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2025 Volume 44 Issue 5  Published: 2025-10-20
    Reviews
  • Xinping WANG , Zongying CAI , Weigang CAO , Yunhe MO , Yun WEN
    doi: 10.13355/j.cnki.sfyj.2025.05.001

    Cobalt vanadate, as the anode material of lithium-ion batteries, has attracted much attention due to its characteristics such as high specific capacity, excellent rate performance and environmental friendliness. Several common structures of cobalt vanadate anode materials are introduced. The research progress of the main synthesis and modification methods of this material is elaborated with emphasis, including hydrothermal synthesis method, co-precipitation synthesis method and electrospinning synthesis method, as well as composite modification, surface modification and ion doping modification methods, etc. The key synthesis and modification research directions and application prospects of this material in the future are also prospectively presented.

  • Experiment Research
  • Linsen WEI , Shaoyan PAN , Xuan LI , Xiaoyan XIANG
    doi: 10.13355/j.cnki.sfyj.2025.05.002

    During the process of extracting vanadium from vanadium slag by sodium roasting-water leaching method, silicon in the leaching solution will react with alkali to form sodium silicate and enter the solution, affecting the recovery rate and quality of the product. To address this issue, the selective precipitation of silicon in vanadium leachate by the magnesium salt method was studied. Thermodynamic equilibrium diagrams of the Mg-Si-V-H2O system were constructed to investigate the distribution characteristics of free ions within the pH range of 7~14. Additionally, the relationship between pH and precipitation saturation indices was established to evaluate the precipitation behaviors of MgSiO3 and Mg(VO3)2 under different pH conditions. The calculation results reveal that the solubility of MgSiO3 is relatively low, while that of Mg(VO3)2 is relatively high, which can achieve the selective precipitation of silicon in the vanadium leaching solution. The verification test results demonstrate that the pH of the solution has a significant influence on the precipitation rate of silicon in the vanadium leaching solution. When pH=10, the silicon precipitation rate can reache 86.3%, and the vanadium loss rate is only 3.2%, with a good effect.

  • Experiment Research
  • Jia MA , Guang LI , Kaikai YE , Chunfeng LI , Yuhui TIAN , Chen ZHANG , Shouxun ZHANG , Xianming HOU
    doi: 10.13355/j.cnki.sfyj.2025.05.003

    Xinjiang hydrothermal uranium-beryllium deposit is a critical polymetallic resource in China, yet the occurrence characteristics of uranium and its migration behavior during beneficiation and metallurgy remain unclear. The occurrence state of uranium and its migration patterns during flotation-leaching processes were systematically investigated through multi-scale mineralogical characterization techniques (polarizing microscope, SEM, AMICS, EPMA). The results indicate that uranium primarily occurs in uranophane (76%), pitchblende (16%), and kasolite (6%). Uranium minerals exhibit fine dissemination sizes (10~70 μm) and low liberation degrees (<5%). The samples needs to be further finely ground to increase the dissociation degree of uranium minerals, so that they can fully contact the flotation reagents, thereyby ensuring the beneficiation effect. Among these factors, uranophane is a primary constraint on uranium leaching due to its fine-grained encapsulation and potential formation of surface silica gel coatings during leaching. While grinding the raw ore to -45 μm significantly improves mineral liberation, insufficient selectivity of flotation reagents results in non-significant distribution patterns between beryllium concentrate and tailings. Sulfuric acid roasting effectively decomposes silicate frameworks, achieving a uranium leaching rate exceeding 99%. The study can provide theoretical insights for optimizing the co-extraction of uranium and beryllium from complex polymetallic ores.

  • Experiment Research
  • Ziqin LIN , Chen ZHANG , Yongtao LIU , Jie SUI , Jiwei LU , Zhitao YUAN , Yubao HUO , Shuo LIU , Xianming HOU
    doi: 10.13355/j.cnki.sfyj.2025.05.004

    In response to the issue that traditional beneficiation processes and direct leaching methods are difficult to achieve economically effective recovery for a certain low-grade and refractory molybdenum oxide ore, based on its process mineralogical characteristics, the application of superconducting magnetic separation for pre-enrichment of the low-grade and refractory molybdenum oxide ore was studied. The effects of magnetic separation conditions such as background magnetic field strength, slurry flow velocity, separation slurry concentration, slurry feeding method and other magnetic separation conditions on the pre-enrichment concentrate indicators were investigated. The results show that by adopting the upper feeding method and under the suitable conditions of background magnetic field strength of 4 T, slurry flow velocity of 0.025 m/s, and separation slurry concentration of 10%, the pre-enrichment concentrate has Mo grade of 0.75% and recovery rate of 64%. Through theoretical calculation and recovery mechanism analysis of the magnetic separation recovery process, a high-efficiency separation scheme is optimized and designed, which includes coarse (-0.5 mm+0.025 mm) and fine (-0.025 mm) particle size classification and separation processes, as well as the coordinated matching of high magnetic field strength (5 T) and high flow rate (0.04 m/s). The final process indicators are:Mo grade in the concentrate of 0.88%, recovery rate of 63.79%, and enrichment ratio of 3.95. The method can achieve the goal of efficient pre-enrichment of low-grade and refractory molybdenum oxide ores, meet the feed grade requirements of subsequent leaching processes, and has certain application potential.

  • Experiment Research
  • Lingfei YU , Beiping ZHU , Zelin ZHANG , Xianguo SHI , Xianyou CHEN
    doi: 10.13355/j.cnki.sfyj.2025.05.005

    For zinc acid leaching residue, the reduction leaching of zinc, iron and copper and the enrichment of lead and silver were studied by using zinc concentrate as the reducing agent and zinc smelting waste electrolyte as the leaching agent under micro-pressure conditions. The micro-pressure reduction leaching residue was then leached with hot acid. The effects of various factors on the two-stage leaching were investigated. The results show that the optimal conditions for micro-pressure reduction leaching are pressure of 0.2 MPa, final acid concentration of 35 g/L, reaction temperature of 100 ℃, liquid volume to solid mass ratio of 8/1, zinc concentrate addition of 1.1 times the theoretical amount, stirring speed of 400 r/min, and reaction time of 2 h. The micro-pressure reduction leaching residue obtained under these conditions was leached with hot acid at 90 ℃ and a final acid concentration of 110 g/L for 2 h. The total leaching rates of zinc, iron and copper after the two-stage leaching can reach 95.81%, 92.67% and 92.63%, respectively, and the residue rate is 24.61% of the zinc acid leaching residue, which can achieve the reduction of the residue. Lead and silver are enriched in the hot acid leaching residue, with a sulfur mass fraction of 23.42%. The leaching residue has a high content of valuable metals and strong potential for self-heating. The method utilizes the reducing property of zinc concentrate and the oxidizing property of Fe3+ in the zinc acid leaching residue leaching solution to achieve efficient and comprehensive recovery of zinc acid leaching residue, and has certain application and promotion value.

  • Experiment Research
  • Pengfei YANG , Sheng ZHANG , Junfeng LAN , Youming YE , Xuezhen XIE , Yanmeng CHEN
    doi: 10.13355/j.cnki.sfyj.2025.05.006

    High efficient and selective recovery of lithium from spent LiFePO4 batteries by hydrogen peroxide oxidative leaching method was studied. The effects of hydrogen peroxide concentration, solid mass to liquid volume ratio, leaching temperature and time on the leaching behavior of lithium were examined. Kinetic analysis, XRD and SEM were used to investigate the leaching mechanism. The results show that under the optimal conditions of hydrogen peroxide concentration of 20%, solid mass to liquid volume ratio of 3 mg/1 mL, leaching temperature of 40 ℃ and leaching time of 40 min, the leaching rate of lithium can reach 99%, while the leaching rate of iron is only 0.53%, and the leaching process is mainly controlled by internal diffusion. The method can provide technical support for the efficient selection and recovery of lithium in spent LiFePO4 batteries.

  • Experiment Research
  • Wenpeng XIE , Suling YAO , Yuanpeng FU , Xianshu DONG
    doi: 10.13355/j.cnki.sfyj.2025.05.007

    Iron and fluorine co-doped manganese ion sieve HMFeO-F was prepared by high temperature solid phase method. The effects of calcination temperature, calcination time and doping ratio on the structure of the ion sieve were investigated by XRD, SEM, FT-IR and BET, and its adsorption performance was studied. The results show that the adsorption capacity for lithium of HMFeO-F is 31.57 mg/g under the conditions of calcination temperature of 800 ℃, calcination time of 10 h, molar ratio of lithium to manganese of 1/2, and doping mole fractions of Fe and F of 5% and 10%, respectively. The Mn dissolution loss rate during the adsorption process is only 4.52%, which is 61% lower than that of the undoped. At the same time, the introduction of magnetic Fe3O4 makes the magnetic recovery rate of the material can reach 90.2%. After five cycles of tests, the equilibrium adsorption capacity for lithium of HMFeO-F can still reach 25.87 mg/g, and the manganese dissolution loss rate remains within 5%. For a coal gangue acid leaching solution with a lithium mass concentration of 12.98 mg/L, lithium is adsorbed by HMFeO-F, and the lithium adsorption rate can reach 99%. The use of ion sieve to extract lithium from coal gangue can not only develop a new way to extract lithium, but also is expected to achieve the high-value utilization of coal gangue.

  • Experiment Research
  • Zhiyu XIONG , Yuemei MAO , Shiyou LI , Jiayao LIU , Qiqi DENG , Taotao ZENG
    doi: 10.13355/j.cnki.sfyj.2025.05.008

    The original biochar (BC) was prepared by pyrolysis using chestnut shells as raw materials, and then the phosphate-modified nitrogen-doped biochar (NP-BC) was prepared by nitrogen doping and phosphate modification methods. The adsorption performance of BC and NP-BC for uranium in wastewater was investigated. The surface morphology and elements of BC and NP-BC were analyzed by means of SEM, EDS, BET, FT-IR and XPS, and the adsorption mechanism of BC and NP-BC for uranium was discussed. The results show that for the wastewater with an initial mass concentration of uranium of 10 mg/L and initial pH of 4, under the conditions of NP-BC dosage of 0.2 g/L and reaction temperature of 30 ℃, the adsorption removal rate of U(Ⅵ) can reach 99.32%. The influence of coexisting anions and cations on the division of U(Ⅵ) in NP-BC increases with the increase of ion concentration. The adsorption process is more suitable to be described by the pseudo-second-order kinetic model and the Langmuir isothermal adsorption model. It is concluded through FT-IR and XPS analysis that the adsorption mechanism of uranium by NP-BC is the coordination effect and reduction effect of oxygen-containing functional groups, nitrogen-containing functional groups and phosphate groups.

  • Experiment Research
  • Qingli GAO , Yan CUI , Yan LIN
    doi: 10.13355/j.cnki.sfyj.2025.05.009

    In the process of extracting antimony by alkaline electro-deposition, problems such as cracking of the cathode deposited antimony, causing warping and shedding, occur due to insufficient interfacial bonding force between Sb and Fe, surface sandblasting pretreatment technology was proposed. The effects of the sandblasting pretreatment on the cathodic reduction and nucleation mechanism of antimony ions were systematically analyzed by combining cyclic voltammetry, steady-state polarization curves, and time-current transient curves. The results show that for the alkaline electro-deposition system of antimony, after sandblasting pretreatment of the iron-based cathode surface, the initial potential of the cathodic reduction reaction shifts to the left and positive. At the same overpotential, the current density is significantly increased compared to that without sandblasting treatment, and transfer coefficient and exchange current density are also enhanced. This indicates that the sandblasting treatment of the cathode surface can reduce the energy barrier of the cathodic reduction reaction of antimony ions, significantly increase the reduction reaction rate, and promote the three-dimensional nucleation process of antimony on the cathode surface, thereby obtaining a dense. well-shaped cathode antimony deposit layer. Further in-depth research was conducted on the influence of sandblasting particle size on the antimony electro-deposition process, and the optimal sandblasting particle size was determined to be 80 mesh. Under the condition, the cathode current efficiency is increased to 80.1%, the cell voltage is 2.031 V, the direct current power consumption per ton of antimony is reduced to 1674.76 kW·h/t, and the purity of cathode antimony reaches 98.81%.

  • Experiment Research
  • Kai WANG
    doi: 10.13355/j.cnki.sfyj.2025.05.010

    To address the issue of low extraction efficiency of aluminum from fly ash in pulverized coal furnaces due to its mullite structure, a process combining high—temperature enhanced decalcification with medium recycling to remove calcium and extract alumina from activated fly ash clinker was proposed. The optimal process parameters for decalcification and alumina extraction were determined through single-factor experiments. The results indicate that the optimal decalcification conditions are reaction temperature of 160 ℃, hydrochloric acid concentration of 12%, and reaction time of 4 h. Under the conditions, the CaO removal rate exceeds 98%, while the Al2O3 dissolution rate is effectively suppressed below 5%. The optimal alumina extraction conditions are temperature of 60 ℃, hydrochloric acid concentration of 26%, and reaction time of 0.5 hours, achieving an Al2O3 dissolution rate of over 93% and controlling the Ca2+ concentration in the leachate below 0.39 g/L. Innovatively, a closed-loop calcium chloride recycling system is constructed, enabling recovery rate of over 90% for the activator in filtrate reuse tests. The process can achieve efficient calcium-aluminum separation and recycling of additives, offering a low-carbon solution for alumina extraction from fly ash.

  • Experiment Research
  • Muyi CHENG , Jiafeng WANG , Youdong FANG , Chang SU , Ningning LYU
    doi: 10.13355/j.cnki.sfyj.2025.05.011

    The phosphorus content in sludge incineration ash is relatively high. Extracting and recovering it can effectively alleviate the contradiction between the supply and demand of phosphorus. Leaching of phosphorus from sludge incineration ash with nitric acid was studied. The effects of nitric acid concentration, leaching temperature, leaching time and the ratio of liquid volume to solid mass on the leaching rate of phosphorus were investigated. The restrictive links of phosphorus leaching were determined and the kinetic equation was established. The results show that under the conditions of nitric acid concentration of 1 mol/L, temperature of 298 K, leaching time of 60 min, stirring speed of 500 r/min, and liquid volume to solid mass ratio of 40 mL/1 g, the leaching rate of phosphorus reaches 91.36%. Internal diffusion control is the limiting link in the phosphorus leaching process, and the activation energy of the leaching reaction is 2.11 kJ/mol. The method has a relatively high phosphorus extraction efficiency. It is an efficient and feasible technology for recovering phosphorus from sludge incineration ash and can provide an important technical approach to alleviate the contradiction between supply and demand of phosphorus resources.

  • Experiment Research
  • Meimei PAN , Kui HUANG , Haili DONG , Zhangqing CHEN , Shanjin MAO
    doi: 10.13355/j.cnki.sfyj.2025.05.012

    The composition and physicochemical properties of waste lead paste are complex, and its recycling and utilization are difficult. Among them, the reduction of high-valent PbO2 is a key problem in the recycling and treatment process of waste lead paste. The reduction sulfation reaction of converting PbO2 in waste lead paste to PbSO4 using the glucose-sulfuric acid system at room temperature was studied. The effects of sulfuric acid concentration, glucose excess coefficient, liquid volume to solid mass ratio and reaction time on the reduction sulfation process of waste lead paste were investigated. The results show that under the optimal reaction conditions of waste lead paste of 5 g, sulfuric acid concentration of 85%, excess coefficient of glucose of 3, liquid volume to solid mass ratio of 3/1, and reaction time of 3 h, the reduction rate of PbO2 is 91.88% and the mass fraction of PbSO4 is 92.52%. The system can reduce and sulfate various complex components in waste lead paste to obtain PbSO4 products of higher purity. It is green and efficient, and convenient for the subsequent recycling and treatment of waste lead paste.

  • Experiment Research
  • Zhaochun YE , Yuanzhi YE , Fei ZHANG , Zhaorong LUO , Zhiyan ZHONG
    doi: 10.13355/j.cnki.sfyj.2025.05.013

    Using high-tellurium copper crude selenium as raw material, the process of preparing 4N selenium powder by high temperature oxidatio—water dissolution-low temperature reduction—temperature rise transformation was studied. The effects of key process parameters in each process on the purification of crude selenium to prepare 4N selenium powder were investigated, and the reduction reaction of selenium and the competitive behavior of selenium and tellurium were analyzed based on thermodynamic theory. The results show that under the optimal process conditions of oxidation temperature of 550 ℃, oxidation time of 3.0 h, oxygen flow rate of 2.5 m3/h, reduction temperature of 25 ℃, hydrazine hydrate concentration of 15%, stirring speed of 300 r/min, reaction endpoint solution pH=6.5, and transformation temperature of 55 ℃, the selenium product can meet the standard of 4N selenium powder. The method can provide a new technical route for the production of high-purity 4N grade selenium.

  • Experiment Research
  • Xicong LYU , Wentao TANG , Zhujun LIANG , Yuandong LIU , Mengxue LI
    doi: 10.13355/j.cnki.sfyj.2025.05.014

    Removal of impurities (arsenic, antimony, bismuth) from copper electrolytic waste liquid by hydrogen sulfide was studied. The effects of the excess coefficient of hydrogen sulfide, reaction temperature, reaction time and stirring speed on the impurity removal of copper electrolytic waste liquid were investigated. The experimental conditions were further optimized by the response surface methodology, and the experiments were verified under these conditions. The results show that the optimal test conditions are as follows:the excess coefficient of hydrogen sulfide is 1.9, the reaction temperature is 68.1 ℃, the reaction time is 2.1 h, and the stirring speed is 524 r/min. Under the optimal conditions, the average impurity removal rate of copper electrolysis waste liquid can reach 94.2%. The optimized process parameters determined by the method are reliable and applicable, and will not affect the subsequent recovery of nickel elements.

  • Experiment Research
  • Yunlong CAI
    doi: 10.13355/j.cnki.sfyj.2025.05.015

    A big data-driven hydrometallurgical full-process optimization control model was proposed. Firstly, a LSTM model based on improved attention mechanism was constructed, and the self-attention mechanism was used to enhance the model’s attention to key time steps to improve the prediction accuracy. Secondly, the dynamic adjustment and control of real-time production parameters are realized by using DDQN algorithm improved by priority experience playback. Finally, the optimal control model of economic benefit of the whole process is designed to obtain the optimal solution. The results show that the coefficient of determination R2 of the model is 0.92, 0.90, 0.92 in different numerical simulations, which shows that the model is superior to the traditional method in many aspects.

  • Experiment Research
  • Yifan ZHOU
    doi: 10.13355/j.cnki.sfyj.2025.05.016

    To address the problem of low prediction accuracy and large noise data in gold leaching rate prediction, a high-efficiency intelligent prediction method was proposed. Combining the improved XGBoost and LightGBM models, a dynamic learning rate, regularization optimization, and Bayesian optimization algorithm were used to design an ensemble learning model for gold leaching rate prediction. The results show that the ensemble learning model has a significantly improved prediction accuracy compared to traditional single models, and its MSE is about 28.8% and 22.9% lower than XGBoost and LightGBM, respectively. The model has high stability in real production environments. The ensemble learning model can effectively improve the prediction accuracy of gold leaching rate and has strong practical application value.