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Comparative Analysis of Sulfation Roasting-Water Leaching Process for Recovery of NdFeB and CeFeB Wastes

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 1-7
A separate CeO2phase appears in the oxidized material of CeFeB waste and changes its valence state during the sulfation roasting process,which differs from NdFeB waste.Therefore,this paper conducted a comparative analysis of the sulfation roasting process of the oxidized materials of these two wastes.The research results show that the highest sulfation rates of the oxidized materials of NdFeB and CeFeB wastes are 91.7%and 96.1%,respectively.The sulfation process of the former mainly occurs in the medium-temperature roasting stage,while that of the latter mainly occurs in the low-temperature infiltration stage with the generation of an intermediate Ce(SO4)2in the medium-temperature roasting stage.The final products of sulfation roasting for both are Fe2O3and RE2(SO4)3.Their high-temperature roasted materials have an loose structure with uneven pore size,and most of the rare earth-rich phases are encapsulated by the non-rare earth phases.Apart from CeO2,the roasting mechanism of the CeFeB waste is consistent with that of the NdFeB waste:rare earth oxides and Fe2O3reacts with sulfuric acid to generate water-soluble rare earth sulfates and Fe2(SO4)3;Fe2SO43is decomposed into Fe2O3and SO3at high temperature,and SO3further reacts with unreacted rare earth oxides to generate rare earth sulfates.CeO2reacts with sulfuric acid to form Ce(SO42at first,which is then decomposed into Ce2(SO4)3.The SO3generated during the decomposition process further reacts with CeO2to generate water-soluble Ce2(SO4)3.
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Research on the Recycling Process of Praseodymium-Neodymium Metal Polished Waste

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 8-12
At room temperature(5~35 ℃),rare earths,fluorine and iron in Pr-Nd metal polished waste were recovered and recycled by screening,wet magnetic separation,acidification,oxalic acid precipitation and roasting.The obtained Pr-Nd oxide and Pr-Nd fluoride exhibit high purity,and the recovery rates of rare earths,fluorine,and iron are also high.The recovery rate of rare earths exceeds 96%,fluorine 90%,and iron 93%.The waste acid produced in the process of recovering the acid insolubles and the dust and washing water produced in the process of washing sieve oversize can be recycled in the treatment of the next batch.The whole process not only realizes the secondary resource utilization,but also produces no waste residue,saving the production costs and solving the problem of waste residue in environmental protection.The recovery and treatment method of Pr-Nd metal polished waste proposed by this process is simple and easy to operate and industrialize.
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Process Design of Rare Earth Metal Smelting Production Line

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 13-17
The existing processes of rare earth metal smelting are analyzed.Molten salt electrolysis with fluoride system,calcium thermal reduction and lanthanum thermal reduction can be used to produce different rare earth products in accordance with their properties.A feasible scheme for automatic feeding and discharging in the electrolysis process is proposed.A complete set of equipment consisting of a bale breaker,automatic feeding equipment and control system is adopted in the feeding process,realizing mechanized charging,automatic feeding,and information-based statistical analysis.The vacuum siphon or manipulator could be used for the discharging process.The treatment scheme of “three wastes”,especially the waste gas,is proposed with nearly all dust being recovered,fluorine being solidified into calcium fluoride for comprehensive utilizayion,and waste gas being emitted in compliance with standards.
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Study on the Process of Extracting Vanadium Pentoxide from Stone Coal Boiling Roasting Material

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 18-23
In response to the problems of large differences in raw materials,long process flow,low vanadium recovery rate(mostly below 60%),and high cost in extracting vanadium from stone coal boiling roasting materials,a process route of mixing acid,curing and leaching-oxidation neutralization-ion exchange-vana-dium precipitation with ammonium salt-calcination was adopted to extract vanadium.The experimental results show that under the conditions of sulfuric acid dosage of 20% of the raw material weight,curing temperature of 100 ℃,and curing time of 6 h,the vanadium leaching rate of stone coal boiling roasting material reaches 90.2%.The final product V2O5 powder quality is stable and reliable,which reaches the level of industry standards.This process has a short process flow,low engineering construction investment,high vanadium recovery rate,and low vanadium smelting cost,achieving good economic and technical indicators.
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Extraction of Vanadium from Stone Coal in Xiangxi by Concentrated Sulfuric Acid Curing Leaching

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 24-27
The concentrated sulfuric acid curing leaching was used in extracting vanadium from Xiangxi stone coal,the effects of sulfuric acid dosage,decarbonization temperature,curing time,curing temperature,and leaching time on leaching rate of vanadium were researched by single factor experiments and orthogonal experiments.The experiment results show that the leaching rate of vanadium is 83.2% under the conditions of decarbo-nization temperature of 600 ℃,sulfuric acid dosage of 24%,curing temperature of 180 ℃,curing time of 8 h and leaching time of 8 h.The vanadium extraction process does not produce harmful gases and reduces environmental pollution.
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Research on Process of Iron Removal from Leaching Solution of Retired Ternary Lithium-Ion Battery Materials

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 28-32
Taking the leaching solution of retired ternary lithium-ion battery materials as the research object,the process of iron removal from the leaching solution was studied.The effects of the terminal pH value of the leaching solution after iron removal,reaction time,reaction temperature,and oxidant addition coefficient β(nNaClO_(3)∶nFe) on the removal of iron from the leaching solution of ternary lithium-ion battery materials were investigated.The optimized process parameters are as follows:terminal pH value 4.5,reaction time 2.5 h,reaction temperature 85 ℃,and β=1.1.Under these optimized conditions,the iron removal rate is greater than 98%,and nickel content in slag is less than 0.2%.The research results provide a scientific basis for the comprehensive utilization of retired ternary lithium-ion battery materials.
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Process and Kinetics Study of Se Preparation by SO2 Reduction of SeO2

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 33-38
The effects of reaction temperature,H2SO4 concentration,SO2 flow rate and reaction time on the preparation process of Se by SO2 reduction of SeO2 were investigated,the kinetics of the process was stu-died,and the optimal process conditions and kinetic restrictive control links were obtained.The results show that under the conditions of the reaction temperature of 40 ℃,H2SO4 concentration of 1 mol/L,SO2 flow rate of 60 mL/min,and reaction time of 30 min,the reduction rate of Se reaches 99.73%,preparing Se with a purity of 99.85%.By controlling the conditions,different forms of Se can be obtained:amorphous red Se at low temperatures and well-crystallized black Se at high temperatures.The preparation process of Se by SO2 reduction of SeO2 conforms to the Avrami model,controlled by diffusion with an apparent activation energy of 1.98 kJ/mol,and described by the kinetics equation of-ln(1-X)=0.178×e-238/Tt1.276.
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Effects of Triton X-100 and OP-10 on Dispersivity of Nano-Sized Tungsten Carbide Powder in Absolute Ethanol

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 39-46
Nano-sized tungsten carbide powder is an important raw material for the preparation of ultrafine nano-cemented carbide.However,due to its large specific surface area,agglomeration is easy to occur,hindering the full play of its inherent excellent performance.To reduce the agglomeration of the nano-sized tungsten carbide powder,two surfactants,Triton X-100 and OP-10,were used for dispersion.Sedimentation experiment,absorbance test,particle size analysis and transmission electron microscope were used to study the dispersion performance of nano-sized tungsten carbide in absolute ethanol.The results show that when the mass fractions of Triton X-100 and OP-10 are 2% and 1.5% with ultrasonic times of 30 min and 50 min,respectively,the dispersion effect of the nano-sized tungsten carbide suspension reaches the best.Under the same ultrasonic time and with the same concentrations,OP-10 exhibits better dispersion effect than Triton X-100.Infrared analysis shows that Triton X-100 and OP-10 mainly reduce the agglomeration by adsorbing onto the surface of nano-sized tungsten carbide.
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Study on Preparation and Electrochemical Performance of NiMoS4@MoS3

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 47-51
The NiMoS4@MoS3 composite electrode material based on nickel foam was successfully prepared using the three-step hydrothermal method.The phase structure and micromorphology of the electrode material were studied by X-ray diffraction(XRD) and scanning electron microscope(SEM) and its electrochemical performance was tested by cyclic voltammetry(CV),galvanostatic charge and discharge(GCD),and electrochemical impedance spectroscopy(EIS).The results show that charge and discharge duration of the NiMoS4@MoS3 electrode reaches 5 600 s with specific capacitance of 4 744 mF/cm2 at 1 mA/cm2.In addition,the composite electrode shows relatively symmetrical redox peaks in the CV curve and symmetrical charge and discharge platform in the GCD curve,indicating its excellent charge and discharge efficiency and stability.The research provides a new insight for the design and preparation of high-performance electrochemical energy storage materials.
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Preparation of Nd3+ Doped LaBO3 Phosphors by Solution Combustion Method

Rare Metals and Cemented Carbides | Vol., Issue 4, 2023 | pp. 52-56
Using La(NO3)3·6H2O and H3BO3 as raw materials,C2H5NO2 as combustion agent,and Nd(NO3)3·6H2O as modifier,Nd3+ doped LaBO3 phosphors were synthesized by solution combustion method.The products were characterized by X-ray diffraction(XRD),scanning electron microscope(SEM),ultraviolet-visible diffuse reflection spectrum(UV-Vis DRS),and fluorescence spectrum(PL).The results show that the prepared powders are all orthorhombic lanthanum borate and the phosphors prepared under the optimized conditions of calcination temperature of 875 ℃ and Nd3+ doping amount of 3% have the best luminescent performance,showing good light absorption performance in both ultraviolet and visible light regions and emitting blue-green light,which can be widely used in the fields of laser illumination and LED lighting.
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