xiangtan manganese and Lengshuijiang.
The mechanism of chemical extractant on the tailings is very complex, involving a series of complex physical and chemical processes such as precipitation/dissolution, complexation/dissociation, adsorption/readsorption, etc. All the physical and chemical properties of extractant species, dosage of extractant, pH, extraction time, the mineral tailings type, types of heavy metals and the fraction of heavy metal speciation are influence factors of chemical extractant. EDTA was a high-quality chemical extractant in our study, which showed a good adaptability and high efficiency on different types of tailings. Of the four kinds of extractants in this study, the best extractant for Yongzhou lead-zinc mine tailings was EDTA; the best extractant for Xiangtan manganese tailings required further verification except that adipic acid extractant was not suitable; the best extraction agent needs further proof for Chejiang copper tailings except that the extractant citric acid was not suitable. Selecting a suitable extractant was a prerequisite for the success of chemical extraction technology. Generally, EDTA was a good choice. However, if the heavy metal pollutant was mainly in oxidable form, oxidative extractant was suitable, such as nitric acid, potassium permanganate, etc. If the heavy metal pollutant was mainly in reducible form, reductive extractant was suitable, such as oxalic acid. If the heavy metal pollutant was mainly in acid extractable form, EDTA or inorganic acid (such as hydrochloric acid, nitric acid and sulfuric acid and so on) was suitable extractant. Rhamnolipid can enhance the efficiency of extraction, but its application should not be considered because it would add the cost of repair. Humus can influence the repair efficiency, and the impact is likely to be both positive and negative. In this experiment adding humus in the chemical extraction of tailings should not to be considered in terms of technology. The optimal conditions for Yongzhou lead-zinc tailings chemical extraction were:EDTA concentration of0.05mol/L, pH5, solid-liquid ratio (m/v)1:20, and extraction time was more than12h. Citric acid showed better extraction efficiency for the manganese, lead and cadmium in Xiangtan manganese tailings remediation. Compared with hydrochloric acid and EDTA, it was the best extraction agent, but for the removal of lead, EDTA was better.
In soil column experiment, three extractants were ordered by the performance of the extraction efficency as EDTA>HNC>3>CaCl2. EDTA was a good extractant for the chemical extraction of Pb, Zn, Cu and Cd. The extraction efficiency of EDTA for four kinds of metal was in the order:Cd> Zn> Cu> Pb. During extraction process, Pb, Cu and Cd polluants were easy to be readsorbed by soil particles, so that the effect of extraction efficency also reduced significantly with the increase of soil depth, especially Cu. There was no correlation between the effect of Zn extraction efficency and the soil depth. The extraction efficiency was greatly affected by the speciation of heavy metals, but not heavy metal with form of strong activity can be completely extracted by extractant, and the form of inert heavy metal can not be extracted. The results indicated the four kinds of metal speciation can be extracted by extractants, and the form of acid soluable increased after extracted by HNO3and CaCl2. After extraction, with the increase in the depth of the soil column, the concentrations of metal in all forms were increased, particularly in the acid soluable. In soil column experiment, the heavy metal content of arbitrary soil cross-section was a three-dimensional variable with time and soil column depth, and its content was increased gradually to the maximum then dropped in the process of remediation. The most appropriate time of soil column experiments was about12hours.
Humic acid can be used in improvement of heavy metal contaminated soils, it was reported that there were different effects on different heavy metals by adding humic acid in soil. The speciation of Pb and Cd in soil was strongly affected by humic acid, but the speciation of Cu and Zn can hardly be affected by humic acid. Accordingly, the soil polluted by Pb and Cd can be remedied by humic acid to decrease its bioavailability.
被调查的10个有色金属矿山尾矿的重金属含量都严重超标,主要的重金属污染物有铅、锌、铜和镉。其中,铜山岭、冷水江与黄沙坪三处样品中Zn含量均严重超标,分别为10475.63mg/kg、151500.00mg/kg和12922.50mg/kg；永州铅锌矿、宝山铜矿、冷水江铅锌矿和黄沙坪铅锌矿的Pb含量特别高,分别为5846.42mg/kg、4742.30mg/kg、6470.00mg/kg和6850.17mg/kg。从重金属的存在形态分析上来看,各种重金属在尾矿中的主要存在形态各异：Pb主要以Fe/Mn氧化物结合态和残留态形式存在,可交换态与碳酸盐结合态的Pb含量极少,但永州铅锌矿尾矿中可交换态的Pb高达69%,这对周边环境有着极大影响；Cd主要以残留态存在,其它形态没有呈现明显的规律性；大部分的Cu主要以硫化物和有机物结合态存在,其次是残留态；Zn的主要存在形态是硫化物和有机物结合态与残留态。根据尾砂样的PI值和DI值分析,建议尽快进行治理与恢复的矿区是：永州铅锌矿、宝山铜矿、湘潭锰矿和冷水江铅锌矿。
应用化学萃取剂对尾矿的重金属污染进行修复的机理非常复杂,其中涉及沉淀/溶解、配合/离解、吸附/解析等一系列复杂的物理化学过程。萃取剂本身的物理化学性质、用量、pH值、萃取时间、尾矿的矿物种类及性质、重金属种类、重金属的存在形态等等都将对萃取效率产生影响。EDTA是一种优质的化学萃取剂,其对于不同的尾矿显示出了良好的适应性和高效性。其萃取效率受重金属的存在形态、萃取系统的pH值、碱金属离子的浓度、铁锰离子浓度等因素的制约。本研究所采用的4种萃取剂中,永州铅锌矿尾矿的最佳萃取剂为EDTA;湘潭锰矿尾矿的萃取剂除了乙二酸不适合外,最佳萃取剂需要进一步论证；车江铜矿尾矿的萃取剂除了柠檬酸不适合外,最佳萃取剂需要进一步论证。萃取剂的选择是化学萃取技术是否成功的前提条件,通常说来,EDTA是一种不错的选择,但是,若重金属污染物以可还原态为主,可以考虑使用还原性的萃取剂,如草酸；若重金属污染物以可氧化态为主,可以考虑氧化性的萃取剂,如硝酸,高锰酸钾等；若重金属污染物以酸可提取态为主,可以考虑EDTA或者无机酸,如盐酸,硝酸和硫酸等。鼠李糖脂可以提高萃取效率,但是就技术应用上来讲,权衡修复成本,建议不予考虑。腐殖质可以影响修复效率,这种影响可能是正面的也有可能是负面的。永州铅锌矿尾矿EDTA化学萃取修复的最佳条件为：EDTA浓度0.05mol/L,pH值5.0,固液比(m/v)为1：20,萃取时间大于12h。柠檬酸对于湘潭锰矿尾矿中的锰、铅和镉均表现较好的萃取效果,相对于盐酸和EDTA,其是湘潭锰矿尾矿的最佳萃取剂,柠檬酸对于锰的萃取效率随萃取时间、萃取剂的用量的增加而增加,但是对于铅的去除,EDTA效果更佳。
土壤柱实验中,三种萃取剂的萃取效率依次为：EDTA>HNO3>CaCl2,EDTA对Pb、Zn、Cu和Cd均表现出较好的萃取效果；EDTA对于4种金属萃取效率的高低顺序为：Cd>Zn>Cu>Pb。萃取时,由于萃取液中的重金属污染物容易被土壤颗粒重吸附,尾砂中的Pb、Cu和Cd含量随着尾砂深度的增加而增加,使得萃取效率随土壤柱深度的增加而降低,尤其Cu表现明显。Zn的萃取效果则与土壤柱深度不呈现出相关性。重金属的存在形态对萃取效率有很大的影响,但并不是活性较强的形态就能被萃取剂完全萃取,惰性的形态就不能被萃取剂萃取,研究结果显示4种金属的4个形态,均能被萃取剂萃取,而且HNO3和CaCl2萃取后酸可提取态重金属含量反而上升了。萃取后,随着土壤柱深度的增加,金属的各形态浓度均有所增加,尤其表现在酸可提取态。土壤柱实验中,任意单元的土壤截面的重金属含量是一个随萃取时间和土壤柱深度变化的三维变量,其含量的变化趋势为先逐渐上升,达到最大值后逐渐慢慢下降的过程。土壤柱实验的最适宜的修复时间为12小时左右。
腐殖酸可以用来改良重金属污染土壤。研究者发现腐殖酸的添加对土壤中不同的重金属元素有不同的影响。两组土样中Pb和Cd的形态分布受腐殖酸的影响比较大,腐殖酸的添加有望降低土壤中Pb和Cd的生物活性。Cu和Zn受腐殖酸的影响比较小,形态分布变化并无规律性。
Hunan province is a famous "town of non-ferrous metals", and the long-term non-ferrous metal mining has produced a large number of non-ferrous mineral tailings. Tailings were usually disposed by damming at the valley. Tailings contain a large number of heavy metal pollutants, which have significant impacts on the regional ecological environment because of lack of tailings seepage treatment. In this paper, this environmental problem was systematically studied. A comprehensive survey of heavy metal contamination and evaluation of10large-scale mine tailings reservoirs in Hunan province was conducted, then the mechanism of chemical extraction techniques, small-scale soil column experiments and chemical modification techniques were carried out. The results were expected to offer technical and theoretical references for the development of tailings treatment and management. The results show that:
The heavy metal contents of the10non-ferrous metal mine tailings surveyed in this study all exceeded the standard. The main heavy metal pollutants were lead, zinc, copper and cadmium. The contents of Zn in samples from Tongshanling, Lengshuijiang and Huangshaping were particularly high (10475.63mg/kg,151500.00mg/kg and12922.50mg/kg, respectively). In Yongzhou, Baoshan, Lengshuijiang and Huangshaping, the Pb contents were particularly high (5846.42mg/kg,4742.30mg/kg,6470.00mg/kg and6850.17mg/kg, respectively). For the speciation analysis of heavy metal, there were a variety of main different forms of heavy metals in the tailings:Pb was mainly in the form of Fe/Mn oxide bound and residual state, and Pb content existed in the form of exchangeable and carbonate bound was very few. However, the Pb content of exchangeable bound in Yongzhou samples was as high as69%. Cd mainly existed in residual state, and there was no obviously regularity of the other forms. Most of Cu was in the sulfide/organic bound, followed by the residual state. Zn was in the main existing forms of sulfide and organic matter bound and residual state. According to the analysis of PI values and DI values of soil samples, the mining sites which needed treatment and remediation as soon as possible were:Yongzhou, Baoshan, Xiangtan manganese and Lengshuijiang.
The mechanism of chemical extractant on the tailings is very complex, involving a series of complex physical and chemical processes such as precipitation/dissolution, complexation/dissociation, adsorption/readsorption, etc. All the physical and chemical properties of extractant species, dosage of extractant, pH, extraction time, the mineral tailings type, types of heavy metals and the fraction of heavy metal speciation are influence factors of chemical extractant. EDTA was a high-quality chemical extractant in our study, which showed a good adaptability and high efficiency on different types of tailings. Of the four kinds of extractants in this study, the best extractant for Yongzhou lead-zinc mine tailings was EDTA; the best extractant for Xiangtan manganese tailings required further verification except that adipic acid extractant was not suitable; the best extraction agent needs further proof for Chejiang copper tailings except that the extractant citric acid was not suitable. Selecting a suitable extractant was a prerequisite for the success of chemical extraction technology. Generally, EDTA was a good choice. However, if the heavy metal pollutant was mainly in oxidable form, oxidative extractant was suitable, such as nitric acid, potassium permanganate, etc. If the heavy metal pollutant was mainly in reducible form, reductive extractant was suitable, such as oxalic acid. If the heavy metal pollutant was mainly in acid extractable form, EDTA or inorganic acid (such as hydrochloric acid, nitric acid and sulfuric acid and so on) was suitable extractant. Rhamnolipid can enhance the efficiency of extraction, but its application should not be considered because it would add the cost of repair. Humus can influence the repair efficiency, and the impact is likely to be both positive and negative. In this experiment adding humus in the chemical extraction of tailings should not to be considered in terms of technology. The optimal conditions for Yongzhou lead-zinc tailings chemical extraction were:EDTA concentration of0.05mol/L, pH5, solid-liquid ratio (m/v)1:20, and extraction time was more than12h. Citric acid showed better extraction efficiency for the manganese, lead and cadmium in Xiangtan manganese tailings remediation. Compared with hydrochloric acid and EDTA, it was the best extraction agent, but for the removal of lead, EDTA was better.
In soil column experiment, three extractants were ordered by the performance of the extraction efficency as EDTA>HNC>3>CaCl2. EDTA was a good extractant for the chemical extraction of Pb, Zn, Cu and Cd. The extraction efficiency of EDTA for four kinds of metal was in the order:Cd> Zn> Cu> Pb. During extraction process, Pb, Cu and Cd polluants were easy to be readsorbed by soil particles, so that the effect of extraction efficency also reduced significantly with the increase of soil depth, especially Cu. There was no correlation between the effect of Zn extraction efficency and the soil depth. The extraction efficiency was greatly affected by the speciation of heavy metals, but not heavy metal with form of strong activity can be completely extracted by extractant, and the form of inert heavy metal can not be extracted. The results indicated the four kinds of metal speciation can be extracted by extractants, and the form of acid soluable increased after extracted by HNO3and CaCl2. After extraction, with the increase in the depth of the soil column, the concentrations of metal in all forms were increased, particularly in the acid soluable. In soil column experiment, the heavy metal content of arbitrary soil cross-section was a three-dimensional variable with time and soil column depth, and its content was increased gradually to the maximum then dropped in the process of remediation. The most appropriate time of soil column experiments was about12hours.
Humic acid can be used in improvement of heavy metal contaminated soils, it was reported that there were different effects on different heavy metals by adding humic acid in soil. The speciation of Pb and Cd in soil was strongly affected by humic acid, but the speciation of Cu and Zn can hardly be affected by humic acid. Accordingly, the soil polluted by Pb and Cd can be remedied by humic acid to decrease its bioavailability.
引文
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