高锑低银类铅阳极泥制备五氯化锑新工艺

研究采用控电氯化浸出-低压连续蒸馏-氧化结晶法处理高锑低银类铅阳极泥制备五氯化锑的新工艺.结果表明:稀盐酸酸洗可有效去除铅阳极泥中的氟和硅:当溶液电位控制在430 mV以上时,阳极泥中锑、铜和铋的浸出率均大于99%,浸出液中三价锑离子的浓度高达310 g/L,浸出液经冷却结晶后银的入渣率为91.12%,铅的入渣率为96.35%;当蒸馏温度为190℃时,蒸馏余物中三氯化锑已接近无水三氯化锑熔盐,无水三氯化锑熔盐通氯氧化-结晶分离所获得的五氯化锑产品质量完全达到试剂级产品的要求,而金属铁、铋和铜等均残留在结晶分离残渣中,锑的回收率大于95%.     

基于超结构模型的铅阳极泥制备锑白工艺水网络优化

为降低铅阳极泥回收工艺过程中废水排放对环境的影响,以高锑低银类铅阳极泥湿法制备锑白为研究对象,构造针对过程盐酸减排的水网络超结构,提出带反应单元的杂质物料平衡模型,建立水网络求解非线性规划问题,并通过实验数据调和整定用水与处理单元特征参数,求解非线性规划问题并根据最优解进行了工业装置路线设计。将该方法应用于铅阳极泥制备锑白工艺设计时,可将废水中酸和有毒金属的排放浓度控制到给定值以下,优化后水的重复利用率可达到87.4%;采用基于超结构的非线性规划对此工艺过程进行优化,可以获得合理的水网络结构,达到减排效果。     

锌阳极泥矿浆中铅银矿物的赋存状态及其与黄药的作用(英文)

用热力学方法分析锌阳极泥矿浆的强氧化背景矿浆电位及其对铅、银和黄原酸盐赋存状态的影响。结果表明,在强氧化背景矿浆电位下,铅以 Pb2+或 PbSO4形式存在,银以金属银、AgCl 和 Ag2O 等形式存在,黄原酸盐以其氧化后的二聚物双黄药形式存在。XRD 分析结果表明,锌阳极泥中的铅矿物主要是铅矾,主要的银矿物之一是氯银矿。单矿物浮选实验表明,双黄药对氯银矿的捕收力远强于对铅矾的。用 Material Studio(Adsorption Locater)模块计算了两种吸附质(铅矾和氯银矿)与不同吸附剂(双黄药, H2O, OH-, Cl-, SO42-)的作用能变化。结果表明,在存在 SO42-的条件下,双黄药只能吸附在氯银矿表面。红外光谱测试证实了双黄药对氯银矿的选择性吸附作用。     

Preparation of clarificant for glass from As-Sb dust

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Thermodynamic analysis of separating lead and antimony in chloride system

In chloride system, thermodynamic analysis is a useful guide to separate lead and antimony as well as to understand the separation mechanism. An efficient and feasible way for separating lead and antimony was discussed. The relationships of [Pb2+][Cl-]2-lg[Cl]T and E-lg[Cl]T in Pb-Sb-Cl-H2O system were studied, and the solubilities of lead chloride at different antimony concentrations were calculated based on principle of simultaneous equilibrium. The results show that insoluble salt PbCl2 will only exist stably in a certain concentration range of chlorine ion. This concentration range of chlorine ion expands a little with increasing the concentration of antimony in the system while narrows as the system acidity increases. The solubility of Pb2+ in solution decreases with increasing the concentration of antimony in the system, whereas increases with increasing the concentration of total chlorine. The concentration range of total chlorine causing lead solubility less than 0.005 mol/L increases monotonically.     

铅阳极泥脱砷预处理研究

采用氢氧化钠溶液循环浸出法对铅阳极泥进行预脱砷,考察了液固比、氢氧化钠浓度、浸出温度和浸出时间对脱砷效果的影响;在液固比10∶1、氢氧化钠浓度2.5 mol/L、浸出温度80℃、浸出时间8 h的条件下,砷的浸出率可达94%以上;含砷浸出液经硫化钠沉砷后可返回浸出工序循环使用,硫化钠与砷质量比为3∶1时,沉砷率可达88%以上,同时回用浸出工序后,砷浸出率达94%以上,浸出液循环使用对脱砷没有影响。     

Preparation of lead sulfate powder directly from galena concentrates

A new approach to prepare PbSO4 powder is studied. Using the methods of the leaching of galena concentrates in the ferric chloride media, selective purification and chemical sedimentation, PbS concentrate can be converted into PbSO4. The conversion recovery is 97.39%, the purity of PbSO4 powder is above 99% and its average crystallite size is about 42 nm. In this process, emission of lead vapour and SO2 cannot occur. The experimental results demonstrate the feasibility of realizing a green route to prepare the lead sulfate powder.     

铅鼓风炉中铜、硫、砷和锑对银分布的影响(英文)

研究铅鼓风炉中杂质对银分布的影响。将含有不同Cu、S、As和Sb含量的铅烧结块在管式炉中于1573K下进行烧结,然后随炉冷却。烧结气氛为还原性的CO+CO2气体(p(CO)/p(CO2)=2.45)。采用SEM-EDS对所得样品进行表征。结果表明:烧结样品中含有5种不互溶的相,即炉渣(CaO,FeO,SiO2)、冰铜(S,Cu,Fe)、硬渣(As,Fe,Cu)、Cu-Sb相和铅块。银在Cu与Sb形成的熔体中的溶解度比在液态铅中的高。S与Cu形成冰铜,As与Cu形成硬渣。S和As能减少Cu-Sb合金的生成量,从而降低铅块中银的损失。     

铜阳极泥选冶联合工艺有价金属走向考察及改进建议

铜阳极泥是资源综合回收的优选对象,分析各有价金属的分散情况对后续的回收有着指导性的方向作用。铜阳极泥选冶联合工艺较为成熟,具有不断外延拓展金属回收的空间。针对4000 t铜阳极泥物料的生产数据,考察了该工艺有价金属的走向,统计分析了金、银、硒、碲、铅、锑、铋、铜等在工艺流程中的分布率,摸清了有价金属主要分散情况。分析表明,金、银、硒、碲最大的分散点均为浮选尾矿,分别占分散总量的67%、37%、34%、58%,确定为重点管控对象。并结合统计分析结果对提高金、银、硒、碲回收率及铅、锑、铋、铜的回收提出了改进建议。     

Behavior of silver and lead in selective chlorination leaching process of gold-antimony alloy

The behavior of silver and lead in the selective chlorination leaching process of gold-antimony alloy was analyzed in detail and appropriate recovery methods were developed.A reduction method by adding gold-antimony alloy powder was adopted to recover silver according to the thermodynamics calculation.The reducing rate of silver can exceed 99%at 80℃for 1.5 h when the dosage of gold-antimony alloy powder is 10%.The dissolution equilibrium curved surfaces of PbSO4 and PbCl2 under different conditions were dra...     

从铂钯精矿中氯化浸出Au、Pt、Pd

针对铜阳极泥处理过程中生产的铂钯精矿,以氯酸钠为氧化剂,采用湿法氯化浸出,使金、铂、钯等贵金属以氯配合物进入溶液。研究了浸出的最佳工艺条件。结果表明,金、铂、钯的浸出率均达到99%以上。     

铜阳极泥处理过程中中和渣中碲的提取与制备

采用硫酸浸出二氧化硫还原方法从中和渣中制取单质碲。研究表明:采用硫酸浸出中和渣,当反应温度为30℃、反应时间为0.5 h、硫酸浓度为53.9 g/L、硫酸用量为理论用量的1.5倍时,碲浸出率为99.99%;采用亚硫酸钠还原酸浸液中碲时,碲(Ⅳ)发生水解生成二氧化碲;采用二氧化硫还原酸浸液中碲时,当反应温度为75℃、反应时间为2 h、盐酸浓度为3.2 mol/L、二氧化硫流量为0.4 L/min时,碲回收率达到99.84%。X射线衍射(XRD)分析表明二氧化硫还原得到的产物为单质碲,电感耦合等离子体发射光谱(ICP)分析表明,碲粉中碲含量为98.27%。扫描电子显微系统(SEM)分析表明,碲粉的形态为针形。     

从铅银渣中回收金银概况

为实现铅银渣中金银的综合回收,对铅银渣物理化学性质、有价金属含量、赋存状态、铅银渣中金银的回收方法、研究进展及其应用情况进行综述。铅银渣粒度细、酸度强、可溶物含量高,渣中矿物经历过相体转化由硫化物转变成氧化物,以再造矿物形式存在,选矿难度大;铅银渣有价金属铜、铅、锌、金、银含量较高,经济价值可观。目前,从铅银渣中回收金银的主要方法为浮选法、湿法、火法、湿法-火法联合、选冶联合等。通过分析各种方法优缺点,指出单一的浮选法流程简单、成本低,但金银回收率低;湿法、火法或湿法-火法工业应用良好,但是存在工艺复杂、成本高;选冶联合方法金属回收率高、流程适应性强,便于连续操作,具有较好的发展应用前景。     

复杂铜精矿除锑的建模与工艺优化(英文)

对一种含1.69%Sb和0.14%Sn的铜精矿进行碱性硫化物浸出以除去Sb和Sn,对浸出条件建立数学模型,并对工艺条件进行优化。采用响应面方法并结合面心立方中央复合设计来优化工艺参数。选取浸出温度、硫化物浓度和固体含量作为变量参数,而将Sb和Sn的浸出率和达到浸出90%Sb所需时间作为响应参数。结果表明:温度和硫化物浓度对Sb和Sn的浸出影响显著,而固体含量的影响不显著。建立了一个数学模型来描述浸出条件,实验验证了该模型是可靠与准确的。     

以含铜硒的粗碲为原料采用化学法制备高纯碲(英文)

以含铜、硒的粗碲为原料,采用硝酸氧化、盐酸浸出、二氧化硫还原、氢气气氛高温处理的化学方法制备高纯碲。在浓硝酸(69%)用量为化学计量的0.96倍、液固比为4:1、反应温度为20°C、反应时间为30min的条件下,用硝酸氧化粗碲,粗碲中铜的去除率达到99%。粗碲氧化后用盐酸浸出,在浓盐酸用量为化学计量的1.67倍、液固比为4:1、反应温度为20°C、反应时间为30min的条件下,碲的浸出率为99%。浸出液中Te(IV)经二氧化硫还原,碲粉纯度达到99.95%。碲粉在反应温度为730K的氢气中处理30min,其纯度由99.95%上升到99.9995%。     

Selective removal of As from arsenic-bearing dust rich in Pb and Sb

The selective removal of arsenic from arsenic-bearing dust containing Pb and Sb in alkaline solution was studied. The influence of NaOH concentration, temperature, leaching time, liquid to solid ratio, and the presence of elemental sulfur on the dissolution of As, Sb and Pb in NaOH solution was investigated. The results indicate that the presence of elemental sulfur can effectively prevent leaching of lead and antimony from arsenic. The Sb₂O₃, As₂O₃ and Pb₅(AsO₄)₃OH in the raw material convert to NaSb(OH)₆ and PbS in the leaching residue, while arsenic is leached out as As(III) or As(V) ions in the leaching solution. Arsenic leaching efficiency of 99.84% can be achieved under the optimized conditions, while 97.82% of Sb and 99.97% of Pb remain in the leach residue with the arsenic concentration of less than 0.1%. A novel route is presented for the selective removal of arsenic and potential recycle of lead and antimony from the arsenic-bearing dust leached by NaOH solutions with the addition of elemental sulfur.     

Optimization of operating parameters and kinetics for chloride leaching of lead from melting furnace slag

The feasibility and kinetics of lead recovery from the slag of traditional lead melting furnace using chloride leaching were investigated. The effects of operating parameters such as leaching time, NaCl concentration, FeCl₃ concentration, liquid/solid ratio, stirring rate, temperature, and particle size on recovery of lead were studied and the optimization was done through the response surface methodology (RSM) based on central composite design (CCD) model. The optimum conditions were achieved as follows: leaching time 60 min, 80 °C, stirring rate 800 r/min, NaCl concentration 200 g/L, FeCl₃ concentration 80 g/L, liquid/solid ratio 16, and particle size less than 106 μm. More than 96% of lead was effectively recovered in optimum condition. Based on analysis of variance, the reaction temperature, liquid/solid ratio, and NaCl concentration were determined as the most effective parameters on leaching process, respectively. Kinetics study revealed that chloride leaching of galena is a first-order reaction and the diffusion through solid reaction product and chemical reaction control the mechanism. The activation energy of chloride leaching of galena was determined using Arrhenius model as 27.9 kJ/mol.     

Separation of arsenic and antimony from dust with high content of arsenic by a selective sulfidation roasting process using sulfur

The separation of arsenic and antimony from dust with high content of arsenic was conducted via a selective sulfidation roasting process. The factors such as roasting temperature, roasting time, sulfur content and nitrogen flow rate were investigated using XRD, EPMA and SEM–EDS. In a certain range, the sulfur addition has an active effect on the arsenic volatilization because the solid solution phase ((Sb,As)₂O₃) in the dust can be destroyed after the Sb component in it being vulcanized to Sb₂S₃ and this generated As₂O₃ continues to volatile. In addition, an amorphization reaction between As₂O₃ and Sb₂O₃ is hindered through the sulfidation of Sb₂O₃, which is also beneficial to increasing arsenic volatilization rate. The results show that volatilization rates of arsenic and antimony reach 95.36% and only 9.07%, respectively, under the optimum condition of roasting temperature of 350 °C, roasting time of 90 min, sulfur content of 22% and N₂ flow rate of 70 mL/min. In addition, the antimony in the residues can be reclaimed through a reverberatory process.     

氧化锌贫矿提锌渣中铅和银的氯盐一步浸出

运用X射线衍射、扫描电镜和X射线能谱等分析手段,对山东某地深度氧化锌贫矿提锌后渣进行工艺矿物学特征分析可知,矿物中金属赋存状态复杂,属难选矿物。开发出氯盐一步法浸出铅和银的新工艺,考察反应温度、NaCl浓度、添加剂用量、液固比、HCl加入量和浸出时间对浸出过程的影响。结果表明:加入添加剂对铅的浸出率没有影响,但可以显著提高银的浸出率。条件试验研究得出最佳工艺条件如下:浸出温度90℃、NaCl浓度390 g/L、添加剂用量15 mL、液固比(质量比)7?1、HCl加入量3 mL、浸出时间3 h。在此最佳工艺条件下,铅的浸出率达到95%左右,银的浸出率达到90%左右。