The efficient recycling of spent lithium iron phosphate(LiFePO_(4),also referred to as LFP)should convert Fe(Ⅱ)to Fe(Ⅲ),which is key to the extraction of Li and separation of Fe and is not well understood.Herein,we ...The efficient recycling of spent lithium iron phosphate(LiFePO_(4),also referred to as LFP)should convert Fe(Ⅱ)to Fe(Ⅲ),which is key to the extraction of Li and separation of Fe and is not well understood.Herein,we systematically study the oxidation of LiFePO_(4)in the air and in the solution containing oxidants such as H_(2)O_(2)and the effect of oxidation on the leaching behaviors of LFP.In the air,O_(2)breaks down the LFP olivine structure at 550℃for 1 h by oxidizing Fe(Ⅱ)to Fe(Ⅲ)in terms of converting LFP to Li_(3)Fe_(2)(PO_(4))_(3)and Fe_(2)O_(3).After that,Li is leached in 0.5 M sulfuric acid solution and is further recycled as Li_(3)PO_(4)with a Li recovery efficiency of 97.48%.Meanwhile,Fe is recovered as FePO_(4)and Fe_(2)O_(3).Compared with H_(2)SO_(4)-H_(2)O_(2),the air oxidation saves H_(2)O_(2)but increases the leaching efficiency of Fe and H_(2)SO_(4)consumption.The discrepancy of Fe leaching efficiency can be attributed to the different leaching mechanisms involving the solid-to-solid and solid-to-liquid-to-solid conversions.Furthermore,the results of the Everbatt model analysis show that the air roasting-H_(2)SO_(4)leaching method has low emission and potentially high income,which is simple and safe.Overall,this work will deepen the understanding of acid leaching of LFP and favorably stimulate the maturation of the LFP recycling technique.展开更多
In this study,a synergistic sulfidation-acid leaching process was proposed to recover valuable metals from gypsum residue and zinc-containing fume.The equilibrium phase composition of the sulfidation reaction and calc...In this study,a synergistic sulfidation-acid leaching process was proposed to recover valuable metals from gypsum residue and zinc-containing fume.The equilibrium phase composition of the sulfidation reaction and calculations of the thermodynamic stability region show that 89.36%Zn,>99%Pb and>99%Cu of gypsum residue and zinc-containing fume can be sulfured to ZnS,PbS and Cu 2 S,under sufficient sulfur partial pressure,low oxygen partial pressure and 400-1000℃.Sulfidation roasting experiments show that the sulfidation rate of Cu,Pb and Zn reach 81.43%,88.25% and 92.31%,respectively,under the roasting conditions of material mass ratio of 30 g:10 g,carbon dosage of 3.75 g,roasting temperature of 800℃ for 3 h.E−pH plots show that ZnS,PbS and Cu_(2)S can be enriched in the leaching residue,under leaching conditions at 25℃,pH<4 and-0.4 V<φ(E)<0.04 V.The leaching experiments showed that the sulfide is retained in the leaching residue,while the leaching rates of Cu,Pb and Zn are 1.94%,2.05% and 1.51%,respectively,under the conditions of 25℃,C_(HCl) of 0.5 mol/L,L/S of 5 mL/g,stirring rate of 300 r/min,and stirring time of 30 min.This study provides a new approach for the synergistic disposal of gypsum residue and zinc containing fume.展开更多
The demand for Ni and Co has surged due to the rapid expansion of the electric vehicle industry.Thus,developing efficient and eco-friendly metallurgical routes for extracting these metals has become imperative.This st...The demand for Ni and Co has surged due to the rapid expansion of the electric vehicle industry.Thus,developing efficient and eco-friendly metallurgical routes for extracting these metals has become imperative.This study introduces a sustainable and effective method for extracting Ni and Co from Ni–Co–Fe alloy powder obtained from limonitic laterite ores through selective reduction and magnetic separation.The leaching efficiency for Ni,Co,and Fe was 89.4%,94.8%,and 96.5%,respectively,under the following conditions for leaching:3 mol/L H_(2)SO_(4),85℃,10 m L/g liquid–solid ratio,and 90 min leaching time.The incorporation of H_(2)O_(2)enhanced the leaching efficiency for Ni,Co,and Fe.The redox potential of the solution plays a crucial role in acid dissolution,and H_(2)O_(2)enhances Ni and Co dissolution.Phosphate precipitation facilitated the removal of Fe from the leachate,affording a 96.1%Fe removal ratio and 2.29%Ni loss.展开更多
The process mineralogy of kaolin associated quartz flotation concentrate was studied.The experimental results show that the content of SiO2 in the flotation concentrate is 99.66%,and the main impurity elements in the ...The process mineralogy of kaolin associated quartz flotation concentrate was studied.The experimental results show that the content of SiO2 in the flotation concentrate is 99.66%,and the main impurity elements in the concentrate are Al,Fe,K,and Na.The gangue minerals in the flotation concentrate are mainly mica and feldspar symbiosis with quartz in the form of connexion or mineral inclusion.By taking the flotation concentrate as the raw material,the experimental research on HF concentration,HCl concentration,HNO3 concentration,acid leaching temperature,acid leaching time,and the leaching liquid solid ratio of hot pressing acid leaching conditions was carried out.Finally,the factors affecting the quality of purified products were analyzed.Through the acid leaching experiment,it can be seen that hydrofluoric acid has a greater effect on Al and Fe elements,hydrochloric acid has a greater effect on Fe elements,and nitric acid concentration has a smaller effect on impurity elements(which can also be confirmed from the thermodynamic analysis);the acid leaching temperature,the acid leaching time,and the leaching liquid solid mass ratio are proportional to the acid leaching effect.The Al content decreases from 1304.73 to 214.10μg/g,and the aluminum removal rate is 86.12%.The Fe content decreases from 39.35 to 3.72μg/g,and the iron removal rate is 90.55%.Thermodynamic and kinetic studies show that at 220℃,the chemical reaction between quartz and gangue minerals and the leaching agent can be spontaneous in the direction of positive reaction,and gangue minerals and the leaching agent had priority reaction.The mixed acid leaching process accords with the diffusion control model,Ea is 15.16 kJ/mol,which can provide a theoretical guidance for the purification of quartz.展开更多
The leaching behavior of metals from a nickeliferous limonitic laterite ore was investigated by high pressure acid leaching process for the extraction of nickel and cobalt.The effects of sulfuric acid added,leaching t...The leaching behavior of metals from a nickeliferous limonitic laterite ore was investigated by high pressure acid leaching process for the extraction of nickel and cobalt.The effects of sulfuric acid added,leaching temperature,leaching time and liquid/solid(L/S) ratio on metals extraction were examined.More than 97% Ni,96% Co,93% Mn,95% Mg and less than 1% Fe are extracted under optimum conditions.Analysis of the high pressure acid leaching residue by chemical and XRD analysis indicates that the residual iron and sulfur are mainly present in phases of hematite and alunite,respectively.The high pressure leaching process provides a simple and efficient way for the high recovery of nickel and cobalt from laterite ore,leaving residue as a suitable iron resource.展开更多
A method of activation roasting followed by acid leaching using titanium slag was introduced to prepare Ti-rich material. The effects of HaPO4 dosage, roasting temperature, and roasting time on TiO2 grade were investi...A method of activation roasting followed by acid leaching using titanium slag was introduced to prepare Ti-rich material. The effects of HaPO4 dosage, roasting temperature, and roasting time on TiO2 grade were investigated. A Ti-rich material containing 88.54% TiO2, 0.42% (CaO+MgO) was obtained when finely ground titanium slag was roasted with 7.5% H3PO4 at 1000 ℃ for 2 h, followed by a two-stage leaching in boiling dilute sulfuric acid for 2 h. The XRD patterns show that the product is titanium dioxide with a rutile structure. Mechanism studies show that structures of anosovite solid solution and silicate minerals are destroyed in the roasting process. As a result, titanium components in titanium slag are transformed into TiO2 (futile) while impurities are transformed into acid-soluble phosphate and quartz.展开更多
Zinc neutral leaching residue(ZNLR) from hydrometallurgical zinc smelting processing can be determined as hazardous intermediate containing considerable amounts of Cd and Zn which have great threats to the environme...Zinc neutral leaching residue(ZNLR) from hydrometallurgical zinc smelting processing can be determined as hazardous intermediate containing considerable amounts of Cd and Zn which have great threats to the environment. The ZNLR contained approximately 35.99% Zn, 15.93% Fe and 0.26% Cd, and Cd mainly existed as ferrites in the ZNLR in this research. Reductive acid leaching of ZNLR was investigated. The effects of hydrazine sulfate concentration, initial sulfuric acid concentration, temperature, duration and liquid-to-solid ratio on the extraction of Cd, Zn and Fe were examined. The extraction efficiencies of Cd, Zn and Fe reached 90.81%, 95.83% and 94.19%, respectively when the leaching parameters were fixed as follows: hydrazine sulfate concentration, 33.3 g/L; sulfuric acid concentration, 80 g/L; temperature, 95 °C; duration of leaching, 120 min; liquid-to-solid ratio, 10 m L/g and agitation, 400 r/min. XRD and SEM-EDS analyses of the leaching residue confirmed that lead sulfate(Pb SO4) and hydrazinium zinc sulfate((N2H5)2Zn(SO4)2) were the main phases remaining in the reductive leaching residue.展开更多
To analyze the thermodynamic characteristics of leaching process of converter slag, φ-pH diagram of V-Ti-H2O system at oxygen partial pressure of 0.5 MPa, ionic mass concentration of 0.1 mol/kg and temperatures rangi...To analyze the thermodynamic characteristics of leaching process of converter slag, φ-pH diagram of V-Ti-H2O system at oxygen partial pressure of 0.5 MPa, ionic mass concentration of 0.1 mol/kg and temperatures ranging from 60 to 200 ℃ was obtained by recently published critically assessed standard Gibbs energies and activity coefficients of various species. When pH2, stable regions of V3+, VO2+ and VO2+ exist in the stable region of TiO2. The pH values of stable regions of vanadium and titanium decrease and redox potentials become more positive with the temperature increasing. Vanadium and titanium could be separated by one-step leaching based on thermodynamics. The experiment results of pressure acid leaching of converter slag show that leaching rates of vanadium and titanium are 96.87% and 8.76% respectively, at 140 ℃ of temperature, 0.5 MPa of oxygen partial pressure, 0.055-0.075mm of particle size, 15:1 of liquid to solid ratio, 120 min of leaching time, 500 r/min of stirring speed and 200 g/L of initial acid concentration. Vanadium and titanium could be selectively separated in the pressure acid leaching process, and the experiment result is in agreement with thermodynamic calculation result.展开更多
The effects of oxidation-reduction treatment and mechanical activation on the hydrochloric acid leaching performance of Panxi ilmenite concentration were investigated.The results show that both of oxidation-reduction ...The effects of oxidation-reduction treatment and mechanical activation on the hydrochloric acid leaching performance of Panxi ilmenite concentration were investigated.The results show that both of oxidation-reduction treatment and mechanical activation significantly accelerate the extraction of Fe,Ca and Mg from Panxi ilmenite concentration;however,the CaO and MgO contents of the calcined residues obtained from oxidized-reduced ilmenite concentration are higher than the standard values required by chlorination process.The Ca and Mg in oxidized-reduced ilmenite concentration can be leached much faster after mechanical activation,yielding a synthetic rutile which meets the requirements of chlorination process containing 90.50% TiO2 and 1.37% total iron as well as combined CaO and MgO of 1.00%.The optimum oxidation and reduction conditions are as follows:oxidization at 900 ℃ in the presence of oxygen for 15 min and reduction at 750 ℃ by hydrogen for 30 min.展开更多
The leaching processes of zinc plant purification residue in sulfuric acid solution were investigated with respect to the effects of sulfuric acid concentration, reaction temperature, and particle size. A particle siz...The leaching processes of zinc plant purification residue in sulfuric acid solution were investigated with respect to the effects of sulfuric acid concentration, reaction temperature, and particle size. A particle size of 75?80 μm was required to leach 99.8%cobalt and 91.97%zinc at 70 °C for 20 min when the sulfuric acid concentration was 100 g/L and the ratio of liquid to solid was 50?1 (mL/g). The leaching kinetics of zinc plant purification residue in sulfuric acid solution system conformed well to the shrinking core model, and the dissolution rates of cobalt and zinc were found to be controlled by diffusion through a porous product layer. The apparent activation energy values of cobalt and zinc reaction were calculated to be 11.6931 kJ/mol and 6.6894 kJ/mol, respectively, according to the Arrhenius formula equation. The results show that diffusion through the inert particle pores is the leaching kinetics rate-controlling step.展开更多
[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with H...[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 (5:1) and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.展开更多
To extract molybdenum and nickel from the roasted Ni-Mo ore, a process of hydrochloric acid leaching, sulphation roasting and water leaching was investigated. The results showed that this process could get a high leac...To extract molybdenum and nickel from the roasted Ni-Mo ore, a process of hydrochloric acid leaching, sulphation roasting and water leaching was investigated. The results showed that this process could get a high leaching rate of Mo and Ni. Under the optimum conditions of hydrochloric acid leaching (roasted Ni-Mo ore leached with 0.219 mL/g hydrochloric acid addition at 65 ℃ for 30 min with a L/S ratio of 3 mL/g), sulphation roasting (51.9% sulfiaric acid addition, roasting temperature 240 ℃ for 1 h), followed by leaching with the first stage hydrochloric acid leaching solution at 95 ℃ for 2 h, the leaching rates of Mo and Ni reached 95.8% and 91.3%, respectively.展开更多
A technique including direct acid leaching, vanadium precipitation with alkaline, sodium hydroxide releaching, impurity removing by adjusting pH value, precipitation vanadium with ammonium chloride, and vanadium pento...A technique including direct acid leaching, vanadium precipitation with alkaline, sodium hydroxide releaching, impurity removing by adjusting pH value, precipitation vanadium with ammonium chloride, and vanadium pentoxide by roasting steps was proposed according to the characteristic of Xichuan clay vanadium mineral. The factors influencing leaching vanadium such as temperature and the concentration of sulfuric acid were investigated and optimized. The experimental results indicate that the extract ratios of V205 can reach 94% and 92% at a sodium chlorate ratio of 3% and a manganese dioxide ratio of 3%, respectivdy. A completely chemical precipitation method was adopted to decontaminate and enrich the vanadium in the acid leaching solution. The X-ray diffraction (XRD) pattern and the purity analysis of vanadium pentoxide indicate that the purity of final vanadium pentoxide can reach 99% and meet the standard specifications. The total recovery can reach about 75%. The technique has the characteristics of simplicity, less investment, and more environment safety as compared with the traditional salt roasting method.展开更多
Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various det...Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various determination methods. The effects of leaching time,leaching temperature,leaching agent concentration,leaching L/S ratio,granularity of material,additive consumption were investigated based on the mineralogy.The results show that under the conditions of leaching time of 3-4 h, temperature of 150℃,sulfuric acid consumption of 25%?30%,ratio of liquid to solid of 1.2:1,the granularity less than 0.074 mm, additive consumption of 3%-5%,and oxygen pressure of 1.2 MPa,and the vanadium leaching rate can be more than 92%by the method of two-step pressurized acid leaching.The powdery V2O5 product with 99.52%in V2O5 content is obtained by the flowsheet of acid recovery,removing iron by reduction process,solvent extraction,precipitating vanadium with ammonium water,and pyrolysis from the stone-coal oxygen pressure acid-leaching solution.The total recovery efficiency of vanadium is above 85%,which is more than 20%higher than that obtained in the conventional process.Furthermore,the new process does not cause air pollution since no HCl or Cl2 is released by calcination of the raw material.展开更多
The extraction of Sc by acid leaching with CaF2 and solvent extraction with P507 from red mud was proposed.The influence of acid leaching and solvent extraction on recovery of Sc was investigated.The CaF2 can obviousl...The extraction of Sc by acid leaching with CaF2 and solvent extraction with P507 from red mud was proposed.The influence of acid leaching and solvent extraction on recovery of Sc was investigated.The CaF2 can obviously improve the leaching efficiency of Sc and reduce the acid consumption.The leaching efficiency of Sc increases from 74%to 92%and the dosage of acid reduces under suitable conditions by adding 5%CaF2.The minerals in red mud can easily be decomposed and leached into the acid solution with CaF2 through analysis of XRD pattern.The particles of red mud become smaller and multihole.The Sc can be selectively extracted with 10%P507 at the pH value of 0.1 from the acid leaching solution.More than 98%of Sc and less than 10%of Al and Fe are extracted.The SC2O3 with purity of 99%is obtained after the process of reverse extraction with NaOH,H2SO4 dissolution,precipitation by oxalic acid and roasting at 750℃.展开更多
Hydrazine sulfate was used as a reducing agent for the leaching of Li,Ni,Co and Mn from spent lithium-ion batteries.The effects of the reaction conditions on the leaching mechanism and kinetics were characterized and ...Hydrazine sulfate was used as a reducing agent for the leaching of Li,Ni,Co and Mn from spent lithium-ion batteries.The effects of the reaction conditions on the leaching mechanism and kinetics were characterized and examined.97%of the available Li,96%of the available Ni,95%of the available Co,and 86%of the available Mn are extracted under the following optimized conditions:sulfuric acid concentration of 2.0 mol/L,hydrazine sulfate dosage of 30 g/L,solid-to-liquid ratio of 50 g/L,temperature of 80℃,and leaching time of 60 min.The activation energies of the leaching are determined to be 44.32,59.37 and 55.62 k J/mol for Li,Ni and Co,respectively.By performing X-ray diffraction and scanning electron microscopy in conjunction with energy dispersive X-ray spectroscopy,it is confirmed that the main phase in the leaching residue is MnO2.The results show that hydrazine sulfate is an effective reducing agent in the acid leaching process for spent lithium-ion batteries.展开更多
The kinetics of oxygen pressure acid leaching marmatite with high indium content was studied. The effects of particle size, agitation rate, temperature, HSOconcentration, and oxygen partial pressure on leaching rate o...The kinetics of oxygen pressure acid leaching marmatite with high indium content was studied. The effects of particle size, agitation rate, temperature, HSOconcentration, and oxygen partial pressure on leaching rate of indium were investigated. The results show that when the agitation rate is above 600 r-min, its influence on indium leaching rate is insignificant. It is determined that the leaching rates increase with the increase in sulfuric acid concentration, temperature, partial oxygen pressure, and the decrease in particle size. Moreover, the results demonstrate that the process of indium leaching is controlled by interface chemical reaction, with apparent activation energy of 65.7 k J-mol. The apparent reaction orders of sulfuric acid and oxygen partial pressure are determined to be 0.749 and 1.260, respectively. The leaching reaction process follows shrinking unreacted core model. And finally, the kinetics model equation is established for indium.展开更多
Selective recovery of scandium and titanium from red mud leaching solution was achieved through neutralization precipitation followed by acid leaching approach.In the neutralization precipitation section,the effects o...Selective recovery of scandium and titanium from red mud leaching solution was achieved through neutralization precipitation followed by acid leaching approach.In the neutralization precipitation section,the effects of pH,temperature and reaction time on metal precipitation efficiency were investigated.Under the optimal co ndition,the precipitation efficiencies of scandium and titanium were 93.74%and 99.47%,respectively.In the acid leaching section,the effects of acidity,temperature,reaction time,and raffinate to acid solution ratio on leaching efficiency were investigated.Under the optimal condition,the leaching efficiencies of scandium and titanium were 99.97%and 5.44%,respectively.The loss of scandium and titanium were 6.3%and 5.9%,respectively.Compared with the traditional extraction procedure of scandium in red mud,this method could separate titanium from scandium effectively,which is beneficial for the purification of the products and improvement of value of the metal.展开更多
The effects of the acid leaching and alkali fusion on the leaching efficiency of Y,Eu,Ce,and Tb from the waste rare earth fluorescent powders were investigated in this paper.The results show that hydrochloric acid is ...The effects of the acid leaching and alkali fusion on the leaching efficiency of Y,Eu,Ce,and Tb from the waste rare earth fluorescent powders were investigated in this paper.The results show that hydrochloric acid is better than sulfuric acid in the first acid leaching,and NaOH is better than Na2CO3in the alkali fusion.In the first acid leaching,the Wloss is 20.94%when the waste rare earth fluorescent powders are acid leached in H?concentration 3 mol L-1and S/L ratio 1:3 for 4 h due to red powders dissolved.The better results of the alkali fusion can be got at 800℃ for 2 h when the NaOH is used.The blue powders and the green powders can be dissolved into NaAlO2and oxides such as rare earth oxide(REO).The REO can be dissolved in H?concentration 5 mol L-1,S/L1:10 for 3 h in the second acid leaching.The leaching rates of the Y,Eu,Ce,and Tb are 99.06%,97.38%,98.22%,and 98.15%,respectively.The leaching rate of the total rare earth is 98.60%.展开更多
A new hydrometallurgical route for separation and recovery of Cu from Cu-As-bearing copper electrorefining black slime was developed. The proposed process comprised oxidation acid leaching of Cu-As-bearing slime and s...A new hydrometallurgical route for separation and recovery of Cu from Cu-As-bearing copper electrorefining black slime was developed. The proposed process comprised oxidation acid leaching of Cu-As-bearing slime and selective sulfide precipitation of Cu from the leachate. The effects of various process parameters on the leaching and precipitation of Cu and As were investigated. At the first stage, Cu extraction of 95.2% and As extraction of 97.6% were obtained at 80 ℃ after 4 h with initial H2 SO4 concentration of 1.0 mol/L and liquid-to-solid ratio of 10 mL/g. In addition, the leaching kinetics of Cu and As was successfully reproduced by the Avrami model, and the apparent activation energies were found to be 33.6 and 35.1 kJ/mol for the Cu and As leaching reaction, respectively, suggesting a combination of chemical reaction and diffusion control. During the selective sulfide precipitation, about 99.4% Cu was recovered as CuS, while only 0.1% As was precipitated under the optimal conditions using sulfide-to-copper ratio of 2.4:1, time of 1.5 h and temperature of 25 ℃.展开更多
基金supported by the Chilwee Group(No.CWDY-ZH-YJY-202101-001)the Fundamental Research Funds for the Central Universities(No.2042023kf0214)the Starting Funding from Wuhan University.
文摘The efficient recycling of spent lithium iron phosphate(LiFePO_(4),also referred to as LFP)should convert Fe(Ⅱ)to Fe(Ⅲ),which is key to the extraction of Li and separation of Fe and is not well understood.Herein,we systematically study the oxidation of LiFePO_(4)in the air and in the solution containing oxidants such as H_(2)O_(2)and the effect of oxidation on the leaching behaviors of LFP.In the air,O_(2)breaks down the LFP olivine structure at 550℃for 1 h by oxidizing Fe(Ⅱ)to Fe(Ⅲ)in terms of converting LFP to Li_(3)Fe_(2)(PO_(4))_(3)and Fe_(2)O_(3).After that,Li is leached in 0.5 M sulfuric acid solution and is further recycled as Li_(3)PO_(4)with a Li recovery efficiency of 97.48%.Meanwhile,Fe is recovered as FePO_(4)and Fe_(2)O_(3).Compared with H_(2)SO_(4)-H_(2)O_(2),the air oxidation saves H_(2)O_(2)but increases the leaching efficiency of Fe and H_(2)SO_(4)consumption.The discrepancy of Fe leaching efficiency can be attributed to the different leaching mechanisms involving the solid-to-solid and solid-to-liquid-to-solid conversions.Furthermore,the results of the Everbatt model analysis show that the air roasting-H_(2)SO_(4)leaching method has low emission and potentially high income,which is simple and safe.Overall,this work will deepen the understanding of acid leaching of LFP and favorably stimulate the maturation of the LFP recycling technique.
基金Projects(52174269,52374293)supported by the National Natural Science Foundation of ChinaProject(2022RC1123)supported by the Science and Technology Innovation Program of Hunan Province,China。
文摘In this study,a synergistic sulfidation-acid leaching process was proposed to recover valuable metals from gypsum residue and zinc-containing fume.The equilibrium phase composition of the sulfidation reaction and calculations of the thermodynamic stability region show that 89.36%Zn,>99%Pb and>99%Cu of gypsum residue and zinc-containing fume can be sulfured to ZnS,PbS and Cu 2 S,under sufficient sulfur partial pressure,low oxygen partial pressure and 400-1000℃.Sulfidation roasting experiments show that the sulfidation rate of Cu,Pb and Zn reach 81.43%,88.25% and 92.31%,respectively,under the roasting conditions of material mass ratio of 30 g:10 g,carbon dosage of 3.75 g,roasting temperature of 800℃ for 3 h.E−pH plots show that ZnS,PbS and Cu_(2)S can be enriched in the leaching residue,under leaching conditions at 25℃,pH<4 and-0.4 V<φ(E)<0.04 V.The leaching experiments showed that the sulfide is retained in the leaching residue,while the leaching rates of Cu,Pb and Zn are 1.94%,2.05% and 1.51%,respectively,under the conditions of 25℃,C_(HCl) of 0.5 mol/L,L/S of 5 mL/g,stirring rate of 300 r/min,and stirring time of 30 min.This study provides a new approach for the synergistic disposal of gypsum residue and zinc containing fume.
基金financially supported by the National Natural Science Foundation of China(Nos.52174288 and 51804346)。
文摘The demand for Ni and Co has surged due to the rapid expansion of the electric vehicle industry.Thus,developing efficient and eco-friendly metallurgical routes for extracting these metals has become imperative.This study introduces a sustainable and effective method for extracting Ni and Co from Ni–Co–Fe alloy powder obtained from limonitic laterite ores through selective reduction and magnetic separation.The leaching efficiency for Ni,Co,and Fe was 89.4%,94.8%,and 96.5%,respectively,under the following conditions for leaching:3 mol/L H_(2)SO_(4),85℃,10 m L/g liquid–solid ratio,and 90 min leaching time.The incorporation of H_(2)O_(2)enhanced the leaching efficiency for Ni,Co,and Fe.The redox potential of the solution plays a crucial role in acid dissolution,and H_(2)O_(2)enhances Ni and Co dissolution.Phosphate precipitation facilitated the removal of Fe from the leachate,affording a 96.1%Fe removal ratio and 2.29%Ni loss.
文摘The process mineralogy of kaolin associated quartz flotation concentrate was studied.The experimental results show that the content of SiO2 in the flotation concentrate is 99.66%,and the main impurity elements in the concentrate are Al,Fe,K,and Na.The gangue minerals in the flotation concentrate are mainly mica and feldspar symbiosis with quartz in the form of connexion or mineral inclusion.By taking the flotation concentrate as the raw material,the experimental research on HF concentration,HCl concentration,HNO3 concentration,acid leaching temperature,acid leaching time,and the leaching liquid solid ratio of hot pressing acid leaching conditions was carried out.Finally,the factors affecting the quality of purified products were analyzed.Through the acid leaching experiment,it can be seen that hydrofluoric acid has a greater effect on Al and Fe elements,hydrochloric acid has a greater effect on Fe elements,and nitric acid concentration has a smaller effect on impurity elements(which can also be confirmed from the thermodynamic analysis);the acid leaching temperature,the acid leaching time,and the leaching liquid solid mass ratio are proportional to the acid leaching effect.The Al content decreases from 1304.73 to 214.10μg/g,and the aluminum removal rate is 86.12%.The Fe content decreases from 39.35 to 3.72μg/g,and the iron removal rate is 90.55%.Thermodynamic and kinetic studies show that at 220℃,the chemical reaction between quartz and gangue minerals and the leaching agent can be spontaneous in the direction of positive reaction,and gangue minerals and the leaching agent had priority reaction.The mixed acid leaching process accords with the diffusion control model,Ea is 15.16 kJ/mol,which can provide a theoretical guidance for the purification of quartz.
文摘The leaching behavior of metals from a nickeliferous limonitic laterite ore was investigated by high pressure acid leaching process for the extraction of nickel and cobalt.The effects of sulfuric acid added,leaching temperature,leaching time and liquid/solid(L/S) ratio on metals extraction were examined.More than 97% Ni,96% Co,93% Mn,95% Mg and less than 1% Fe are extracted under optimum conditions.Analysis of the high pressure acid leaching residue by chemical and XRD analysis indicates that the residual iron and sulfur are mainly present in phases of hematite and alunite,respectively.The high pressure leaching process provides a simple and efficient way for the high recovery of nickel and cobalt from laterite ore,leaving residue as a suitable iron resource.
基金Project(NCET-10-0834) supported by the Program for New Century Excellent Talents in University,China
文摘A method of activation roasting followed by acid leaching using titanium slag was introduced to prepare Ti-rich material. The effects of HaPO4 dosage, roasting temperature, and roasting time on TiO2 grade were investigated. A Ti-rich material containing 88.54% TiO2, 0.42% (CaO+MgO) was obtained when finely ground titanium slag was roasted with 7.5% H3PO4 at 1000 ℃ for 2 h, followed by a two-stage leaching in boiling dilute sulfuric acid for 2 h. The XRD patterns show that the product is titanium dioxide with a rutile structure. Mechanism studies show that structures of anosovite solid solution and silicate minerals are destroyed in the roasting process. As a result, titanium components in titanium slag are transformed into TiO2 (futile) while impurities are transformed into acid-soluble phosphate and quartz.
基金Project(2012FJ1010)supported by the Key Project of Science and Technology of Hunan ProvinceChina+2 种基金Project(51474247)supported by the National Natural Science Foundation of ChinaProject(2012GS430201)supported by the Science and Technology Program for Public WellbeingChina
文摘Zinc neutral leaching residue(ZNLR) from hydrometallurgical zinc smelting processing can be determined as hazardous intermediate containing considerable amounts of Cd and Zn which have great threats to the environment. The ZNLR contained approximately 35.99% Zn, 15.93% Fe and 0.26% Cd, and Cd mainly existed as ferrites in the ZNLR in this research. Reductive acid leaching of ZNLR was investigated. The effects of hydrazine sulfate concentration, initial sulfuric acid concentration, temperature, duration and liquid-to-solid ratio on the extraction of Cd, Zn and Fe were examined. The extraction efficiencies of Cd, Zn and Fe reached 90.81%, 95.83% and 94.19%, respectively when the leaching parameters were fixed as follows: hydrazine sulfate concentration, 33.3 g/L; sulfuric acid concentration, 80 g/L; temperature, 95 °C; duration of leaching, 120 min; liquid-to-solid ratio, 10 m L/g and agitation, 400 r/min. XRD and SEM-EDS analyses of the leaching residue confirmed that lead sulfate(Pb SO4) and hydrazinium zinc sulfate((N2H5)2Zn(SO4)2) were the main phases remaining in the reductive leaching residue.
基金Project(2007CB613504)supported by the National Key Basic Research Program of ChinaProjects(51004033,50974035,51074047)supported by the National Natural Science Foundation of ChinaProject(2008BAB34B01)supported by National Science and Technology Support Plan of China during the 11th Five-Year Plan
文摘To analyze the thermodynamic characteristics of leaching process of converter slag, φ-pH diagram of V-Ti-H2O system at oxygen partial pressure of 0.5 MPa, ionic mass concentration of 0.1 mol/kg and temperatures ranging from 60 to 200 ℃ was obtained by recently published critically assessed standard Gibbs energies and activity coefficients of various species. When pH2, stable regions of V3+, VO2+ and VO2+ exist in the stable region of TiO2. The pH values of stable regions of vanadium and titanium decrease and redox potentials become more positive with the temperature increasing. Vanadium and titanium could be separated by one-step leaching based on thermodynamics. The experiment results of pressure acid leaching of converter slag show that leaching rates of vanadium and titanium are 96.87% and 8.76% respectively, at 140 ℃ of temperature, 0.5 MPa of oxygen partial pressure, 0.055-0.075mm of particle size, 15:1 of liquid to solid ratio, 120 min of leaching time, 500 r/min of stirring speed and 200 g/L of initial acid concentration. Vanadium and titanium could be selectively separated in the pressure acid leaching process, and the experiment result is in agreement with thermodynamic calculation result.
基金Project(2009FJ3082)supported by Research Project of Science and Technology in Hunan Province,ChinaProject(2007CB613606)supported by the National Basic Research Program of China
文摘The effects of oxidation-reduction treatment and mechanical activation on the hydrochloric acid leaching performance of Panxi ilmenite concentration were investigated.The results show that both of oxidation-reduction treatment and mechanical activation significantly accelerate the extraction of Fe,Ca and Mg from Panxi ilmenite concentration;however,the CaO and MgO contents of the calcined residues obtained from oxidized-reduced ilmenite concentration are higher than the standard values required by chlorination process.The Ca and Mg in oxidized-reduced ilmenite concentration can be leached much faster after mechanical activation,yielding a synthetic rutile which meets the requirements of chlorination process containing 90.50% TiO2 and 1.37% total iron as well as combined CaO and MgO of 1.00%.The optimum oxidation and reduction conditions are as follows:oxidization at 900 ℃ in the presence of oxygen for 15 min and reduction at 750 ℃ by hydrogen for 30 min.
基金Project(51072233)supported by the National Natural Science Foundation of China
文摘The leaching processes of zinc plant purification residue in sulfuric acid solution were investigated with respect to the effects of sulfuric acid concentration, reaction temperature, and particle size. A particle size of 75?80 μm was required to leach 99.8%cobalt and 91.97%zinc at 70 °C for 20 min when the sulfuric acid concentration was 100 g/L and the ratio of liquid to solid was 50?1 (mL/g). The leaching kinetics of zinc plant purification residue in sulfuric acid solution system conformed well to the shrinking core model, and the dissolution rates of cobalt and zinc were found to be controlled by diffusion through a porous product layer. The apparent activation energy values of cobalt and zinc reaction were calculated to be 11.6931 kJ/mol and 6.6894 kJ/mol, respectively, according to the Arrhenius formula equation. The results show that diffusion through the inert particle pores is the leaching kinetics rate-controlling step.
基金Supported by Science and Technology Planning Project of Zhejiang Province(2015C32001)Special Fund for Research Institutes from Science and Technology Department of Zhejiang Province(2016F30021)Natural Science Foundation of China(21407127)~~
文摘[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 (5:1) and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.
基金Project(51104186)supported by the National Natural Science Foundation of ChinaProjects(2016zzts282,2016zzts283)supported by the Fundamental Research Funds for the Central Universities of Central South University,China
文摘To extract molybdenum and nickel from the roasted Ni-Mo ore, a process of hydrochloric acid leaching, sulphation roasting and water leaching was investigated. The results showed that this process could get a high leaching rate of Mo and Ni. Under the optimum conditions of hydrochloric acid leaching (roasted Ni-Mo ore leached with 0.219 mL/g hydrochloric acid addition at 65 ℃ for 30 min with a L/S ratio of 3 mL/g), sulphation roasting (51.9% sulfiaric acid addition, roasting temperature 240 ℃ for 1 h), followed by leaching with the first stage hydrochloric acid leaching solution at 95 ℃ for 2 h, the leaching rates of Mo and Ni reached 95.8% and 91.3%, respectively.
基金This research was financially supported by the National Natural Science Foundation of China (No.20576137)the Major State Basic Research Development Program of China (No.2003CB716001).
文摘A technique including direct acid leaching, vanadium precipitation with alkaline, sodium hydroxide releaching, impurity removing by adjusting pH value, precipitation vanadium with ammonium chloride, and vanadium pentoxide by roasting steps was proposed according to the characteristic of Xichuan clay vanadium mineral. The factors influencing leaching vanadium such as temperature and the concentration of sulfuric acid were investigated and optimized. The experimental results indicate that the extract ratios of V205 can reach 94% and 92% at a sodium chlorate ratio of 3% and a manganese dioxide ratio of 3%, respectivdy. A completely chemical precipitation method was adopted to decontaminate and enrich the vanadium in the acid leaching solution. The X-ray diffraction (XRD) pattern and the purity analysis of vanadium pentoxide indicate that the purity of final vanadium pentoxide can reach 99% and meet the standard specifications. The total recovery can reach about 75%. The technique has the characteristics of simplicity, less investment, and more environment safety as compared with the traditional salt roasting method.
基金Project(2006AA06Z130)supported by the High-tech Research and Development Program of ChinaProject(50874053)supported by the National Natural Science Foundation of ChinaProject(2007GA010)supported by Science and Technology Bureau of Yunnan Province,China
文摘Vanadium extraction from stone-coal was investigated by oxygen pressure acid leaching and solvent extraction.The mineralogy of the stone-coal from Tongren City of Guizhou Province,China,was investigated by various determination methods. The effects of leaching time,leaching temperature,leaching agent concentration,leaching L/S ratio,granularity of material,additive consumption were investigated based on the mineralogy.The results show that under the conditions of leaching time of 3-4 h, temperature of 150℃,sulfuric acid consumption of 25%?30%,ratio of liquid to solid of 1.2:1,the granularity less than 0.074 mm, additive consumption of 3%-5%,and oxygen pressure of 1.2 MPa,and the vanadium leaching rate can be more than 92%by the method of two-step pressurized acid leaching.The powdery V2O5 product with 99.52%in V2O5 content is obtained by the flowsheet of acid recovery,removing iron by reduction process,solvent extraction,precipitating vanadium with ammonium water,and pyrolysis from the stone-coal oxygen pressure acid-leaching solution.The total recovery efficiency of vanadium is above 85%,which is more than 20%higher than that obtained in the conventional process.Furthermore,the new process does not cause air pollution since no HCl or Cl2 is released by calcination of the raw material.
基金Project supported by the National Natural Science Foundation of China(51804103,51904097)Fundamental Research Funds for the Universities of Henan Province(NSFRF180319)the Scientific and Technological Project of Henan Province(172102310679,182102310846)。
文摘The extraction of Sc by acid leaching with CaF2 and solvent extraction with P507 from red mud was proposed.The influence of acid leaching and solvent extraction on recovery of Sc was investigated.The CaF2 can obviously improve the leaching efficiency of Sc and reduce the acid consumption.The leaching efficiency of Sc increases from 74%to 92%and the dosage of acid reduces under suitable conditions by adding 5%CaF2.The minerals in red mud can easily be decomposed and leached into the acid solution with CaF2 through analysis of XRD pattern.The particles of red mud become smaller and multihole.The Sc can be selectively extracted with 10%P507 at the pH value of 0.1 from the acid leaching solution.More than 98%of Sc and less than 10%of Al and Fe are extracted.The SC2O3 with purity of 99%is obtained after the process of reverse extraction with NaOH,H2SO4 dissolution,precipitation by oxalic acid and roasting at 750℃.
基金Project(51674298)supported by the National Natural Science Foundation of ChinaProject supported by Anhui Province Research and Development Innovation Program,China。
文摘Hydrazine sulfate was used as a reducing agent for the leaching of Li,Ni,Co and Mn from spent lithium-ion batteries.The effects of the reaction conditions on the leaching mechanism and kinetics were characterized and examined.97%of the available Li,96%of the available Ni,95%of the available Co,and 86%of the available Mn are extracted under the following optimized conditions:sulfuric acid concentration of 2.0 mol/L,hydrazine sulfate dosage of 30 g/L,solid-to-liquid ratio of 50 g/L,temperature of 80℃,and leaching time of 60 min.The activation energies of the leaching are determined to be 44.32,59.37 and 55.62 k J/mol for Li,Ni and Co,respectively.By performing X-ray diffraction and scanning electron microscopy in conjunction with energy dispersive X-ray spectroscopy,it is confirmed that the main phase in the leaching residue is MnO2.The results show that hydrazine sulfate is an effective reducing agent in the acid leaching process for spent lithium-ion batteries.
基金financially supported by the National High-Tech Research and Development Program of China (No. 2012AA062303)the National Natural Science Foundation of China (Nos. U1402271, 51504059 and 51504058)
文摘The kinetics of oxygen pressure acid leaching marmatite with high indium content was studied. The effects of particle size, agitation rate, temperature, HSOconcentration, and oxygen partial pressure on leaching rate of indium were investigated. The results show that when the agitation rate is above 600 r-min, its influence on indium leaching rate is insignificant. It is determined that the leaching rates increase with the increase in sulfuric acid concentration, temperature, partial oxygen pressure, and the decrease in particle size. Moreover, the results demonstrate that the process of indium leaching is controlled by interface chemical reaction, with apparent activation energy of 65.7 k J-mol. The apparent reaction orders of sulfuric acid and oxygen partial pressure are determined to be 0.749 and 1.260, respectively. The leaching reaction process follows shrinking unreacted core model. And finally, the kinetics model equation is established for indium.
基金Project supported by the National Natural Science Foundation of China(21707167)。
文摘Selective recovery of scandium and titanium from red mud leaching solution was achieved through neutralization precipitation followed by acid leaching approach.In the neutralization precipitation section,the effects of pH,temperature and reaction time on metal precipitation efficiency were investigated.Under the optimal co ndition,the precipitation efficiencies of scandium and titanium were 93.74%and 99.47%,respectively.In the acid leaching section,the effects of acidity,temperature,reaction time,and raffinate to acid solution ratio on leaching efficiency were investigated.Under the optimal condition,the leaching efficiencies of scandium and titanium were 99.97%and 5.44%,respectively.The loss of scandium and titanium were 6.3%and 5.9%,respectively.Compared with the traditional extraction procedure of scandium in red mud,this method could separate titanium from scandium effectively,which is beneficial for the purification of the products and improvement of value of the metal.
基金supported by the National Hi-Tech R&D Program of China (No. 2012AA063202)National Key Project of Scientific and Technical Support Program of China (Nos. 2011BAE13B07, 2012BAC02B01, and 2011BAC10B02)National Natural Science Foundation of China (Nos. 51174247 and 50972013)
文摘The effects of the acid leaching and alkali fusion on the leaching efficiency of Y,Eu,Ce,and Tb from the waste rare earth fluorescent powders were investigated in this paper.The results show that hydrochloric acid is better than sulfuric acid in the first acid leaching,and NaOH is better than Na2CO3in the alkali fusion.In the first acid leaching,the Wloss is 20.94%when the waste rare earth fluorescent powders are acid leached in H?concentration 3 mol L-1and S/L ratio 1:3 for 4 h due to red powders dissolved.The better results of the alkali fusion can be got at 800℃ for 2 h when the NaOH is used.The blue powders and the green powders can be dissolved into NaAlO2and oxides such as rare earth oxide(REO).The REO can be dissolved in H?concentration 5 mol L-1,S/L1:10 for 3 h in the second acid leaching.The leaching rates of the Y,Eu,Ce,and Tb are 99.06%,97.38%,98.22%,and 98.15%,respectively.The leaching rate of the total rare earth is 98.60%.
基金financial supports from the National Natural Science Foundation of China (51634010,51904354)the National Science Fund for Distinguished Young Scholars of China (51825403)+1 种基金the National Key R&D Program of China (2018YFC1900306,2019YFC1907405)Key Research and Development Program of Hunan Province,China (2019SK2291)。
文摘A new hydrometallurgical route for separation and recovery of Cu from Cu-As-bearing copper electrorefining black slime was developed. The proposed process comprised oxidation acid leaching of Cu-As-bearing slime and selective sulfide precipitation of Cu from the leachate. The effects of various process parameters on the leaching and precipitation of Cu and As were investigated. At the first stage, Cu extraction of 95.2% and As extraction of 97.6% were obtained at 80 ℃ after 4 h with initial H2 SO4 concentration of 1.0 mol/L and liquid-to-solid ratio of 10 mL/g. In addition, the leaching kinetics of Cu and As was successfully reproduced by the Avrami model, and the apparent activation energies were found to be 33.6 and 35.1 kJ/mol for the Cu and As leaching reaction, respectively, suggesting a combination of chemical reaction and diffusion control. During the selective sulfide precipitation, about 99.4% Cu was recovered as CuS, while only 0.1% As was precipitated under the optimal conditions using sulfide-to-copper ratio of 2.4:1, time of 1.5 h and temperature of 25 ℃.