铜阳极泥中碲的回收与提纯及其基础理论研究
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摘要
碲被誉为“工业的维生素,现代高新技术的桥梁”,在材料领域发挥着越来越重要的作用。由于其资源缺乏,如何经济高效地分离、回收碲并制备高纯碲,正成为人们关注的焦点。目前碲主要来源于铜阳极泥,研究铜阳极泥中碲的回收与提纯具有重要的价值与现实意义。本文以铜阳极泥为原料,发明了硫酸预浸分铜-碳酸钠转化脱铅-硫酸焙烧蒸硒-盐酸浸碲铋、催化还原法回收碲、化学法提纯等新工艺提取、回收碲并制备高纯碲,并对卤素催化还原硫酸溶液中Te(Ⅳ)的机理和碲提纯过程中的热力学进行了研究。
首先铜阳极泥经过硫酸预浸分铜,得到分铜液。当反应温度为80℃、硫酸与物料中铜物质的量之比为1.5：1、液固比为3：1、反应时间为1.5h时,铜浸出率为89.5%、碲浸出率为20.4%。
分铜阳极泥与Na2C03混和湿磨后,过滤除去硫酸根,随后阳极泥中的铅用硝酸除去。当Na2C03与分铜阳极泥中铅物质的量之比为2.5：1、液固比为2：1、球料比为8：1、反应时间为3h时,对阳极泥进行碳酸钠转化,分离硫酸根后用硝酸浸出,当硝酸与铅物质的量之比为6：1时,铅去除率为70%。
分铅阳极泥与浓硫酸混匀后焙烧,对硒进行分离。当硫酸与物料中硒碲物质的量之比为1.2：1、反应温度为680℃、反应时间为3h时,硒去除率达到95%。
分硒阳极泥用盐酸浸出碲,得到盐酸浸碲液。当盐酸浓度为6mol.L-1、液固比为3：1、反应温度为80℃、反应时间为2h时,铜阳极泥中碲总浸出率为93.6%,贵金属金银得到富集,金由0.152%上升到0.34%,银由7.81%上升到14.34%。
硫酸预浸分铜液经蒸发结晶后,得到常温结晶母液。母液中的硒通过S02或Na2S03还原分离。当反应温度为80℃、硫酸浓度为240g·L-1、SO2流量为35ml·min-1、反应时间为2h时,用SO2从2L硫酸铜结晶母液分离硒,硒回收率为96.50%,碲沉淀率仅为1.05%。分硒后溶液通过C1-催化-SO2还原,碲回收率为99.60%。
硫酸预浸分铜液通过深度蒸发结晶脱铜,获得高浓度硫酸结晶母液,其硫酸浓度为880g·L-1-1000g·L-1。通过卤素催化SO2还原回收高浓度硫酸结晶母液中的碲。当反应温度为85℃、硫酸浓度为880g·L-1、Cl-浓度为0.5mol·L-1、SO2流量40L-h-1、反应时间为2h时,碲的回收率为99.25%。5m3的工业实验表明,碲回收率为98.32%,固体产物中碲、铜和氯的质量分数分别为51.10%、27.35%和13.68%。XRD结果表明,产物为单质碲和氯化亚铜的混和物。
通过硫脲配合浸出、双氧水氧化-硫酸浸出、硝酸氧化浸出三种方法的对比,选择硝酸氧化浸出法分离碲铜渣中的碲和铜。按Cu2C12生成CuCl2和Cu(NO3)2、Te生成TeO2、起氧化作用的HNO3生成NO2进行计算,当硝酸用量为理论用量的0.96倍时,铜去除率为97.50%、碲浸出率为1.05%,铜与碲得到有效分离,碲转化为TeO2。
分铜后的碲渣通过两次氧化-盐酸浸出、预还原除硒,还原得到碲粉。碲粉在450℃和氢气气氛下处理,得到符合YS/T222-1996标准的4N+碲。
利用离子交换、紫外-可见分光光度、XRD、溶解度测定等手段对Cl-催化的机理进行了研究。研究表明,在低浓度硫酸溶液中Te(Ⅳ)以TeOOH+形式存在,硫酸浓度超过700g·L-1后,溶液中TeOOH4脱水缩合形成环状结构的Te2O3SO4,导致Te(Ⅳ)稳定性增强,难以被S02还原。Cl-可破坏高浓度硫酸溶液中Te2O3SO4的结构,随着溶液中Cl-浓度的增加,Te(Ⅳ)逐步向TeOCl2、TeCl4、H2TeCl6转化,Te(Ⅳ)的活性增强。Cl-催化反应动力学研究表明,当溶液中Cl-浓度为0.1mol·L-1时,其活化能为44.87kJ·mol-1;Cl-浓度为0.3mol·L-1时,其活化能为36.714kJ·mol-1.XRD表明,以Cl-和Br-为催化剂时产物为单质碲,以I-为催化剂时产物为Re4I4。
元素在提纯碲的不同阶段的分配率和除杂热力学分析表明,通过硝酸氧化硫酸浸出、预还原除硒、两次氧化浸出-SO2还原、氢气气氛和高温下处理碲粉,可以除去杂质获得高纯碲。当溶液中HCl不低于6mol·L-1时,碲粉中的铜、铅、锑、银等杂质与Cl-形成配合物,并与钙、镁、铝、铁等金属离子保留在滤液中。二次还原碲粉在450℃和氢气氛围下还原,砷以As4O6、硒以H2Se形式与碲分离。
与传统工艺相比,该提取碲的工艺具有转炉处理能力高,能耗、酸用量和烟气量低等优点。与传统回收碲的方法相比,卤素催化还原法具有回收成本低、碲品位高、物料易处理的特点。化学法制备高纯碲具有生产条件易控制、直收率高、成本低、产品质量稳定、易大规模化等优点。
Tellurium, which is called the vitamin of industry and the bridge of modern advanced technologies, plays more and more important role in material field. Much attention is paid on recovery of tellurium from tellurium-containing materials and preparation of high pure tellurium by a cheap and efficient method because its resource is scarce. Tellurium comes mainly from copper anode slime. It is very valuable to study on recovery and preparation of tellurium. A novel method is invented, which includes extraction and recovery of tellurium from copper anode slime by preleaching copper with H2SO4, deleading with Na2CO3, removing selenium by roasting de-lead anode slime mixed with concentrated sulfur acid, leaching tellurium and bismuth with HCl from roasted anode slime, reducing Te(IV) in leachate with SO2under the action of Cl-and purifying tellurium by chemical method. Reduction catalytic mechanism of halogens ion on Te(IV) in the H2SO4solution and thermodynamic analysis on removal of impurities during the purification are studied in this paper.
Firstly, copper-containing solution is obtained after preleaching copper anode slime with H2SO4. Leaching rate of copper and tellurium are89.5%and20.4%when reaction temperature is80℃, molar ratio of H2SO4to Cu in the material is1.5:1, ratio of liquid to solid is3:1and reaction time is1.5h.
Mixed with Na2CO3, de-copper anode slime is grinded for3h, PbSO4is transformed into PbCO3when molar ratio of Na2CO3to Pb in anode slime is2.5:1, ratio of liquid to solid is2:1, quality ratio of steel ball to anode slime is8:1. SO42-is removed by washing. Subsequently, lead is leached with HNO3. Leaching rate of lead is70%when molar ratio of HNO3to Pb in de-copper anode slime is6:1.
Se is removed by roasting after de-lead anode slime is mixed with concentrated sulfuric acid. Removal rate of Se reaches95%when molar rate of H2SO4to sum of both Se and Te is1.2:1, reaction temperature is680℃and reaction time is3h.
tellurium-containing leachate is obtained by leaching with HCl after removal of Se by vaporation. Total extracting rate of tellurium in copper anode slime is93.6%when concentration of HCl acid is6mol·L-1, rate of liquid to solid is3:1, reaction temperature is80℃and reaction time is2h. At the same time, some noble metals such as gold and sliver are enriched, contents of gold in anode slime increases from0.152%to0.34%, and sliver increases from7.81%to14.34%.
Crystallization mother solution is acquired by evaporating and crystallizing pre-leachate under normal temperature. Se in solution is separated beforehand by reduction with SO2. Removal rate of Se in the2L solution is96.50%and precipitation rate of tellurium is less than1.05%when reaction temperature is80℃, concentration of sulfur acid is240g·L-1, flow of SO2is35ml·min-1and reaction time is2h. Recovery rate of tellurium reaches99.60%under the action of Cl-and SO2after removal of selenium.
Crystallization mother solution, in which concentration of H2SO4is in the range of880g·L-1～1000g·L-1, is acquired after copper has been recovered from solution by deep evaporation. Tellurium in the crystallization mother solution is recovered under the action of Cl-and SO2, and its recovery rate reaches99.25%when reaction temperature is85℃, concentration of H2SO4is880g·L-1, concentration of Cl-is0.5mol·L-1, flow of SO2is40L·h-1and reaction time is2h. Result of5m3volume industrial experiment indicates that recovery rate of tellurium is98.32%, mass percents of Te, Cu and Cl in solid product are51.10%,27.35%and13.68%, respectively. XRD result shows that elemental tellurium and Cu2Cl2have existed in the product.
Compared with thiourea complexation leaching and oxidation with H2O2-leaching with sulfur acid, leaching with HNO3is chosen as a way to separate copper from tellurium in the Cu-Te residue. Stoichiometric dosage of HNO3can be calculated according to rules that Cu2Cl2is transformed into CuCl2and Cu(NO3)2, Te is transformed TeO2and HNO3playing oxidation role is transformed into NO2. Removal rate of copper reachs97.5%and leaching rate of tellurium is1.05%when dosage of HNO3is0.96time of stoichiometric dosage, and tellurium is tranformed into TeO2.
Powdered tellurium is obtained after Se has been removed beforehand and Te is treated twice by method of oxidation, leaching and reduction.Finally,4N+tellurium satisfied with standard of YS/T222-1996is acquired after powdered tellurium is treated under450℃and hydrogen ambient.
Catalytic mechanism of Cl-on reduction of Te (Ⅳ) is studied by means of methods such as ion-exchange, UV-VS spectrophotometry, XRD and determination of solubility. The results show that Te(IV) exists in form of TeOOH+when concentration of H2SO4in solution is less than700g·L-1, TeOOH+is gradually dehydrated and changed Te2O3SO4when concentration of H2SO4is over700g·L-1. Therefore, Te (Ⅳ) becomes more stable and more difficult to be reduced by SO2. Structure of Te2O3SO4in high concentration H2SO4solution is destroyed by Cl-, with the increasing of Cl-concentration,Te(Ⅳ) is transformed step by step into TeOCl2, TeCl4and H2TeCl6, and Te(IV) is getting more and more active. The study on catalytic kinetic of Cl-shows activation energy is44.87kJ·mol-1when Cl-concentration is0.1mol·L-1, and activation energy is36.714kJ·mol-1when Cl-concentration is0.3mol·L-1. XRD results confirm that product is elemental tellurium when Cl-and Br-are used as catalyst, the product is Tel (Te4I4) when I-is used as catalyst.
Distribute ratio of elements in the tellurium-containing residue during purification and thermodynamic analysis show that impurities can be removed efficiently and high pure tellurium can be obtained by oxidizing with HNO3and leaching with H2SO4, removing selenium beforehand, oxidizing-leaching-reducing and treating under hydrogen ambient and high temperature. Impurities such as Cu, Pb, Sb and Ag in powdered tellurium combine with Cl-to form complexes and are kept in the solution together with Ca, Al, Mg and Fe when concentration of HC1in solution is not less than6mol·L-1. Arsenic is evaporated in forms of As4O6, Se is removed in form of H2Se under450℃and hydrogen ambient.
Compared with traditional technologies, this technology on extracting tellurium has many advantages such as large treatment capacity of convert, low consumption of energy and acid, little flue gas volume. Contrasted to the traditional method in which precipitating tellurium with copper powder, the catalytic reduction method has its advantages such as low cost, high content of tellurium in the product and easy treatment. High pure tellurium is prepared by chemical method. This method has advantages such as easy control, low cost, high direct recovery rate, stable quality of product and large scale.
首先铜阳极泥经过硫酸预浸分铜,得到分铜液。当反应温度为80℃、硫酸与物料中铜物质的量之比为1.5：1、液固比为3：1、反应时间为1.5h时,铜浸出率为89.5%、碲浸出率为20.4%。
分铜阳极泥与Na2C03混和湿磨后,过滤除去硫酸根,随后阳极泥中的铅用硝酸除去。当Na2C03与分铜阳极泥中铅物质的量之比为2.5：1、液固比为2：1、球料比为8：1、反应时间为3h时,对阳极泥进行碳酸钠转化,分离硫酸根后用硝酸浸出,当硝酸与铅物质的量之比为6：1时,铅去除率为70%。
分铅阳极泥与浓硫酸混匀后焙烧,对硒进行分离。当硫酸与物料中硒碲物质的量之比为1.2：1、反应温度为680℃、反应时间为3h时,硒去除率达到95%。
分硒阳极泥用盐酸浸出碲,得到盐酸浸碲液。当盐酸浓度为6mol.L-1、液固比为3：1、反应温度为80℃、反应时间为2h时,铜阳极泥中碲总浸出率为93.6%,贵金属金银得到富集,金由0.152%上升到0.34%,银由7.81%上升到14.34%。
硫酸预浸分铜液经蒸发结晶后,得到常温结晶母液。母液中的硒通过S02或Na2S03还原分离。当反应温度为80℃、硫酸浓度为240g·L-1、SO2流量为35ml·min-1、反应时间为2h时,用SO2从2L硫酸铜结晶母液分离硒,硒回收率为96.50%,碲沉淀率仅为1.05%。分硒后溶液通过C1-催化-SO2还原,碲回收率为99.60%。
硫酸预浸分铜液通过深度蒸发结晶脱铜,获得高浓度硫酸结晶母液,其硫酸浓度为880g·L-1-1000g·L-1。通过卤素催化SO2还原回收高浓度硫酸结晶母液中的碲。当反应温度为85℃、硫酸浓度为880g·L-1、Cl-浓度为0.5mol·L-1、SO2流量40L-h-1、反应时间为2h时,碲的回收率为99.25%。5m3的工业实验表明,碲回收率为98.32%,固体产物中碲、铜和氯的质量分数分别为51.10%、27.35%和13.68%。XRD结果表明,产物为单质碲和氯化亚铜的混和物。
通过硫脲配合浸出、双氧水氧化-硫酸浸出、硝酸氧化浸出三种方法的对比,选择硝酸氧化浸出法分离碲铜渣中的碲和铜。按Cu2C12生成CuCl2和Cu(NO3)2、Te生成TeO2、起氧化作用的HNO3生成NO2进行计算,当硝酸用量为理论用量的0.96倍时,铜去除率为97.50%、碲浸出率为1.05%,铜与碲得到有效分离,碲转化为TeO2。
分铜后的碲渣通过两次氧化-盐酸浸出、预还原除硒,还原得到碲粉。碲粉在450℃和氢气气氛下处理,得到符合YS/T222-1996标准的4N+碲。
利用离子交换、紫外-可见分光光度、XRD、溶解度测定等手段对Cl-催化的机理进行了研究。研究表明,在低浓度硫酸溶液中Te(Ⅳ)以TeOOH+形式存在,硫酸浓度超过700g·L-1后,溶液中TeOOH4脱水缩合形成环状结构的Te2O3SO4,导致Te(Ⅳ)稳定性增强,难以被S02还原。Cl-可破坏高浓度硫酸溶液中Te2O3SO4的结构,随着溶液中Cl-浓度的增加,Te(Ⅳ)逐步向TeOCl2、TeCl4、H2TeCl6转化,Te(Ⅳ)的活性增强。Cl-催化反应动力学研究表明,当溶液中Cl-浓度为0.1mol·L-1时,其活化能为44.87kJ·mol-1;Cl-浓度为0.3mol·L-1时,其活化能为36.714kJ·mol-1.XRD表明,以Cl-和Br-为催化剂时产物为单质碲,以I-为催化剂时产物为Re4I4。
元素在提纯碲的不同阶段的分配率和除杂热力学分析表明,通过硝酸氧化硫酸浸出、预还原除硒、两次氧化浸出-SO2还原、氢气气氛和高温下处理碲粉,可以除去杂质获得高纯碲。当溶液中HCl不低于6mol·L-1时,碲粉中的铜、铅、锑、银等杂质与Cl-形成配合物,并与钙、镁、铝、铁等金属离子保留在滤液中。二次还原碲粉在450℃和氢气氛围下还原,砷以As4O6、硒以H2Se形式与碲分离。
与传统工艺相比,该提取碲的工艺具有转炉处理能力高,能耗、酸用量和烟气量低等优点。与传统回收碲的方法相比,卤素催化还原法具有回收成本低、碲品位高、物料易处理的特点。化学法制备高纯碲具有生产条件易控制、直收率高、成本低、产品质量稳定、易大规模化等优点。
Tellurium, which is called the vitamin of industry and the bridge of modern advanced technologies, plays more and more important role in material field. Much attention is paid on recovery of tellurium from tellurium-containing materials and preparation of high pure tellurium by a cheap and efficient method because its resource is scarce. Tellurium comes mainly from copper anode slime. It is very valuable to study on recovery and preparation of tellurium. A novel method is invented, which includes extraction and recovery of tellurium from copper anode slime by preleaching copper with H2SO4, deleading with Na2CO3, removing selenium by roasting de-lead anode slime mixed with concentrated sulfur acid, leaching tellurium and bismuth with HCl from roasted anode slime, reducing Te(IV) in leachate with SO2under the action of Cl-and purifying tellurium by chemical method. Reduction catalytic mechanism of halogens ion on Te(IV) in the H2SO4solution and thermodynamic analysis on removal of impurities during the purification are studied in this paper.
Firstly, copper-containing solution is obtained after preleaching copper anode slime with H2SO4. Leaching rate of copper and tellurium are89.5%and20.4%when reaction temperature is80℃, molar ratio of H2SO4to Cu in the material is1.5:1, ratio of liquid to solid is3:1and reaction time is1.5h.
Mixed with Na2CO3, de-copper anode slime is grinded for3h, PbSO4is transformed into PbCO3when molar ratio of Na2CO3to Pb in anode slime is2.5:1, ratio of liquid to solid is2:1, quality ratio of steel ball to anode slime is8:1. SO42-is removed by washing. Subsequently, lead is leached with HNO3. Leaching rate of lead is70%when molar ratio of HNO3to Pb in de-copper anode slime is6:1.
Se is removed by roasting after de-lead anode slime is mixed with concentrated sulfuric acid. Removal rate of Se reaches95%when molar rate of H2SO4to sum of both Se and Te is1.2:1, reaction temperature is680℃and reaction time is3h.
tellurium-containing leachate is obtained by leaching with HCl after removal of Se by vaporation. Total extracting rate of tellurium in copper anode slime is93.6%when concentration of HCl acid is6mol·L-1, rate of liquid to solid is3:1, reaction temperature is80℃and reaction time is2h. At the same time, some noble metals such as gold and sliver are enriched, contents of gold in anode slime increases from0.152%to0.34%, and sliver increases from7.81%to14.34%.
Crystallization mother solution is acquired by evaporating and crystallizing pre-leachate under normal temperature. Se in solution is separated beforehand by reduction with SO2. Removal rate of Se in the2L solution is96.50%and precipitation rate of tellurium is less than1.05%when reaction temperature is80℃, concentration of sulfur acid is240g·L-1, flow of SO2is35ml·min-1and reaction time is2h. Recovery rate of tellurium reaches99.60%under the action of Cl-and SO2after removal of selenium.
Crystallization mother solution, in which concentration of H2SO4is in the range of880g·L-1～1000g·L-1, is acquired after copper has been recovered from solution by deep evaporation. Tellurium in the crystallization mother solution is recovered under the action of Cl-and SO2, and its recovery rate reaches99.25%when reaction temperature is85℃, concentration of H2SO4is880g·L-1, concentration of Cl-is0.5mol·L-1, flow of SO2is40L·h-1and reaction time is2h. Result of5m3volume industrial experiment indicates that recovery rate of tellurium is98.32%, mass percents of Te, Cu and Cl in solid product are51.10%,27.35%and13.68%, respectively. XRD result shows that elemental tellurium and Cu2Cl2have existed in the product.
Compared with thiourea complexation leaching and oxidation with H2O2-leaching with sulfur acid, leaching with HNO3is chosen as a way to separate copper from tellurium in the Cu-Te residue. Stoichiometric dosage of HNO3can be calculated according to rules that Cu2Cl2is transformed into CuCl2and Cu(NO3)2, Te is transformed TeO2and HNO3playing oxidation role is transformed into NO2. Removal rate of copper reachs97.5%and leaching rate of tellurium is1.05%when dosage of HNO3is0.96time of stoichiometric dosage, and tellurium is tranformed into TeO2.
Powdered tellurium is obtained after Se has been removed beforehand and Te is treated twice by method of oxidation, leaching and reduction.Finally,4N+tellurium satisfied with standard of YS/T222-1996is acquired after powdered tellurium is treated under450℃and hydrogen ambient.
Catalytic mechanism of Cl-on reduction of Te (Ⅳ) is studied by means of methods such as ion-exchange, UV-VS spectrophotometry, XRD and determination of solubility. The results show that Te(IV) exists in form of TeOOH+when concentration of H2SO4in solution is less than700g·L-1, TeOOH+is gradually dehydrated and changed Te2O3SO4when concentration of H2SO4is over700g·L-1. Therefore, Te (Ⅳ) becomes more stable and more difficult to be reduced by SO2. Structure of Te2O3SO4in high concentration H2SO4solution is destroyed by Cl-, with the increasing of Cl-concentration,Te(Ⅳ) is transformed step by step into TeOCl2, TeCl4and H2TeCl6, and Te(IV) is getting more and more active. The study on catalytic kinetic of Cl-shows activation energy is44.87kJ·mol-1when Cl-concentration is0.1mol·L-1, and activation energy is36.714kJ·mol-1when Cl-concentration is0.3mol·L-1. XRD results confirm that product is elemental tellurium when Cl-and Br-are used as catalyst, the product is Tel (Te4I4) when I-is used as catalyst.
Distribute ratio of elements in the tellurium-containing residue during purification and thermodynamic analysis show that impurities can be removed efficiently and high pure tellurium can be obtained by oxidizing with HNO3and leaching with H2SO4, removing selenium beforehand, oxidizing-leaching-reducing and treating under hydrogen ambient and high temperature. Impurities such as Cu, Pb, Sb and Ag in powdered tellurium combine with Cl-to form complexes and are kept in the solution together with Ca, Al, Mg and Fe when concentration of HC1in solution is not less than6mol·L-1. Arsenic is evaporated in forms of As4O6, Se is removed in form of H2Se under450℃and hydrogen ambient.
Compared with traditional technologies, this technology on extracting tellurium has many advantages such as large treatment capacity of convert, low consumption of energy and acid, little flue gas volume. Contrasted to the traditional method in which precipitating tellurium with copper powder, the catalytic reduction method has its advantages such as low cost, high content of tellurium in the product and easy treatment. High pure tellurium is prepared by chemical method. This method has advantages such as easy control, low cost, high direct recovery rate, stable quality of product and large scale.
引文
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