Ida~（2-）-H_2O体系浸出低品位氧化锌矿

采用Ida2--H2O体系（亚氨二乙酸盐水溶液）处理高碱性脉石型低品位氧化锌矿,考察浸出时间、液固比、配体总浓度、温度及pH值对矿物中主金属Zn及杂质元素Ca、Mg、Cu、Ni、Fe、Pb、Cd的溶出影响。结果表明：在弱碱性Ida2--H2O体系中,Ca、Mg、Fe不会被大量溶出,有价金属Cu、Ni、Pb、Cd可部分随主金属Zn溶出而进入浸出液;在浸出时间4h、液固比5：1、配体总浓度0.9mol/L、温度70℃、pH8的优化条件下,锌浸出率为76.6%。     

Preparation of Mn−Zn ferrite from spent zinc-carbon batteries by alkali leaching,acid leaching and Co-precipitation

The treatment of spent zinc-carbon batteries for the recovery of valuable metals followed by conversion to Mn−Zn ferrite has been conducted employing two-stage alkali and acid leaching and co-precipitation method. In the first stage, leaching process was carried out with 4 M NaOH, which resulted in a recovery of 63.4 %Zn and 0.1% Mn. Electrowinning of alkali leaching solution containing 12.75 g/L Zn at a current density of 0.2 A/cm² produced Zn metal of 15 nm to 30 nm size and 99.9% purity. The second stage leaching of residue with 3 M H₂SO₄ and 6 vol.% H₂O₂ at a solid/liquid ratio of 1∶10 indicated the leaching efficiency of 98.0% Zn, 97.9% Mn and 55.2% Fe. The obtained leaching solution was finally adjusted to suitable mole ratios of Mn∶Zn∶Fe (1∶1∶4) by the addition of Zn and Fe sulfate salts followed by pH control to produce Mn−Zn ferrite powder. The characterization of the ferrite powder showed uniform nano-crystalline particles of about 20 nm size with spinel structure.     

Ida~(2-)-H_2O体系浸出低品位氧化锌矿(英文)

采用Ida2--H2O体系(亚氨二乙酸盐水溶液)处理高碱性脉石型低品位氧化锌矿,考察浸出时间、液固比、配体总浓度、温度及pH值对矿物中主金属Zn及杂质元素Ca、Mg、Cu、Ni、Fe、Pb、Cd的溶出影响。结果表明:在弱碱性Ida2--H2O体系中,Ca、Mg、Fe不会被大量溶出,有价金属Cu、Ni、Pb、Cd可部分随主金属Zn溶出而进入浸出液;在浸出时间4h、液固比5:1、配体总浓度0.9mol/L、温度70℃、pH8的优化条件下,锌浸出率为76.6%。     

Preparation of pure SbCl3 from lead anode slime bearing high antimony and low silver

A novel treatment process of lead anode slime bearing high antimony and low silver was developed by a potential-controlled chloridization leaching and continuous distillation.The experimental results show a high Sb 3+ concentration,489.2 g/L,in the leaching solution for two-stage countercurrent leaching process,and the leaching rates of Sb,Cu,Bi more than 99% when the potential is controlled at 450 mV.When the leaching solution is distillated and concentrated at 120°C,almost all the silicon compound is evaporated into the concentration distillate and exists as amorphous hydrated silica.By the continuous distillation,high pure SbCl3 could be prepared,and AsCl3 is enriched in the distillate while metals Bi,Cu are enriched in the continuous distillation residue.As a result,the recovery rate of Sb is more than 95%.     

Extraction of valuable metals from low nickel matte by calcified roasting−acid leaching process

A calcified roasting−acid leaching process was developed as a highly effective method for the extraction of valuable metals from low nickel matte in the presence of CaO additive. The influences of process parameters on the metal extraction were studied, including the roasting temperature, roasting time, addition of CaO, H₂SO₄ concentration and liquid−solid ratio. Under the optimum condition, 94.2% of Ni, 98.1% of Cu, 92.2% of Co and 89.3% of Fe were recovered. Additionally, 99.6% of Fe was removed from the leachate as goethite by a subsequent goethite iron precipitation process. The behavior and mechanism of CaO additive in the roasting process was clarified. The role of CaO is to prevent the formation of nonferrous metal ferrite phases by a preferential reaction with Fe₂O₃ during the roasting process. The metal oxides (CuO and Ni_xCu_1−xO) remained stable during high-temperature roasting and were subsequently efficiently leached using a sulfuric acid solution.     

回转窑内渣成分优化实现锌铅元素的高效回收（英文）

在回转窑内从高硅锌浸出渣中实现高效回收锌铅金属。XRD、SEM、EDS及ICP表征结果表明,浸出渣含12.4%SiO₂、16.1%Zn和7.4%Pb(质量分数)。热力学分析表明,在回转窑内1150～1250℃的冶炼环境下,锌浸出渣中极易产生锌和铅的金属蒸气。通过分析13种冶金渣成分的黏度及熔点,发现3种渣成分(47%SiO₂-23%CaO-30%FeO、40%SiO₂-28%CaO-32%FeO、40%SiO₂-30%CaO-30%FeO,质量分数)具有合适的物理特性,即熔点和黏度分别为1150～1280℃和0.2～0.5 Pa·s。工业实验表明,采用优化的渣成分,锌和铅的回收率分别高达97.3%和94.5%,冶炼后渣内锌和铅的含量分别低至0.51%和0.45%(质量分数)。水淬渣的国标浸出实验表明,浸出液中含1.82 mg/L Zn、～0.01 mg/L Cu、0.0004 mg/L As、～0.01 mg/L Cd、0.08 mg/L Pb和～0.02 mg/L Hg,证实锌浸出渣同步实现无害化...     

从锌置换渣中分段浸出锌、铅、镓和锗

采用分段浸出方法从锌置换渣中选择性提取锌、铅、镓和锗.首段浸出过程通过控制合适的硫酸浓度与液固比条件,锌和镓的浸出率达到90％和99％以上,超过92％的锗留在硫酸浸出渣中;二段采用盐酸作为浸出剂选择性提取铅,铅的浸出率为99％,锗损失率小于2％;三段采用1 mol/L氢氧化钠作为浸出剂,通过破坏硅锗固溶体的结构,实现锗...     

Co-reduction of Copper Smelting Slag and Nickel Laterite to Prepare Fe-Ni-Cu Alloy for Weathering Steel

In this study, a new technique was proposed for the economical and environmentally friendly recovery of valuable metals from copper smelting slag while simultaneously upgrading nickel laterite through a co-reduction followed by wet magnetic separation process. Copper slag with a high FeO content can decrease the liquidus temperature of the SiO₂-Al₂O₃-CaO-MgO system and facilitate formation of liquid phase in a co-reduction process with nickel laterite, which is beneficial for metallic particle growth. As a result, the recovery of Ni, Cu, and Fe was notably increased. A crude Fe-Ni-Cu alloy with 2.5% Ni, 1.1% Cu, and 87.9% Fe was produced, which can replace part of scrap steel, electrolytic copper, and nickel as the burden in the production of weathering steel by an electric arc furnace. The study further found that an appropriate proportion of copper slag and nickel laterite in the mixture is essential to enhance the reduction, acquire appropriate amounts of the liquid phase, and improve the growth of the metallic alloy grains. As a result, the liberation of alloy particles in the grinding process was effectively promoted and the metal recovery was increased significantly in the subsequent magnetic separation process.     

Zinc removal from hyperaccumulator Sedum alfredii Hance biomass

Leaching of heavy metals from Sedum alfredii Hance biomass was studied with ammonia-ammonium chloride solution as leaching agent. The research was carried out in two phases: 1) a leaching study to determine the zinc extraction efficiency of this leaching agent, and 2) a thermodynamic analysis to identify the likely reactions and stable Zn(II) species formed in the leaching systems. Taguchi orthogonal experiment, with four variable parameters, leaching temperature, molar ratio of NH₄Cl to NH_3, leaching time and solid-to-liquid(L/S) ratio, and each at three levels, was used to optimize the experiment parameters by the analysis of variances. The results indicate that leaching temperature has the most dominant effect on metal extraction performance, followed by molar ratio of NH₄Cl to NH₃, solid-to-liquid ratio and leaching time. The optimum condition was obtained as follows: temperature of 60°C, molecular ratio of NH₄Cl to NH₃ of 0.6, leaching time of 2 h and solid-to-liquid ratio of 5:1. The total zinc leaching efficiency under optimum conditions reaches 97.95%. The thermodynamic study indicates that the dominant species produced by the leaching process should be the soluble Zn(NH₃)₄₂⁺.     

Extracting Cu,Co, and Fe from white alloy with HCl by adding H<Subscript>2</Subscript>O<Subscript>2</Subscript>

White alloy, mainly containing Cu, Co, and Fe, has been successfully decomposed in HCl solution by adding H₂O₂. This process is discussed in this paper. Through exploratory experiments, hydrochloric acid and H₂O₂ solution were confirmed as the leaching system of white alloy and through a series of condition experiments the effect of HCl concentration, H₂O₂ addition amount, reaction temperature, reaction time, particle size, and liquid-solid ratio of the extraction are studied. The optimal leaching conditions are 5 mol/L HCl concentration, 1.85 mL H₂O₂/g white alloy H₂O₂ addition, 70°C reaction temperature, 90 min. reaction time, 100 mesh particle size, and a 5/1 liquidsolid ratio. With these conditions the extraction of Cu and Co exceeds 99.5%, and the extraction of Fe can reach 98.5%. The results show the addition of H₂O₂ and the introduction of Cl⁻ are very important factors to improve the extraction of metal.     

Kinetics of SiO2 leaching from Al2O3 extracted slag of fly ash with sodium hydroxide solution

Kinetics of SiO₂ leaching from Al₂O₃ extracted slag of fly ash with sodium hydroxide solution was studied. The effect of leaching temperature, mass ratio of NaOH to SiO₂ and stirring speed on SiO₂ leaching rate was investigated. The results show that increasing leaching temperature, mass ratio of NaOH to SiO₂ and stirring speed increases SiO₂ leaching rate. The SiO₂ leaching rate is 95.66% under the optimized conditions. There are two stages for the SiO₂ leaching process, and the leaching reaction is very rapid in the first stage but quite slow in the second stage. The whole leaching process follows the shrinking core model, and the outer diffusion of no product layer is the rate-controlling step. The activation energies of the first and second stages are calculated to be 8.492 kJ/mol and 8.668 kJ/mol, respectively. The kinetic equations of the first and the second stages were obtained, respectively.     

Leaching of blended copper slag in microwave oven

Leaching of blended slag (BS) was investigated in a microwave oven using hydrogen peroxide and acetic acid. The BS was a mixture of converter and flash furnace slag containing 51% Fe₂O₃, 3.8% CuO, and 3.2% ZnO. The important variables that influence the metal extraction yield were leaching time, liquid-solid ratio, H₂O₂ and CH₃COOH concentrations. The preferred leaching conditions were as follows: CH₃COOH concentration 4 mol/L; H₂O₂ concentration 4 mol/L; microwave power 900 W; leaching time 30 min; liquid-solid ratio 25 mL/g BS; leaching temperature 100 °C. Under these conditions, the metal extractions of 95% Cu, 1.6% Fe, and 30% Zn were obtained. The results were compared with the traditional leaching results. It is evident that microwave heating causes a reduction in the leaching time. Also, the extraction yield results indicate that selective leaching of BS can be achieved under the preferred conditions. The dissolution kinetic of BS in hydrogen peroxide with acetic acid is controlled by a shrinking unreacted core model equation. The apparent activation energy and reaction order were found to be 16.64 kJ/mol and 1.09, respectively.     

Selective leaching of arsenic from copper converter flue dust by Na2S and its stabilization with Fe2(SO4)3

The alkaline leaching of arsenic (As₂O₃) by Na₂S, together with its precipitation by Fe₂(SO₄)₃ was studied. Response surface methodology based on central composite design was employed to quantify and qualify the effect of pertinent factors and to develop statistical models for optimization purposes. Based on the obtained results, 89% of arsenic is removed from the dust under following optimum predicted conditions: Na₂S concentration of 100 g/L and solid to liquid ratio of 0.163 g/mL at 80 °C. It is found that solid to liquid ratio and Na₂S concentration are the significant factors influencing the leaching process. In the precipitation process, more than 99.93% of arsenic from the leaching solution is removed in the form of amorphous ferric arsenate, at pH 4.8 when Fe³⁺ to arsenic and H₂O₂ to arsenic molar ratios are set at 5:1 and 4:1, respectively. Also, Fe³⁺ to arsenic ratio and pH are the most significant factors, and the interaction between these terms is significant.     

Selective recovery of lithium from spent lithium iron phosphate batteries using oxidation pressure sulfuric acid leaching system

Oxidation pressure leaching was proposed to selectively dissolve Li from spent LiFePO₄ batteries in a stoichiometric sulfuric acid solution. Using O₂ as an oxidant and stoichiometric sulfuric acid as leaching agent, above 97% of Li was leached into the solution, whereas more than 99% of Fe remained in the leaching residue, enabling a relatively low cost for one-step separation of Li and Fe. And then, by adjusting the pH of leachate, above 95% of Li was recovered in the form of the Li₃PO₄ product through iron removal and chemical precipitation of phosphate.     

NaOH分解含铟铁矾渣新工艺

提出NaOH分解含铟铁矾渣新工艺,考察NaOH用量、液固比、温度和时间对铁矾渣分解率的影响,并讨论铁矾渣中杂质金属,如Zn、In、Cu、Cd、Pb、As、Sb、Sn和Ag等在NaOH分解过程中的行为.结果表明:在m(NaOH)-m(铁矾渣)=0.381 4-1、温度60 ℃、液固比2-1、反应时间2 h的最优条件下,铁矾渣的分解率达到98.03%,而原料中的杂质金属,如Sn、Sb、Zn、In、Cu、Cd、Pb和Ag等绝大部分留在分解渣中,As则以AsO43-的形态大部分进入溶液,浸出率达到83.36%.DSC-TGA热分析和X射线衍射分析结果表明:在NaOH分解过程中,铁矾渣中的铁主要以Fe3O4形式沉淀入渣;分解渣中Fe、In和Zn的含量分别为38.81%、0.23%和12.89%;经稀盐酸选择性浸出铟和锌后,进一步磁选富集可作为炼铁原料.     

Cyclic metallurgical process for extracting V and Cr from vanadium slag: Part II. Separation and recovery of Cr from vanadium precipitated solution

Cyclic metallurgical process for separation and recovery of Cr from vanadium precipitated solution by precipitation with PbCO₃ and leaching with Na₂CO₃ was investigated. The concentration of Cr residue in the solution decreases from 2.360 to 0.001 g/L by adding PbCO₃ into vanadium precipitated solution according to Pb/Cr molar ratio of 2.5, adjusting the pH to 3.0 and stirring for 180 min at 30 °C. Then, the precipitates were leached with hot Na₂CO₃ solution to obtain leaching solution containing Na₂CrO₄ and leaching residue containing PbCO₃. The leaching efficiency of Cr reaches 96.43% by adding the precipitates into 0.5 mol/L Na₂CO₃ solution with the mass ratio of liquid to solid (L/S) of 10:1 mL/g and stirring for 60 min under pH 9.5 at 70 °C. After filtration, leaching residue is reused in Cr precipitation and leaching solution is used to circularly leach the Cr precipitates until Na₂CrO₄ approaches the saturation. Finally, the product of Na₂CrO₄·4H₂O is obtained by evaporation and crystallization of leaching solution.     

Interfacial reaction of Co–Fe films with SiO2 substrates

The interdiffusion reaction between Co_1?xFe_x deposited films of various compositions (x = 0.27, 0.32 and 0.50) and an amorphous SiO₂ substrate during annealing in vacuum at 800 °C was identified by analytical transmission electron microscopy. The reaction results in the formation of Fe₂SiO₄ mixed silicate of olivine structure as an interfacial phase. The following microstructural changes occurring during this reaction are inferred: (a) recrystallization of as-deposited films during the 800 °C annealing results in large grains of the body centered cubic Co–Fe solid solution; (b) metals diffuse into the SiO₂ substrate and nucleate grains of the Fe₂SiO₄ silicate along the film/SiO₂ interface; (c) silicon and oxygen partially released during the reaction, in turn, diffuse into an unreacted metallic film and form precipitates of the (Co,Fe)₃O₄ spinel phase and solid solution of Si in Co–Fe. To our best knowledge, the formation of silicates with olivine-type structure (known as fayalite for Fe) as products of the metal/SiO₂ reaction has never been reported before. Thermodynamic evaluation of the reaction employing the semi-empirical CALPHAD (Calculation of Phase Diagrams) method supports the experimental findings, although the reaction requires an excess of oxygen.     

High-temperature oxidation kinetics of Cu-Si alloys containing up to 4.75 wt.% Si inp_{{\text{O}}_{\text{2}} } =0.01 atm and pure CO2

The oxidation of Cu-Si alloys (containing up to 4.75 wt. % Si) in =0.01 atm from 800 to 1000°C has been investigated using thermogravimetry and other techniques. A 0.04% Si alloy followed a parabolic oxidation law with a rate similar to that of pure Cu. As the Si concentration increased the rate decreased and became irregular owing to SiO₂ particles or flakes at the alloy-scale interface. It is considered that sintering of SiO₂ particles and rupture of the sinter because of contraction during sintering are responsible for the irregular kinetics. A SiO₂ layer forms directly on the 4.75% Si alloy which oxidizes uniformly. The SiO₂ was always amorphous. In pure CO₂ a similar pattern of amorphous SiO₂ particles, flakes, and layers occurs.     

Enhanced corrosion resistance of Zn–Cu–Ti alloy with addition of Cu–Ti amorphous ribbons in 3.5% NaCl solution

In the present study, Zn–0.3Cu–0.3Ti alloy (sample I) was fabricated by a simple low-temperature melting method using Cu–50Ti amorphous alloy ribbons for corrosion in 3.5% NaCl solution. As a comparison, crystalline Cu–50Ti master alloy was used to prepare Zn–0.3Cu–0.3Ti alloy (sample II). Sample I comprising Zn, TiZn₃, and TiZn₁₅ phases exhibits an equiaxed microstructure with subgrain structure. Large TiZn₃ particles show cluster feature, whereas intermittent small TiZn₁₅ particles exist at grain boundaries and subgrain boundaries. In sample II, the Zn matrix with typical dendritic microstructure is observed and no large particles are found. Compared with sample II, sample I shows lower weight gain and corrosion current density and a higher slope of cathode polarization curve. The weight gain for sample I is only 0.59 mg·cm⁻², but for sample II, this value reaches 0.70 mg·cm⁻². After 8 days of corrosion, corrosion products are mainly Zn₅(OH)₈Cl·H₂O and ZnO, showing loose particle shape. As corrosion time increases from 2 days to 8 days, corrosion layer thickness increases from about 15 to 24 μm for sample 1.     

Enhanced selectivity of hydrolytic precipitation of Zn from Zn-Ni sulfate solution via chelation of Ni

The selective precipitation of zinc from zinc–nickel sulfate solution with the Zn/Ni molar ratio of 20:1 was studied. Dropwise addition of 0.5 mol/L NaOH solution into the zinc–nickel sulfate solution containing 0, 0.01, 0.02, 0.03 and 0.04 mol/L ethylene diamine tetraacetate (EDTA) as a chelating agent was done. The equilibrium analysis of precipitation pathway was performed using Visual MINTEQ program. The equilibrium analysis showed that the presence of small amounts of EDTA can prevent nickel precipitation in alkaline conditions without any negative effect on zinc precipitation. On this basis, more than 90% of zinc could be precipitated as a product with about 50% Zn and only 0.11% Ni at pH=9.0 merely as a result of the presence of 0.03 mol/L EDTA in the solution. The stirring time of 120 min after precipitation was found to be essential for more complete separation. The X-ray diffraction studies on the precipitate revealed that the precipitated phase was Zn₄(OH)₆SO₄.4H₂O.