Method for recycling rare earth elements in rare earth fluorescent powder waste by ultrasonic-submolten salt process
A rare earth phosphor and sub-molten salt method technology is applied in the fields of environmental protection and comprehensive recycling of secondary resources, and achieves the effects of mild reaction conditions, improved purity and simple process.
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Embodiment 1
[0026] 1) Take 10g of rare earth three-color fluorescent powder waste and put it into the sub-molten salt liquid phase medium of sodium hydroxide. The quality of sodium hydroxide is 20g. The frequency is 20KHz, the reaction temperature is 200°C, and the reaction time is 1h to obtain a mixed reaction product containing lye, alkali solubles and rare earth enriched slag;
[0027] 2) Filtrating the mixed reaction product obtained in step 1) to obtain alkaline filtrate and rare earth enriched slag;
[0028] 3) Immerse the rare earth enrichment slag obtained in step 2) into a 10mol / L hydrochloric acid solution, and add 1mL hydrogen peroxide as a cosolvent at a temperature of 60°C and a leaching time of 1h to obtain a rare earth feed liquid; the rare earth enrichment The solid-to-liquid ratio of slag and hydrochloric acid solution is 1:10g / mL;
[0029] 4) Add ammonia water to the rare earth feed solution obtained in step 3), adjust the pH value to 9, filter, and obtain hydroxide pre...
Embodiment 2
[0034] 1) Take 10g of cathode ray tube fluorescent powder waste and put it into the sub-molten salt liquid phase medium of potassium hydroxide. The frequency is 30KHz, the reaction temperature is 350°C, and the reaction time is 3h to obtain a mixed reaction product containing lye, alkali solubles and rare earth enriched slag;
[0035] 2) Filtrating the mixed reaction product obtained in step 1) to obtain alkaline filtrate and rare earth enrichment slag;
[0036] 3) Immerse the rare earth enrichment slag obtained in step 2) into a 10mol / L nitric acid solution, and add 1.5mL hydrogen peroxide as a cosolvent at a temperature of 70°C and a leaching time of 2 hours to obtain a rare earth feed liquid; the rare earth enrichment The solid-to-liquid ratio of slag and nitric acid solution is 1:15g / mL;
[0037] 4) Add ammonia water to the rare earth feed liquid obtained in step 3), adjust the pH value to 9.5, filter to obtain hydroxide precipitate;
[0038] 5) Add 30mL of 10mol / L nitri...
Embodiment 3
[0042] 1) Take 10g of rare earth three-color fluorescent pink waste and put it into the sub-molten salt liquid phase medium of rubidium hydroxide, in which the mass of rubidium hydroxide is 100g, and carry out the reaction in a reactor equipped with ultrasonic and steam condensation reflux devices , the ultrasonic frequency is 30KHz, the reaction temperature is 400°C, and the reaction time is 6h, to obtain a mixed reaction product containing lye, alkali solubles and rare earth enriched slag;
[0043] 2) Filtrating the mixed reaction product obtained in step 1) to obtain alkaline filtrate and rare earth enriched slag;
[0044]3) Immerse the rare earth enriched slag obtained in step 2) into 10mol / L sulfuric acid solution, and add 2mL of hydrogen peroxide as a co-solvent, the temperature is 70°C, and the leaching time is 2h to obtain a rare earth material liquid; the rare earth enriched slag The solid-to-liquid ratio with sulfuric acid solution is 1:18g / mL;
[0045] 4) Add ammon...
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