微污染饮用水源中砷及几种重金属离子的吸附分离过程研究
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摘要
本文在科技部小城镇科技发展重大项目(2003BA808A17)支持下，根据国际上重金属微污染水体修复技术的发展趋势，针对重金属微污染水源水体特征，并在对上海水源地水体重金属污染背景调查的基础上，提出了三种有效修复技术方案：弱碱性阴离子交换树脂修复技术，铁、锰矿物修复技术及新型负载吸附剂修复技术。利用红外光谱、扫描电镜、X-射线衍射等现代分析测试手段对自主合成的几种新型吸附剂进行了分析表征，并通过影响因素分析、吸附等温试验和吸附动力学试验等详细探讨了三种修复技术的适用条件和微观作用机理。论文可以为重金属微污染水源水体的修复、突发性重金属污染事故的应急处理等提供理论指导和实际技术支持。
论文主要分为四个部分。(Ⅰ)微污染水体沉积物中重金属及砷的迁移转化规律研究；(Ⅱ)弱碱性阴离子交换树脂对微污染水源中重金属及砷的分离过程研究；(Ⅲ)铁锰氧化物吸附剂分离水体中重金属及砷的研究；(Ⅳ)负载吸附剂去除水体中重金属及砷的研究。
第一部分：
首先对上海水源地(包括上覆水和沉积物)中重金属作了背景调查，并利用BCR顺序提取法测定分析了上海水源地沉积物中Cr，Cu、Pb、Zn、Cd、Co、Ni六种元素的形态分布特征。结果表明：①上覆水中上述重金属含量未超过生活饮用水水质标准，符合地表水Ⅱ类水质标准。②沉积物中上述重金属总量分析表明：排污口及邻近地区重金属污染相对严重；港口地区重金属污染严重；河流下游比上游污染严重。③沉积物重金属形态分析表明：黄浦江水从上游淀峰流往下游吴淞口处的过程中，沿途受到重金属的污染，并且增加的重金属多以环境不稳定的形态(如酸溶态和可还原态)存在，它们在水体环境发生变化时，就有可能溶解、置换而释放入水体，给环境造成不可忽视的威胁。
随后以黄浦江沉积物为研究对象，研究了黄浦江沉积物对重金属吸附动力学及黄浦江沉积物砷释放的规律。结果表明：①黄浦江沉积物对重金属Cd，Pb，Cu，Zn及As(V)都具有较强的吸附能力，对重金属优先选择吸附的顺序为：Pb＞Cu＞Zn≈Cd＞As(V)；黄浦江沉积物与As(V)的结合强度随时间延长而不断增大，并且黄浦江沉积物对As(V)吸附表面的非均相程度非常高。②扰动、温度升高有利于As(V)的释放；As(V)的释放随pH的变化呈现“V”字形，pH增大和降低都有利于As(V)的释放，在pH5附近，As(V)释放量最低；PO_4~(3-)和HCO_3~-对As(V)的释放影响极为明显，As(V)释放量随溶液中PO_4~(3-)和HCO_3~-浓度的增大而增大。
第二部分：
通过苯乙烯、丙烯酸和环氧树脂类的对比筛选，选择了弱碱性环氧树脂331，分别系统研究了该树脂对Cu~(2+)，Cd~(2+)及Cr(Ⅴ)的去除效果及动力学吸附行为。同时，通过模拟实际受污染水体，探讨了在Cu~(2+)、Cd~(2+)、Cr(Ⅵ)共存的体系中，弱碱性阴离子树脂331去除重金属的作用规律及相关的机理。论文还就弱碱性阴离子交换树脂对As(Ⅴ)的吸附去除能力进行了初步探讨。结果表明：①环氧系弱碱性阴离子交换树脂对重金属具有更高的选择性，能够在高背景的碱金属和碱土金属离子共存下实现水体中微量重金属污染离子的高效分离。②在痕量的浓度水平及近中性的pH值范围内，331弱碱性环氧阴离子交换树脂对Cu~(2+)，Cd~(2+)及Cr(Ⅴ)具有较好的选择性去除效果，最大吸附容量分别为84.03，44.58和77.52mg／g；其中对Cu~(2+)和Cd~(2+)的去除主要是通过表面络合作用；对Cr(Ⅵ)的去除不仅有离子交换作用，同时还有表面络合作用，且离子交换速率快于表面络合速率。③当Cr(Ⅵ)存在于多种重金属共存的体系中时，弱碱性阴离子优先吸附Cr(Ⅵ)，并大大降低了对其他几种重金属离子的吸附。因此，如果在利用弱碱性阴离子树脂处理Cu~(2+)、Ni~(2+)、Co~(2+)、pb~(2+)、Mn~(2+)、Cd~(2+)等重金属阳离子时，必须要考虑到Cr(Ⅵ)(CrO_4~(2-)及HCrO_4~-)的竞争吸附影响。④SO_4~(2-)的存在显著降低弱碱性阴离子交换树脂对As(Ⅴ)的去除效果。
第三部分：
选择两类铁矿α-FeOOH(针铁矿)和β-FeOOH(四方纤铁矿)以及自然界存在最为广泛的δ-MnO_2(水钠锰矿)，深入研究了它们对重金属和As(Ⅴ)的吸附性能，并对吸附机理作了相关探讨。结果发现：①α-FeO(OH)、β-FeO(OH)均可以在自然水体pH范围有效吸附Cr(Ⅵ)，吸附速度快，最大吸附容量分别为50.25mg／g和42.02mg／g；②α-FeO(OH)和β-FeO(OH)均能够有效吸附水体中的As(Ⅴ)，其最佳pH范围分别为pH5～6.5和pH3.5～7，最大吸附量分别为5.05 mg／g和23.42 mg／g；③四种方法合成的δ-MnO_2均能将初始浓度约为1mg／L的重金属Zn，Pb，Cd，Ni，Cu和Co的含量降低到饮用水安全标准值范围；四种方法合成的δ-MnO_2对重金属的吸附动力学、吸附容量均有所差异，这可能是四种方法合成的δ-MnO_2微观结构不同而造成的，具有进一步深入探讨的价值。④四种方法合成的δ-MnO_2对As(Ⅴ)的吸附能力大小有如下顺序：δ-MnO_2(KMnO_4+MnSO_4)＞δ-MnO_2(KMnO_4+MnCl_2)＞δ-MnO_2(KMnO_4+HCl)＞δ-MnO_2(KMnO_4+Mn(NO_3)_2)。
第四部分：
主要研究将铁锰粉末材料负载到较大颗粒载体树脂上、制备容易实现固液分离的复合吸附剂R-MnO_2(MnO_2负载树脂D301)及RFM(铁锰氧化物负载树脂D301)，并研究了它们对重金属及砷的去除效果。结果发现：①所制备的吸附剂R-MnO_2能够在较广泛pH值范围(pH3～8)有效去除饮用水体中微量重金属，是
一种微污染源水中微量重金属的有效吸附剂；R-MnO_2对Zn~(2+)，Cd~(2+)，Cu~(2+)，Co~(2
+)和Ni~(2+)的最大吸附容量分别为78.13，63.69，131.58，68.49，55.25mg／g，吸附
能力顺序：Cu~(2+)＞Zn~(2+)，Cd~(2+)，Co~(2+)＞Ni~(2+)；吸附重金属后的R-MnO_2可以用0.05
mol／L的HNO_3有效洗脱再生。②所制备的吸附剂R-MnO_2可以在酸性条件下(pH
≈2)有效吸附水体中As(V)，吸附速度快，尤其是对低浓度As(V)(1mg／L左右)，
吸附率接近100％；预测R-MnO_2吸附As(V)是特性吸附、非特性吸附及沉淀与
共沉淀效应的共同结果。③所制备的吸附剂RFM可以在广泛的pH范围(pH4～
9)有效吸附水体中As(V)，吸附率接近100％；IR和XRD表征RFM发现其
表面有丰富的羟基，预测RFM吸附As(V)是非特性吸附和特性吸附作用的共同
结果，配位交换的专性吸附是主要吸附方式。
Aiming at the recent development trend of remediation technologies for water sources contaminated with slight pollution of heavy metals, this dissertation has put forward three remediation schemes based on the situation of Shanghai water resource. These three schemes include Weak base anion exchange resin remediation technique, iron & manganese mineral remediation technique, and loaded adsorbent remediation technique. Adopting modern analytical and test technologies, that included FTIR、 SEM、XRD and so on, the optimized conditions and possible mechanisms of the separation processes of heavy metals were investigated for these technologies. Under the support of Key Project of Ministry of Science and Technology, the purpose of this paper is to provide technical and theoretical suggestions and support for the efficient remediation of water sources with slight heavy metals pollution, it will also be benefit for dealing with the emergency affairs of heavy metal pollution in water sources.
This paper consists of four parts. ( I) Mobility and release of several heavy metals and arsenic between the sediment and the water (II) Study on the separation of several heavy metals and arsenic in the slight-polluted water by Weak base anion exchange resin (III) Study on the adsorption of several heavy metals and arsenic by mineral material such as α -FeO(OH)、β -FeO(OH) and δ -MnO_2 (IV) Study on the adsorption of several heavy metals and arsenic by loaded adsorbents such as R-MnC>2 and RFM.
( I ) In the first part of the dissertation, the background investigation was carried out to know the content of heavy metals in the overlaying water and surface layer sediments from Shanghai drinking water sources. Then BCR sequential extraction method was employed to analyze the distribution characteristics of heavy metals including Cr, Cu, Pb, Zn, Cd, Co and Ni in the sediments. The obtained experimental results showed :
① The contents of heavy metals from overlaying water were not beyond the domestic drinking water standard, they can meet the second class water quality for surface water.
② According to the data of heavy metals in sediments: The heavy metals pollution at the discharge location and their adjacent areas were more serious than other locations. The heavy metals pollution at the port area was very serious. The heavy metals pollution at the downriver area was more serious than that of upriver area.
③The distribution state of heavy metals in Huangpu river made it clear that the Huangpu river was contaminated by heavy metals when it flows from upriver area Dianfeng to downriver area Wusongkou, and the increased concentration of heavy metals was mainly caused by acid soluble fraction, which may endanger the total environment.
Subsequently, the Huangpu river was selected for further study, the adsorption dynamics of heavy metals and Arsenic release between the sediment and the surface water was investigated. The following conclusions were given out from the experimental results.
The surface sediments have strong affinity capacity for heavy metals such as Cu, Pb, Zn, Cd, and As. The affinitiy sequence was Pb＞Cu＞Zn≈Cd＞As(Ⅴ). The affinity capacity was increasing with the extension of reaction time. The extent of heterogeneous of sorption sites was high.
The increase of the vibration and the temperature could facilitate the discharge of As(Ⅴ) from the sediment. With the increase or the decrease of pH, the discharge amount of As(Ⅴ) will increase, and at the range of pH 5, the discharge amount was the lowest. The presence of PO_4~(3-) HCO_3~- could affect the discharge process greatly, and the discharge amount of As(Ⅴ) increased with the increment of PO_4~(3-) or HCO_3~- concentrations.
(Ⅱ) In the second part of this paper, through the comparative investigation among the styrene resin, acrylic acid resin and epoxide resin, we selected Weak base anion exchange resin 331 as adsorbent to study the adsorption behaviors of Cu(Ⅱ), Cd(Ⅱ), and Cr(Ⅵ) on it respectively. Furthermore, with weak base anion exchange resin 331, batch systems were investigated through simulating the actual polluted water in which Cu~(2+), Cd~(2+), Cr(Ⅵ) were co-existed in aqueous solution. At last, elementary study on the adsorption of the Arsenic(Ⅴ) were also carried out. The experimental results showed:
①Weak base anion-exchange resin is capable of selectively removing heavy metals from high concentrations of co-existed alkaline and alkaline earth metals through complexing action.
②The maximum amounts of metals adsorbed by weak base anion exchange resin 331were 44.58, 84.03 and 77.52 mg/g for Cd~(2+), Cu~(2+), and Cr(Ⅵ) respectively. For the removal process of Cu~2 and Cd~(2+), it based on the complexing action. For Cr(Ⅵ), the removal was associated with the ion-exchange and compexing action, and the rate for ion exchange was faster than that for complexing action.
③The adsorption behaviors of heavy metals onto 331 weak base anion-exchange resin were strongly influenced by the presence of competing ions in the solution. When Cr(Ⅵ) is co-existing with other heavy metals, the weak base anion-exchange resin had a preferred adsorption of Cr(Ⅵ), which led to the fewer adsorption for other heavy metal ions. Hence, if the weak base anion-exchange resin is applied to treat the heavy metals like Cu~(2+), Ni~(2+), Co~(2+), Pb~(2+), Mn~(2+), Cd~(2+) and so on, the competitive adsorption of Cr(Ⅵ) (CrO_4~(2-) and HCrO_4~-) must be considered.
④the presence of SO_4~(2-) caused the interference in the removal of As(Ⅴ) by weak base anion-exchange resin 331.
(Ⅲ) In the third part of this paper,α-FeOOH,β-FeOOH (goethite and lepidocrote) andδ-MnO_2 were synthesized for the further research. Batch experiments of adsorption were conducted to study the removal efficiency of heavy metals and arsenic from aqueous solutions. The behaviors and the possible mechanisms for As(Ⅴ) removal were discussed. The results showed:
①Cr(Ⅵ) can be efficiently removed byα- FeO(OH) andβ- FeO(OH) within the natural water source pH range. The adsorption process follows Langmuir and Freundlich isotherm models, the maximal capacity were 50.25mg/g and 42.02mg/g, respectively. The adsorption capacity of Cr(Ⅵ) decreased with the increment of ion strength, the existence of HCO_3~- or H_2PO_4~- decreased the adsorption capacity by about 20%.
②As(Ⅴ) can be efficiently removed byα- FeO(OH) andβ- FeO(OH), the optimal pH range were pH 5～6.5 and pH 3.5～7, respectively. The maximal adsorption capacities were 5.05 mg/g and 23.42 mg/g respectively.
③δ-MnO_2 synthesized by four different methods had the capacity to reduce the contents of Zn, Pb, Cd, Ni, Cu, Co in water solution to meet the drinking water quality standard when the initial heavy metal concentration was 1mg/L. Four types ofδ-MnO_2 had the different adsorption kinetics and capacities, which might result from the different micro-surface structures.
④The sequence of adsorption capacity wasδ-MnO_2 (KMnO_4+MnSO_4)＞δ-MnO2 (KMnO_4+MnCl_2)＞δ-MnO_2 (KMnO_4+ HCl)＞δ-MnO_2 ( KMnO_4 +Mn(NO_3)_2. The adsorption kinetics for As(Ⅴ) were similar, the results meant that chemical reaction might be the principal control procedure and the it could be described by pseudo-second order rate equation.
(Ⅳ) In the last part, loaded absorbent R-MnO_2 and RFM was synthesized by loading manganese (hydr)oxides and/or iron (hydr)oxides on weak basic anion exchange resin D301. Batch experiments of adsorption were conducted to study the removal of heavy metals and Arsenic from aqueous solutions.
①The loaded adsorbent R-MnO_2 showed a high capacity for the removal of trace amount of heavy metals such as Cu~(2+), Co~(2+) Zn~(2+) and Ni~(2+) with the coexistence of high concentration of alkali and alkaline-earth metal ions at the wide range of pH 3-8. The maximum removal capacity was 78.13, 63.69, 129.87, 67.11 and 54.64mg/g for Zn~(2+), Cd~(2+), Cu~(2+), Co~(2+) and Ni~(2+) respectively. The sequence of adsorption capacity was Cu~(2+)＞Zn~(2+), Cd~(2+), Co~(2+)＞Ni~(2+). With 0.05mol/L HNO_3, R-MnO_2 could be regenerated to the efficiency of 80%. The IR and XRD analysis results indicated that the metal oxide loaded on the D301 resin was the mixture ofδ-MnO_2 and MnO(OH). The high removal efficiency of heavy metals on R-MnO_2 was mainly due to the specific adsorption via surface hydroxide complexation reaction.
②The loaded adsorbent R-MnO_2 can be used as an efficient adsorbent for the removal of As(Ⅴ) from aqueous solution at pH=2. In the case of water samples contaminated by low As(Ⅴ) concentration, the removal rate can reach almost 100%. Arsenic adsorption by R-MnO_2 decreased with the increase of ion strength, the presence of PO_4~(3-) or HCO_3~- inhibited the arsenic adsorption. The adsorption process followed pseudo second-order kinetics. The arsenic removal was supposed as the common results of specified adsorption, non-specified adsorption, precipitation and co-precipitation.
③The loaded adsorbent RFM can be used as an efficient absorbent for the removal of As(Ⅴ) from aqueous solution in a wide pH range 4-9. In the case of water solution contaminated with low As(Ⅴ) concentration, the removal rate can reach almost 100%. Arsenic adsorption by RFM decreased with the increment of ion strength, the presence of PO_4~(3-), HCO_3~- inhibited the arsenic adsorption process. The IR analysis results indicate that the surface of RFM has rich hydroxyl groups. The arsenic removal was supposed as the common results of electrostatic adsorption and ligand exchange reactions, and the ligand exchange reactions are the main sorption mode.
论文主要分为四个部分。(Ⅰ)微污染水体沉积物中重金属及砷的迁移转化规律研究；(Ⅱ)弱碱性阴离子交换树脂对微污染水源中重金属及砷的分离过程研究；(Ⅲ)铁锰氧化物吸附剂分离水体中重金属及砷的研究；(Ⅳ)负载吸附剂去除水体中重金属及砷的研究。
第一部分：
首先对上海水源地(包括上覆水和沉积物)中重金属作了背景调查，并利用BCR顺序提取法测定分析了上海水源地沉积物中Cr，Cu、Pb、Zn、Cd、Co、Ni六种元素的形态分布特征。结果表明：①上覆水中上述重金属含量未超过生活饮用水水质标准，符合地表水Ⅱ类水质标准。②沉积物中上述重金属总量分析表明：排污口及邻近地区重金属污染相对严重；港口地区重金属污染严重；河流下游比上游污染严重。③沉积物重金属形态分析表明：黄浦江水从上游淀峰流往下游吴淞口处的过程中，沿途受到重金属的污染，并且增加的重金属多以环境不稳定的形态(如酸溶态和可还原态)存在，它们在水体环境发生变化时，就有可能溶解、置换而释放入水体，给环境造成不可忽视的威胁。
随后以黄浦江沉积物为研究对象，研究了黄浦江沉积物对重金属吸附动力学及黄浦江沉积物砷释放的规律。结果表明：①黄浦江沉积物对重金属Cd，Pb，Cu，Zn及As(V)都具有较强的吸附能力，对重金属优先选择吸附的顺序为：Pb＞Cu＞Zn≈Cd＞As(V)；黄浦江沉积物与As(V)的结合强度随时间延长而不断增大，并且黄浦江沉积物对As(V)吸附表面的非均相程度非常高。②扰动、温度升高有利于As(V)的释放；As(V)的释放随pH的变化呈现“V”字形，pH增大和降低都有利于As(V)的释放，在pH5附近，As(V)释放量最低；PO_4~(3-)和HCO_3~-对As(V)的释放影响极为明显，As(V)释放量随溶液中PO_4~(3-)和HCO_3~-浓度的增大而增大。
第二部分：
通过苯乙烯、丙烯酸和环氧树脂类的对比筛选，选择了弱碱性环氧树脂331，分别系统研究了该树脂对Cu~(2+)，Cd~(2+)及Cr(Ⅴ)的去除效果及动力学吸附行为。同时，通过模拟实际受污染水体，探讨了在Cu~(2+)、Cd~(2+)、Cr(Ⅵ)共存的体系中，弱碱性阴离子树脂331去除重金属的作用规律及相关的机理。论文还就弱碱性阴离子交换树脂对As(Ⅴ)的吸附去除能力进行了初步探讨。结果表明：①环氧系弱碱性阴离子交换树脂对重金属具有更高的选择性，能够在高背景的碱金属和碱土金属离子共存下实现水体中微量重金属污染离子的高效分离。②在痕量的浓度水平及近中性的pH值范围内，331弱碱性环氧阴离子交换树脂对Cu~(2+)，Cd~(2+)及Cr(Ⅴ)具有较好的选择性去除效果，最大吸附容量分别为84.03，44.58和77.52mg／g；其中对Cu~(2+)和Cd~(2+)的去除主要是通过表面络合作用；对Cr(Ⅵ)的去除不仅有离子交换作用，同时还有表面络合作用，且离子交换速率快于表面络合速率。③当Cr(Ⅵ)存在于多种重金属共存的体系中时，弱碱性阴离子优先吸附Cr(Ⅵ)，并大大降低了对其他几种重金属离子的吸附。因此，如果在利用弱碱性阴离子树脂处理Cu~(2+)、Ni~(2+)、Co~(2+)、pb~(2+)、Mn~(2+)、Cd~(2+)等重金属阳离子时，必须要考虑到Cr(Ⅵ)(CrO_4~(2-)及HCrO_4~-)的竞争吸附影响。④SO_4~(2-)的存在显著降低弱碱性阴离子交换树脂对As(Ⅴ)的去除效果。
第三部分：
选择两类铁矿α-FeOOH(针铁矿)和β-FeOOH(四方纤铁矿)以及自然界存在最为广泛的δ-MnO_2(水钠锰矿)，深入研究了它们对重金属和As(Ⅴ)的吸附性能，并对吸附机理作了相关探讨。结果发现：①α-FeO(OH)、β-FeO(OH)均可以在自然水体pH范围有效吸附Cr(Ⅵ)，吸附速度快，最大吸附容量分别为50.25mg／g和42.02mg／g；②α-FeO(OH)和β-FeO(OH)均能够有效吸附水体中的As(Ⅴ)，其最佳pH范围分别为pH5～6.5和pH3.5～7，最大吸附量分别为5.05 mg／g和23.42 mg／g；③四种方法合成的δ-MnO_2均能将初始浓度约为1mg／L的重金属Zn，Pb，Cd，Ni，Cu和Co的含量降低到饮用水安全标准值范围；四种方法合成的δ-MnO_2对重金属的吸附动力学、吸附容量均有所差异，这可能是四种方法合成的δ-MnO_2微观结构不同而造成的，具有进一步深入探讨的价值。④四种方法合成的δ-MnO_2对As(Ⅴ)的吸附能力大小有如下顺序：δ-MnO_2(KMnO_4+MnSO_4)＞δ-MnO_2(KMnO_4+MnCl_2)＞δ-MnO_2(KMnO_4+HCl)＞δ-MnO_2(KMnO_4+Mn(NO_3)_2)。
第四部分：
主要研究将铁锰粉末材料负载到较大颗粒载体树脂上、制备容易实现固液分离的复合吸附剂R-MnO_2(MnO_2负载树脂D301)及RFM(铁锰氧化物负载树脂D301)，并研究了它们对重金属及砷的去除效果。结果发现：①所制备的吸附剂R-MnO_2能够在较广泛pH值范围(pH3～8)有效去除饮用水体中微量重金属，是
一种微污染源水中微量重金属的有效吸附剂；R-MnO_2对Zn~(2+)，Cd~(2+)，Cu~(2+)，Co~(2
+)和Ni~(2+)的最大吸附容量分别为78.13，63.69，131.58，68.49，55.25mg／g，吸附
能力顺序：Cu~(2+)＞Zn~(2+)，Cd~(2+)，Co~(2+)＞Ni~(2+)；吸附重金属后的R-MnO_2可以用0.05
mol／L的HNO_3有效洗脱再生。②所制备的吸附剂R-MnO_2可以在酸性条件下(pH
≈2)有效吸附水体中As(V)，吸附速度快，尤其是对低浓度As(V)(1mg／L左右)，
吸附率接近100％；预测R-MnO_2吸附As(V)是特性吸附、非特性吸附及沉淀与
共沉淀效应的共同结果。③所制备的吸附剂RFM可以在广泛的pH范围(pH4～
9)有效吸附水体中As(V)，吸附率接近100％；IR和XRD表征RFM发现其
表面有丰富的羟基，预测RFM吸附As(V)是非特性吸附和特性吸附作用的共同
结果，配位交换的专性吸附是主要吸附方式。
Aiming at the recent development trend of remediation technologies for water sources contaminated with slight pollution of heavy metals, this dissertation has put forward three remediation schemes based on the situation of Shanghai water resource. These three schemes include Weak base anion exchange resin remediation technique, iron & manganese mineral remediation technique, and loaded adsorbent remediation technique. Adopting modern analytical and test technologies, that included FTIR、 SEM、XRD and so on, the optimized conditions and possible mechanisms of the separation processes of heavy metals were investigated for these technologies. Under the support of Key Project of Ministry of Science and Technology, the purpose of this paper is to provide technical and theoretical suggestions and support for the efficient remediation of water sources with slight heavy metals pollution, it will also be benefit for dealing with the emergency affairs of heavy metal pollution in water sources.
This paper consists of four parts. ( I) Mobility and release of several heavy metals and arsenic between the sediment and the water (II) Study on the separation of several heavy metals and arsenic in the slight-polluted water by Weak base anion exchange resin (III) Study on the adsorption of several heavy metals and arsenic by mineral material such as α -FeO(OH)、β -FeO(OH) and δ -MnO_2 (IV) Study on the adsorption of several heavy metals and arsenic by loaded adsorbents such as R-MnC>2 and RFM.
( I ) In the first part of the dissertation, the background investigation was carried out to know the content of heavy metals in the overlaying water and surface layer sediments from Shanghai drinking water sources. Then BCR sequential extraction method was employed to analyze the distribution characteristics of heavy metals including Cr, Cu, Pb, Zn, Cd, Co and Ni in the sediments. The obtained experimental results showed :
① The contents of heavy metals from overlaying water were not beyond the domestic drinking water standard, they can meet the second class water quality for surface water.
② According to the data of heavy metals in sediments: The heavy metals pollution at the discharge location and their adjacent areas were more serious than other locations. The heavy metals pollution at the port area was very serious. The heavy metals pollution at the downriver area was more serious than that of upriver area.
③The distribution state of heavy metals in Huangpu river made it clear that the Huangpu river was contaminated by heavy metals when it flows from upriver area Dianfeng to downriver area Wusongkou, and the increased concentration of heavy metals was mainly caused by acid soluble fraction, which may endanger the total environment.
Subsequently, the Huangpu river was selected for further study, the adsorption dynamics of heavy metals and Arsenic release between the sediment and the surface water was investigated. The following conclusions were given out from the experimental results.
The surface sediments have strong affinity capacity for heavy metals such as Cu, Pb, Zn, Cd, and As. The affinitiy sequence was Pb＞Cu＞Zn≈Cd＞As(Ⅴ). The affinity capacity was increasing with the extension of reaction time. The extent of heterogeneous of sorption sites was high.
The increase of the vibration and the temperature could facilitate the discharge of As(Ⅴ) from the sediment. With the increase or the decrease of pH, the discharge amount of As(Ⅴ) will increase, and at the range of pH 5, the discharge amount was the lowest. The presence of PO_4~(3-) HCO_3~- could affect the discharge process greatly, and the discharge amount of As(Ⅴ) increased with the increment of PO_4~(3-) or HCO_3~- concentrations.
(Ⅱ) In the second part of this paper, through the comparative investigation among the styrene resin, acrylic acid resin and epoxide resin, we selected Weak base anion exchange resin 331 as adsorbent to study the adsorption behaviors of Cu(Ⅱ), Cd(Ⅱ), and Cr(Ⅵ) on it respectively. Furthermore, with weak base anion exchange resin 331, batch systems were investigated through simulating the actual polluted water in which Cu~(2+), Cd~(2+), Cr(Ⅵ) were co-existed in aqueous solution. At last, elementary study on the adsorption of the Arsenic(Ⅴ) were also carried out. The experimental results showed:
①Weak base anion-exchange resin is capable of selectively removing heavy metals from high concentrations of co-existed alkaline and alkaline earth metals through complexing action.
②The maximum amounts of metals adsorbed by weak base anion exchange resin 331were 44.58, 84.03 and 77.52 mg/g for Cd~(2+), Cu~(2+), and Cr(Ⅵ) respectively. For the removal process of Cu~2 and Cd~(2+), it based on the complexing action. For Cr(Ⅵ), the removal was associated with the ion-exchange and compexing action, and the rate for ion exchange was faster than that for complexing action.
③The adsorption behaviors of heavy metals onto 331 weak base anion-exchange resin were strongly influenced by the presence of competing ions in the solution. When Cr(Ⅵ) is co-existing with other heavy metals, the weak base anion-exchange resin had a preferred adsorption of Cr(Ⅵ), which led to the fewer adsorption for other heavy metal ions. Hence, if the weak base anion-exchange resin is applied to treat the heavy metals like Cu~(2+), Ni~(2+), Co~(2+), Pb~(2+), Mn~(2+), Cd~(2+) and so on, the competitive adsorption of Cr(Ⅵ) (CrO_4~(2-) and HCrO_4~-) must be considered.
④the presence of SO_4~(2-) caused the interference in the removal of As(Ⅴ) by weak base anion-exchange resin 331.
(Ⅲ) In the third part of this paper,α-FeOOH,β-FeOOH (goethite and lepidocrote) andδ-MnO_2 were synthesized for the further research. Batch experiments of adsorption were conducted to study the removal efficiency of heavy metals and arsenic from aqueous solutions. The behaviors and the possible mechanisms for As(Ⅴ) removal were discussed. The results showed:
①Cr(Ⅵ) can be efficiently removed byα- FeO(OH) andβ- FeO(OH) within the natural water source pH range. The adsorption process follows Langmuir and Freundlich isotherm models, the maximal capacity were 50.25mg/g and 42.02mg/g, respectively. The adsorption capacity of Cr(Ⅵ) decreased with the increment of ion strength, the existence of HCO_3~- or H_2PO_4~- decreased the adsorption capacity by about 20%.
②As(Ⅴ) can be efficiently removed byα- FeO(OH) andβ- FeO(OH), the optimal pH range were pH 5～6.5 and pH 3.5～7, respectively. The maximal adsorption capacities were 5.05 mg/g and 23.42 mg/g respectively.
③δ-MnO_2 synthesized by four different methods had the capacity to reduce the contents of Zn, Pb, Cd, Ni, Cu, Co in water solution to meet the drinking water quality standard when the initial heavy metal concentration was 1mg/L. Four types ofδ-MnO_2 had the different adsorption kinetics and capacities, which might result from the different micro-surface structures.
④The sequence of adsorption capacity wasδ-MnO_2 (KMnO_4+MnSO_4)＞δ-MnO2 (KMnO_4+MnCl_2)＞δ-MnO_2 (KMnO_4+ HCl)＞δ-MnO_2 ( KMnO_4 +Mn(NO_3)_2. The adsorption kinetics for As(Ⅴ) were similar, the results meant that chemical reaction might be the principal control procedure and the it could be described by pseudo-second order rate equation.
(Ⅳ) In the last part, loaded absorbent R-MnO_2 and RFM was synthesized by loading manganese (hydr)oxides and/or iron (hydr)oxides on weak basic anion exchange resin D301. Batch experiments of adsorption were conducted to study the removal of heavy metals and Arsenic from aqueous solutions.
①The loaded adsorbent R-MnO_2 showed a high capacity for the removal of trace amount of heavy metals such as Cu~(2+), Co~(2+) Zn~(2+) and Ni~(2+) with the coexistence of high concentration of alkali and alkaline-earth metal ions at the wide range of pH 3-8. The maximum removal capacity was 78.13, 63.69, 129.87, 67.11 and 54.64mg/g for Zn~(2+), Cd~(2+), Cu~(2+), Co~(2+) and Ni~(2+) respectively. The sequence of adsorption capacity was Cu~(2+)＞Zn~(2+), Cd~(2+), Co~(2+)＞Ni~(2+). With 0.05mol/L HNO_3, R-MnO_2 could be regenerated to the efficiency of 80%. The IR and XRD analysis results indicated that the metal oxide loaded on the D301 resin was the mixture ofδ-MnO_2 and MnO(OH). The high removal efficiency of heavy metals on R-MnO_2 was mainly due to the specific adsorption via surface hydroxide complexation reaction.
②The loaded adsorbent R-MnO_2 can be used as an efficient adsorbent for the removal of As(Ⅴ) from aqueous solution at pH=2. In the case of water samples contaminated by low As(Ⅴ) concentration, the removal rate can reach almost 100%. Arsenic adsorption by R-MnO_2 decreased with the increase of ion strength, the presence of PO_4~(3-) or HCO_3~- inhibited the arsenic adsorption. The adsorption process followed pseudo second-order kinetics. The arsenic removal was supposed as the common results of specified adsorption, non-specified adsorption, precipitation and co-precipitation.
③The loaded adsorbent RFM can be used as an efficient absorbent for the removal of As(Ⅴ) from aqueous solution in a wide pH range 4-9. In the case of water solution contaminated with low As(Ⅴ) concentration, the removal rate can reach almost 100%. Arsenic adsorption by RFM decreased with the increment of ion strength, the presence of PO_4~(3-), HCO_3~- inhibited the arsenic adsorption process. The IR analysis results indicate that the surface of RFM has rich hydroxyl groups. The arsenic removal was supposed as the common results of electrostatic adsorption and ligand exchange reactions, and the ligand exchange reactions are the main sorption mode.
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