Leaching of cuprite through NH4OH in basic systems

Cuprite is a difficult oxide to leach under acidic conditions (for the maximum extraction of 50%). In this research, the feasibility of leaching cuprite in an ammoniacal medium was studied. The working conditions addressed here were the liquid/solid ratio (120:1–400:1 mL/g), stirring speed (0–950 r/min), temperature (10–45 °C) and NH₄OH concentration (0.05–0.15 mol/L). In addition, different ammoniacal reagents (NH₄F and (NH₄)₂SO₄) were analyzed. The experiments were performed in a 2 L reactor with a heating mantle and a condenser. The most important results were that the maximum leaching rate was obtained at pH 10.5, 0.10 mol/L NH₄OH, 45 °C, 4 h, 850 r/min and a liquid/solid ratio of 400:1, reaching a copper extraction rate of 82%. This result was related to the non-precipitation of copper in solution by the formation of copper tetra-amine. The liquid/solid ratio and stirring speed were essential for increasing the cuprite leaching. The maximum leaching rate was achieved at higher temperatures; however, significant copper leaching rate occurred at temperatures near the freezing point of water (17.9% over 4 h). Increasing NH₄OH concentration and decreasing particle size increased the cuprite leaching rate. The two ammoniacal reagents (NH₄F and (NH₄)₂SO₄) had low extraction rate of copper compared with NH₄OH. The kinetic model representing cuprite leaching was a chemical reaction on the surface. The order of the reaction with respect to the NH₄OH concentration was 1.8, and it was inversely proportional to the radius of the ore particles. The calculated activation energy was 44.36 kJ/mol in the temperature range of 10–45 °C.     

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.     

通过水性还原法用NaBH4制备纳米铜颗粒过程中反应参数对制备过程的影响（英文）

通过水溶液还原法制备纳米铜颗粒,研究了不同反应条件对制备纳米铜的影响。制备纳米铜的最优条件是:当溶液 pH为12、温度为 313K、1%的明胶作为分散剂时,将0.4mol/L NaBH4加入含有 1.2mol/L 氨水的0.2mol/L CuSO4溶液中。此外,进行了一系列实验来模拟反应进程。结果表明,氨水能改变反应进程。当溶液 pH为10时,氨水将Cu2+转化为铜氨络合物,然后被 NaBH4还原为铜颗粒。当溶液pH为12时,氨水将Cu2+转化为氢氧化铜,然后被 NaBH4还原为铜颗粒。     

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.     

通过选择性浸出、结晶和沉积回收废重整催化剂中的镍和铝

研究和优化不同工艺条件下硫酸(3.0~5.5 mol/L)浸出回收Ni和Al的工艺。浸出实验表明,在H₂SO₄浓度5.5 mol/L、反应时间4 h、固液比0.2 g/mL、温度358 K、粒径<100μm、搅拌速度200~250 r/min、催化剂用量5.0 g的条件下,可提取98.5%的NiO和40.7%的Al₂O₃。浸出液中的Al用1.4 mol/L KOH选择性结晶分离,Ni用0.3 mol/L H₂C₂O₄选择性沉淀分离。此法可回收约97.9%的NiO,纯度达98.3%;约25%的Al₂O₃以明矾(纯度为99%)形式回收,14.7%的Al₂O₃以Al-K-C₂O₄-SO₄盐的形式回收。研究结果表明,硫酸是一种合适的选择性浸出溶剂,而且可以从硫酸盐溶液中选择性结晶出明矾。TG-DTA/DTG和XRD表征研究证明,本工艺可以有效地提取和回收镍和铝。     

Co-extraction of valuable metals and kinetics analysis in chlorination process of low-grade nickel-copper sulfide ore

To efficiently co-extract Ni and Cu from low-grade nickel-copper sulfide ore, chlorination roasting with NH₄Cl followed by a water leaching process was investigated. The results show that 98.4% Ni and 98.5% Cu can be synchronously extracted when the ore particle size is 75-80 μm, the roasting time is 2 h, the mass ratio of NH₄Cl to ore is 1.6:1 and the roasting temperature is 550 °C. The evolution behavior of various minerals was elucidated using X-ray diffraction (XRD) coupled with scanning electron microscopy (SEM). The kinetics of the chlorination process based on the differential thermal and thermogravimetric analysis (DTA-TG) data was analyzed by Kissinger method and Flynn-Wall-Ozawa (FWO) method. The chlorination process of low-grade nickel-copper sulfide ore mainly contains two stages: the decomposition of NH₄Cl and the chlorination of ore. The maximum apparent activation energies (E_a) at two stages are determined to be 114.8 and 144.6 kJ/mol, respectively. The condensed product of exhaust gas is determined to be ammonium chloride, which can be recycled as the reactant again, making the process economic and clean.     

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.     

Leaching kinetics of selenium from copper anode slimes by nitric acid-sulfuric acid mixture

The leaching kinetics of selenium from copper anode slimes was studied in a nitric acid-sulfuric acid mixture. The effects of main parameters on selenium leaching showed that the leaching rate of selenium was practically independent of stirring speed, while dependent on temperature and the concentrations of HNO₃ and H₂SO₄. The leaching of selenium includes two stages. The activation energy in the first stage is 103.5 kJ/mol, and the chemical reaction is the rate controlling step. It was almost independent of H₂SO₄ concentration and dependent on HNO₃ concentration since the empirical reaction order with respect to HNO₃ concentration is 0.5613. In the second stage, the activation energy is 30.6 kJ/mol, and the process is controlled by a mixture of diffusion and chemical reaction. The leaching of selenium was almost independent of HNO₃ concentration.     

φ–pH diagram of As–N–Na–H2O system for arsenic removal during alkaline pressure oxidation leaching of lead anode slime

In order to illustrate the thermodynamic characteristics of arsenic during alkaline pressure oxidation leaching process of lead anode slime (NaNO₃ as oxidant; NaOH as alkaline reagent), the φ–pH diagrams of As–Na–H₂O, N–H₂O, As–N–Na–H₂O systems at ionic mass concentration of 0.1 mol/kg and temperatures of 298, 373, 423 and 473 K were established according to thermodynamic calculation. The results show that the existence forms of arsenic are associated with pH value, which mainly exists in the forms of H₃AsO₄, H₂AsO₄^?, HAsO₄^2?, and As₂O₃ in lower pH region, while it mainly exists in the form of when pH>11.14. High alkali concentration and high temperature are advantageous to the arsenic leaching. The alkaline pressure oxidation leaching experiments display that the tendency of arsenic leaching rate confirms the thermodynamic analysis results obtained from the φ–pH diagrams of As–N–Na–H₂O system, and the highest leaching rate of arsenic reaches 95.85% at 453 K.     

氟碳铈矿盐酸浸出过程的动力学

考察盐酸浓度、浸出温度、液固比和矿物粒度对浸出速度的影响.结果表明:在盐酸浓度6 mol/L、浸出温度90C、液固比15:1、矿物粒度25 μm的条件下浸出90 min后,氟碳铈矿中稀土碳酸盐的浸出率达到89.6％,而稀土氟化物的浸出率仪为1.5％.氟碳铈矿浸出过程符合产物层扩散模型,稀土碳酸盐和氟化物浸出过程的表观活...     

Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc residues by chloride

The leaching kinetics of silver and lead simultaneously from zinc residue by chloride was investigated.The effects of stirring speed,temperature,sodium chloride concentration,particle size and liquid/solid ratio on Ag and Pb dissolution in sodium chloride were studied.It was determined that the dissolution rates increased with increasing sodium chloride concentration,temperature and decreasing particle size.The dissolution kinetics followed a shrinking core model,with inter-diffusion through gangue layer as the rate determining step.This finding is in accordance with the apparent activation energy(Ea)of 26.8 kJ.mol-1(Ag)and 26.5 kJ.mo1-1(Pb),and a linear relationship between the rate constant and the reciprocal of squared particle size.The orders of reaction with respect to sodium chloride concentration,temperature and particle size were also achieved.The rate of reaction based on diffusion-controlled process can be expressed by semi-empirical equations.     

盐酸循环浸出强化钼酸钙焙砂分解及资源化回收钙

建立298 K下CaMoO4?CaSO4?H2SO4?H2O,CaMoO4?HCl?H2O和CaSO4?CaCl2?HCl?H2O体系的热力学平衡图.计算结果表明,硫酸钙在盐酸中的溶解度远大于在硫酸中的溶解度.从微观颗粒性质变化的角度探讨钼酸钙焙砂中钼的浸出机理.研究发现,盐酸对钼酸钙焙砂中的钼具有良好的浸出效果,这是...     

Molybdenite–limestone oxidizing roasting followed by calcine leaching with ammonium carbonate solution

Oxidizing roasting of molybdenite with lime can significantly reduce SO₂ pollution compared with the traditional roasting without lime. However, the calcine is subsequently leached by sulfuric acid, resulting in serious equipment corrosion and abundant non-recyclable CaSO₄ slag. In this work, a novel process, in which the molybdenite was roasted with CaCO₃ followed by (NH₄)₂CO₃ solution leaching, was proposed to improve the art of lime roasting–sulfuric acid leaching. Oxidizing roasting of molybdenite with CaCO₃ was investigated through thermodynamic calculation, thermogravimetric analysis and roasting experiments. The results show that the products of the oxidizing reaction of MoS₂ in the presence of CaCO₃ and O₂ are CaSO₄, CaMoO₄ and CO₂ at 573–1000 K. The MoS₂ conversion rate achieves approximately 99% and the sulfur-retained rate attains approximately 95% with a CaCO₃-to-MoS₂ molar ratio of 3.6 at 500 °C for 1 h by adding 5% mineralizer A (mass fraction). The leaching results show that the leaching rate of Mo reaches 98.2% at 85 °C for 7 h with a (NH₄)₂CO₃ concentration of 600 g/L and a liquid–solid ratio of 10 mL/g. The results presented are potential to develop a novel cleaner technique for ammonium molybdate production.     

Dynamics in simultaneous electro-generative leaching for sphalerite-MnO2

The principle for the electro-generative leaching was applied to simultaneous leaching of sphalerite-MnO2. A galvanic system for the bio-electro-generative leaching was set up. The effects of grain size and temperature on rate of zinc extraction fi＇om sphalerite under the conditions of presence and absence ofAcidithiobacillusferrooxidans （A.ferrooxidans） were studied, respectively. The results show that with bacteria, the maximum extraction of zinc fi＇om the ores with grain size of 16.6 μm can reach 32.01% after leaching for 12 h, while to obtain the same extraction ratio in the traditional bio-leaching route （i.e. not electro-generative one）10 d is needed to ore granules with same size. The unreacted shrinking core model was used for describing the reaction-relative and diffusion-relative phenomena presented in the process of the electro-generative leaching with and without bacteria, which is considered to be diffusion controlled. The activation energies of the anodic reaction for leaching system in the presence and absence of bacteria are 11.97 and 14.39 kj/mol, respectively, indicating that leaching rate can be decreased by A. ferrooxidans. SEM was used to study the effect ofA. ferrooxidans on the ores in the simultaneous electro-generative leaching, which indicates that the produced sulfur on the surface of the sulfides can be oxidized by A. ferrooxidans after bio-electro-generative leaching for 24 h, and the transferred charge due to the bacterial oxidation is up to 17.86%, which is an important part of the output electric quantity.     

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 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%.     

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.     

水热法批量制备粒径可控SnO2纳米粉体（英文）

以SnCl4·5H2O为前驱体、NH3·H2O为矿化剂,通过水热还原技术制备平均粒径在5～30nm的SnO2纳米粉末。系统研究小批量生产(1kg/批)条件下,工艺条件包括溶液浓度、反应温度、压力、时间和pH值对SnO2粒径、形貌和晶型的影响,并采用XRD、TEM等测试手段对样品进行表征。结果表明,在保持SnO2粉末晶型和形貌不变的前提下,通过调节反应温度、反应时间等工艺参数,粉末的粒径尺寸可以有效地控制在5～30nm范围内。不同于之前的报道,SnO2粒径尺寸随着反应时间(反应温度)的变化存在新的变化趋势,并推测解释了此晶粒异常生长的机理。     

Column leaching process of rare earth and aluminum from weathered crust elution-deposited rare earth ore with ammonium salts

In order to better understand the leaching process of rare earth (RE) and aluminum (Al) from the weathered crust elution-deposited RE ore, the mass transfer of RE and Al in column leaching was investigated using the chromatographic plate theory. The results show that a higher initial ammonium concentration in a certain range can enhance the mass transfer process. pH of leaching agent in the range of 2 to 8 almost has no effect on the mass transfer efficiency of RE, but plays a positive role in the mass transfer efficiency of Al under strong acidic condition (pH<4). There is an optimum flow rate that makes the highest mass transfer efficiency. The optimum leaching condition of RE is the leaching agent pH of 4–8, ammonium concentration of 0.4 mol/L and flow rate of 0.5 mL/min. The mass transfer efficiencies of RE and Al both follow the order: (NH₄)₂SO₄<NH₄Cl<NH₄NO₃, implying the complexing ability of anion.     

Dechromization and dealumination kinetics in process of Na2CO3-roasting pretreatment of laterite ores

A novel process was proposed for the activation pretreatment of limonitic laterite ores by Na₂CO₃ roasting. Dechromization and dealumination kinetics of the laterite ores and the effect of particle size, Na₂CO₃-ore mass ratio, and roasting temperature on Cr and Al extraction were studied. Experimental results indicate that the extraction rates of Cr and Al are up to 99% and 82%, respectively, under the optimal particle size of 44–74 μm, Na₂CO₃-to-ore mass ratio of 0.6:1, and temperature of 1000 °C. Dechromization within the range of 600–800 °C is controlled by the diffusion through the product layer with an apparent activation energy of 3.9 kJ/mol, and that it is controlled by the chemical reaction at the surface within the range of 900–1100 °C with an apparent activation energy of 54.3 kJ/mol. Besides, the Avrami diffusion controlled model with on apparent activation energy of 16.4 kJ/mol is most applicable for dealumination. Furthermore, 96.8% Ni and 95.6% Co could be extracted from the alkali-roasting residues in the subsequent pressure acid leaching process.