研究目的
To evaluate discarded compact fluorescent lamps (CFLs) as a potential source for recovering rare earth elements (REEs) such as Y, Eu, Ce, and Tb, and to develop an efficient extraction process involving mechanical milling and leaching.
研究成果
Discarded CFLs are a viable source for recovering Y and Eu with high purity (>98%) and recovery rates (>90%) using optimized mechanical milling (20-30 min) and leaching (3-4 M acid). The CAT phosphor phase remains inert, limiting Ce and Tb recovery. The process yields 13 g of mixed Y-Eu oxide from 100 CFLs, demonstrating potential for recycling and reducing environmental impact.
研究不足
The process is effective for Y and Eu recovery but not for Ce and Tb due to the inert nature of the CAT phosphor phase (Al11Ce0.67MgO19Tb0.33), which requires more rigorous conditions. Excessive milling can lead to increased impurity dissolution, hindering precipitation. The study is limited to specific CFL samples and may not generalize to all waste sources.
1:Experimental Design and Method Selection:
The study involved mechanical separation of phosphor powder from discarded CFLs, followed by characterization using XRF, XRD, and SEM/EDS. Leaching experiments were conducted with inorganic acids (HCl, HNO3, H2SO4) at controlled conditions, and precipitation of REEs was performed using oxalic acid. A Box-Behnken response-surface design was used for optimization of milling time, acid concentration, and leaching time.
2:Sample Selection and Data Sources:
End-of-life CFLs were procured from a local electric warehouse. The phosphor powder was separated by sieving below 53 μm size.
3:List of Experimental Equipment and Materials:
Equipment included a planetary ball mill (Retsch PM 100), X-ray fluorescence (XRF) spectrometer (Rigaku Supermini 200), X-ray diffractometer (XRD, Rigaku Smart Lab), scanning electron microscope with EDS (Fe-SEM, Zeiss EVO18), magnetic stirrer (C-Mag HS-7, IKA), pH meter (Cole-Parmer P100), and laboratory oven. Materials included tungsten carbide jars and balls, inorganic acids (HCl, HNO3, H2SO4), oxalic acid, and other chemicals for precipitation.
4:Experimental Procedures and Operational Workflow:
CFLs were shredded and components separated. Phosphor powder was milled in a planetary ball mill for specified times, then leached in acid solutions at 40°C with stirring. Leach residues were filtered and dried. REEs were precipitated from leach solutions using oxalic acid at controlled pH, and precipitates were calcined at 900°C to obtain rare earth oxides (REOs).
5:Data Analysis Methods:
Data were analyzed using statistical software (Design Expert-11) for optimization. Dissolution percentages were calculated based on XRF analysis, and phase identification was done via XRD and EDS.
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X-ray Fluorescence Spectrometer
Supermini 200
Rigaku
Used for mineral element composition analysis of waste phosphor powder.
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X-ray Diffractometer
Smart Lab
Rigaku
Used for phase identification and quantitative analysis of phosphor samples.
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Scanning Electron Microscope
EVO18
Zeiss
Used for morphology study and EDS analysis of powder samples.
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Planetary Ball Mill
PM 100
Retsch
Used for mechanical activation and milling of phosphor powder to liberate rare earth elements.
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Magnetic Stirrer
C-Mag HS-7
IKA
Used for stirring during leaching experiments.
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pH Meter
P100
Cole-Parmer
Used for monitoring pH during precipitation processes.
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