锑矿区沉积物生态风险评价及修复技术研究
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摘要
我国锑矿产量和储备量高居世界首位。锑被广泛用于化工、电子和医药行业,是重要的战略资源。我国锑矿主要集中分布在湖南、贵州、广西等南方省区。锑矿区开采、冶炼和锑制品加工已经导致了矿区严重的水污染。本论文针对我国锑矿区锑污染的现状,开展了矿区沉积物和水环境锑污染调查、锑的生物有效性分析、锑和重金属污染的生态风险评价、污染河流沉积物中锑的稳定性、吸附除锑技术及除锑吸附材料安全性评价的研究工作。
首先调查了广西大厂锑矿区下游河流中水样和沉积物样品中的Sb含量,14个河水样品中Sb浓度范围为59.1～213.8μ g/L,平均值为139.9μ g/L。沉积物中Sb含量范围为5.06～20.9mg/kg,平均值为12.9mg/kg。对沉积物中的Sb使用Tessier形态分析的结果显示,沉积物中铁锰氧化物结合态(中等可利用性)的Sb占8.11～75.1%,平均值53.0%；残渣态(惰性态)的Sb为3.35～39.2%,平均值19.9%；碳酸盐结合态的锑为9.87-32.4%,平均值15.1%；再其次为有机结合态15.5-32.4%,平均值6.21%；水溶态3.10-16.0%,平均值5.82%。除Sb外,沉积物中其它共存重金属Cd、Cu、Ni、As、Zn、Pb和Cr的平均浓度分别为10.9mg/kg、204mg/kg、247mg/kg、19.3mg/kg、1329mg/kg、44.0mg/kg和101mg/kg。采用潜在生态风险指数法评价沉积物中Sb及重金属污染的潜在生态风险结果显示,Cd和Sb的潜在生态风险最大,为该地区主要生态风险因子,其余6种金属的潜在生态风险由大到小依次为Cu, Ni, As, Zn, Pb和Cr。鉴于Cd的相关研究已经比较深入,本文未作进一步研究。
为进一步了解污染河流沉积物特性及其中Sb的释放特性,对14个样点的沉积物进行了物相分析、红外光谱(FTIR)分析和元素分析。结果表明样品所含矿物相、表面官能团、主要元素含量等特性相似。沉积物中主要含有石英石、斜长石、云母、方解石和斜磷锰矿石等矿物,主要金属含量顺序均为Si>Al>Fe>Ca>K>Mg>Mn。进一步考察pH、盐度和腐植酸含量对样品锑释放影响的结果表明,在pH3.0±0.2、固液比1g/0.1L、混合时间3h、混合强度160rpm时,锑释放的浓度范围在22～125μg/L之间。随着盐度增加,14个样点锑释放量均呈增大趋势,浓度变化范围为26～180μg/L。随着腐植酸浓度增加,3个锑释放量最大样点的沉积物样品锑释放量也呈增大趋势,浓度范围为22～153μg/L。在pH、盐度和腐植酸影响这三个因素中,pH对锑释放影响最大。pH对沉积物/酸盐作用的影响是样品所含矿物溶解释放锑和矿物表面荷电特性改变吸附Sb(OH)6-/H3SbO3能力变化两方面综合平衡的结果。在pH=3.0时,沉积物锑释放量与沉积物表面Mn元素显著相关,推测样品斜磷锰矿的含量及其溶解显著地影响锑的释放,矿物(主要是斜磷锰矿)溶解较之表面吸附对锑的释放影响更大。
针对污染的含锑水样,进行了吸附处理研究,利用共沉淀法制备的铁锆氧化物(IZOP)能有效地吸附水中的Sb(V)。对IZOP的结构及表面分析结果表明,该吸附剂粒度为微米级,呈无定形结构,具有较大的比表面积,孔容达到了0.42ml/g。对IZOP除Sb(V)性能测试表明,其最佳吸附pH范围为中性偏酸(<7.5),Sb(V)吸附过程符合准二级速率方程。在中性条件下,初始Sb(V)浓度为20mg/L时,IZOP对Sb(V)的最大吸附容量可达78mg/g。Sb(Ⅴ)在IZOP上的吸附可以用Langmiur等温吸附式描述。经急性毒性实验和小鼠嗜多染红细胞毒理学测试表明该吸附剂本身安全的,处理后耗竭材料符合渗滤性毒性评价标准(TCLP)。
本研究对于了解锑矿区河流水体和沉积物污染现状、沉积物中锑的生物有效性、锑及重金属的生态风险,以及沉积物中锑的稳定性有着明显的参考价值；对于含锑水样的处理和修复有着明显的借鉴意义。总体而言,本研究对于推动目前的锑污染研究和修复方法研究都有着积极的意义。
Antimony production and reserves in China is the highest in the world. It is one of the most important strategic resources and is widely used in chemical, electronics and pharmaceutical industries. Antimony resources in China are mainly produced in the southern provinces of Hunan, Guizhou, Guangxi etc. Mining, smelting and processing of antimony products have led to serious water contamination in antimony-mining areas. Focused on antimony contaminations in water and sediments in antimony-mining areas, this thesis carries out research work on antimony contamination investigation, biological availability analysis, ecological risk analysis of antimony and other heavy metals, the stability and release risk of antimony in sediments of polluted rivers, absorptive removal from water, and safety assessment on adsorption materials.
First, antimony in river water and sediments at downstream rivers from GuangXi Dachang antimony mining areas were investigated.14samples were collected. Antimony in water are from59.1-213.8μg/L, with an average concentration of139.9μg/L. Antimony in sediments are from5.06-20.9mg/kg, with an average concentration of12.9mg/kg. The species of antimony in sediments were analyzed using the Tessier sequential extraction method. The results showed that8.11-75.1%of Sb in sediments were combined to iron oxides and manganese oxides, and3.35-39.2%of antimony in residual,9.87-32.4%associated with carbonate salts,15.5-32.4%in organical-binding form and the other3.10-16.0%in water dissolvable form. In addition, the average concentrations of Cd、Cu、Ni、As、 Zn、Pb and Cr in sediments are10.9mg/kg,204mg/kg,247mg/kg,19.3mg/kg,1329mg/kg,44.0mg/kg and101mg/kg, respectively. In sediments, Cd and Sb, having the largest potential ecological risks, are the major ecological risk factors in this area. The potential ecological risks of the other6metals including Cu, Ni, As, Zn, Pb and Cr are in a descending order. Since Cd contaminations in sediments and water have been intensively reported in recent years, so it is not focused in the further study.
To investigate the effect of aquatic chemistry on antimony release from Sb-contained sediments, samples from the down-stream of an antimony-polluted reviver were characterized. Their X-ray diffraction patterns (XRD), Fourier transform infrared spectra (FTIR) and X-ray fluorescence spectra were collected. Moreover, the effect of pH, salty and concentrations of humic acids on the release of antimony were also investigated. The results showed that all sediment samples contained similar mineral phases, surface groups and similar main element contents. Identified phases included quartz. albite, muscovite, calcite and stewartite. Elements at the surface of the sediments followed the order of Si>Al>Fe>Ca>K>Mg>Mn. Batch release experiments showed that the amounts of released antimony increased with decreasing pH, increasing concentrations of salinity and humic acids. pH was the most important factor to affect antimony release.22～153μg/L of antimony was released from the14sediments at conditions of pH3.0±0.2, the adsorbent dose of1g/0.1L, shaking time of3h at160rpm. With increasing concentrations of salty and humic acid, the released antimony ranged from26to180μg/L, and from22to153μg/L, respectively. Among the three investigated factors, the effect of pH was the most intensive one. It is speculated that the release was caused by pH-related mineral dissolution and desorption, and the final states was an equilibrium of the both processes. At pH=3, the released antimony was positively correlated to the contents of Mn at the surface of sediments. That means that dissolution of stewartite rather than surface adsorption markedly affected the release of antimony.
The adsorption treatment study is adopted on the antimony-polluted water sample, and Iron-Zirconium Oxide Particle (IZOP) prepared by coprecipitation method can effectively absorb Sb(V) from water. Structure and surface analysis on IZOP shows that the adsorbent particle is micron-sized, amorphous-structured, has large specific surface areas, and the pore volume is0.42ml/g. The test of IZOP's absorption of Sb (V) shows that the optimum adsorption pH range is neutral partial acid (<7.5), and Sb (V) adsorption process is in line with the pseudo-second order rate equation. Under neutral conditions, the maximum adsorption capacity was78mg/g at an initial Sb(V) concentration of20mg/L. The isotherm of Sb(V) absorption on the IZOP adsorbent can be modeled by the Langmiur equation. Acute toxicity test and mouse polychromatic erythrocytes toxicology test show that the adsorbent is safe by itself, and the depletion materials after processing meet the Toxicity Characteristic Leaching Procedure (TCLP).
This study provides basic information on Sb pollution in water and sediments in a downstream revier in Dachang Sb-mining area, as well as the bioavailabitliy, and ecological risk and the remediation method. Besides, it has a positive meaning for promoting the research level of antimony contamination investigation and ecological risk assesment and the development of remediation technology.
首先调查了广西大厂锑矿区下游河流中水样和沉积物样品中的Sb含量,14个河水样品中Sb浓度范围为59.1～213.8μ g/L,平均值为139.9μ g/L。沉积物中Sb含量范围为5.06～20.9mg/kg,平均值为12.9mg/kg。对沉积物中的Sb使用Tessier形态分析的结果显示,沉积物中铁锰氧化物结合态(中等可利用性)的Sb占8.11～75.1%,平均值53.0%；残渣态(惰性态)的Sb为3.35～39.2%,平均值19.9%；碳酸盐结合态的锑为9.87-32.4%,平均值15.1%；再其次为有机结合态15.5-32.4%,平均值6.21%；水溶态3.10-16.0%,平均值5.82%。除Sb外,沉积物中其它共存重金属Cd、Cu、Ni、As、Zn、Pb和Cr的平均浓度分别为10.9mg/kg、204mg/kg、247mg/kg、19.3mg/kg、1329mg/kg、44.0mg/kg和101mg/kg。采用潜在生态风险指数法评价沉积物中Sb及重金属污染的潜在生态风险结果显示,Cd和Sb的潜在生态风险最大,为该地区主要生态风险因子,其余6种金属的潜在生态风险由大到小依次为Cu, Ni, As, Zn, Pb和Cr。鉴于Cd的相关研究已经比较深入,本文未作进一步研究。
为进一步了解污染河流沉积物特性及其中Sb的释放特性,对14个样点的沉积物进行了物相分析、红外光谱(FTIR)分析和元素分析。结果表明样品所含矿物相、表面官能团、主要元素含量等特性相似。沉积物中主要含有石英石、斜长石、云母、方解石和斜磷锰矿石等矿物,主要金属含量顺序均为Si>Al>Fe>Ca>K>Mg>Mn。进一步考察pH、盐度和腐植酸含量对样品锑释放影响的结果表明,在pH3.0±0.2、固液比1g/0.1L、混合时间3h、混合强度160rpm时,锑释放的浓度范围在22～125μg/L之间。随着盐度增加,14个样点锑释放量均呈增大趋势,浓度变化范围为26～180μg/L。随着腐植酸浓度增加,3个锑释放量最大样点的沉积物样品锑释放量也呈增大趋势,浓度范围为22～153μg/L。在pH、盐度和腐植酸影响这三个因素中,pH对锑释放影响最大。pH对沉积物/酸盐作用的影响是样品所含矿物溶解释放锑和矿物表面荷电特性改变吸附Sb(OH)6-/H3SbO3能力变化两方面综合平衡的结果。在pH=3.0时,沉积物锑释放量与沉积物表面Mn元素显著相关,推测样品斜磷锰矿的含量及其溶解显著地影响锑的释放,矿物(主要是斜磷锰矿)溶解较之表面吸附对锑的释放影响更大。
针对污染的含锑水样,进行了吸附处理研究,利用共沉淀法制备的铁锆氧化物(IZOP)能有效地吸附水中的Sb(V)。对IZOP的结构及表面分析结果表明,该吸附剂粒度为微米级,呈无定形结构,具有较大的比表面积,孔容达到了0.42ml/g。对IZOP除Sb(V)性能测试表明,其最佳吸附pH范围为中性偏酸(<7.5),Sb(V)吸附过程符合准二级速率方程。在中性条件下,初始Sb(V)浓度为20mg/L时,IZOP对Sb(V)的最大吸附容量可达78mg/g。Sb(Ⅴ)在IZOP上的吸附可以用Langmiur等温吸附式描述。经急性毒性实验和小鼠嗜多染红细胞毒理学测试表明该吸附剂本身安全的,处理后耗竭材料符合渗滤性毒性评价标准(TCLP)。
本研究对于了解锑矿区河流水体和沉积物污染现状、沉积物中锑的生物有效性、锑及重金属的生态风险,以及沉积物中锑的稳定性有着明显的参考价值；对于含锑水样的处理和修复有着明显的借鉴意义。总体而言,本研究对于推动目前的锑污染研究和修复方法研究都有着积极的意义。
Antimony production and reserves in China is the highest in the world. It is one of the most important strategic resources and is widely used in chemical, electronics and pharmaceutical industries. Antimony resources in China are mainly produced in the southern provinces of Hunan, Guizhou, Guangxi etc. Mining, smelting and processing of antimony products have led to serious water contamination in antimony-mining areas. Focused on antimony contaminations in water and sediments in antimony-mining areas, this thesis carries out research work on antimony contamination investigation, biological availability analysis, ecological risk analysis of antimony and other heavy metals, the stability and release risk of antimony in sediments of polluted rivers, absorptive removal from water, and safety assessment on adsorption materials.
First, antimony in river water and sediments at downstream rivers from GuangXi Dachang antimony mining areas were investigated.14samples were collected. Antimony in water are from59.1-213.8μg/L, with an average concentration of139.9μg/L. Antimony in sediments are from5.06-20.9mg/kg, with an average concentration of12.9mg/kg. The species of antimony in sediments were analyzed using the Tessier sequential extraction method. The results showed that8.11-75.1%of Sb in sediments were combined to iron oxides and manganese oxides, and3.35-39.2%of antimony in residual,9.87-32.4%associated with carbonate salts,15.5-32.4%in organical-binding form and the other3.10-16.0%in water dissolvable form. In addition, the average concentrations of Cd、Cu、Ni、As、 Zn、Pb and Cr in sediments are10.9mg/kg,204mg/kg,247mg/kg,19.3mg/kg,1329mg/kg,44.0mg/kg and101mg/kg, respectively. In sediments, Cd and Sb, having the largest potential ecological risks, are the major ecological risk factors in this area. The potential ecological risks of the other6metals including Cu, Ni, As, Zn, Pb and Cr are in a descending order. Since Cd contaminations in sediments and water have been intensively reported in recent years, so it is not focused in the further study.
To investigate the effect of aquatic chemistry on antimony release from Sb-contained sediments, samples from the down-stream of an antimony-polluted reviver were characterized. Their X-ray diffraction patterns (XRD), Fourier transform infrared spectra (FTIR) and X-ray fluorescence spectra were collected. Moreover, the effect of pH, salty and concentrations of humic acids on the release of antimony were also investigated. The results showed that all sediment samples contained similar mineral phases, surface groups and similar main element contents. Identified phases included quartz. albite, muscovite, calcite and stewartite. Elements at the surface of the sediments followed the order of Si>Al>Fe>Ca>K>Mg>Mn. Batch release experiments showed that the amounts of released antimony increased with decreasing pH, increasing concentrations of salinity and humic acids. pH was the most important factor to affect antimony release.22～153μg/L of antimony was released from the14sediments at conditions of pH3.0±0.2, the adsorbent dose of1g/0.1L, shaking time of3h at160rpm. With increasing concentrations of salty and humic acid, the released antimony ranged from26to180μg/L, and from22to153μg/L, respectively. Among the three investigated factors, the effect of pH was the most intensive one. It is speculated that the release was caused by pH-related mineral dissolution and desorption, and the final states was an equilibrium of the both processes. At pH=3, the released antimony was positively correlated to the contents of Mn at the surface of sediments. That means that dissolution of stewartite rather than surface adsorption markedly affected the release of antimony.
The adsorption treatment study is adopted on the antimony-polluted water sample, and Iron-Zirconium Oxide Particle (IZOP) prepared by coprecipitation method can effectively absorb Sb(V) from water. Structure and surface analysis on IZOP shows that the adsorbent particle is micron-sized, amorphous-structured, has large specific surface areas, and the pore volume is0.42ml/g. The test of IZOP's absorption of Sb (V) shows that the optimum adsorption pH range is neutral partial acid (<7.5), and Sb (V) adsorption process is in line with the pseudo-second order rate equation. Under neutral conditions, the maximum adsorption capacity was78mg/g at an initial Sb(V) concentration of20mg/L. The isotherm of Sb(V) absorption on the IZOP adsorbent can be modeled by the Langmiur equation. Acute toxicity test and mouse polychromatic erythrocytes toxicology test show that the adsorbent is safe by itself, and the depletion materials after processing meet the Toxicity Characteristic Leaching Procedure (TCLP).
This study provides basic information on Sb pollution in water and sediments in a downstream revier in Dachang Sb-mining area, as well as the bioavailabitliy, and ecological risk and the remediation method. Besides, it has a positive meaning for promoting the research level of antimony contamination investigation and ecological risk assesment and the development of remediation technology.
引文
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