CN102828030A - Method for recycling rare earth elements in rare earth fluorescent powder waste by ultrasonic-submolten salt process - Google Patents
Method for recycling rare earth elements in rare earth fluorescent powder waste by ultrasonic-submolten salt process Download PDFInfo
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Abstract
The invention belongs to the technical fields of environmental protection and comprehensive utilization of rare-earth secondary resources, and particularly relates to a method for recycling rare earth elements in rare earth fluorescent powder waste by an ultrasonic-submolten salt process. The method comprises the following steps: treating rare earth fluorescent powder waste by an ultrasonic-submolten salt process to obtain rare-earth-rich slag; and sequentially carrying out acid pickling, ammonia water precipitation, acid dissolution, oxalic acid precipitation and high-temperature calcination on the rare-earth-rich slag to obtain rare earth oxides. The invention has the advantages of high industrial operability, short technical process, low cost, low non-rare-earth impurity content in the rare earth oxides, and the like, is simple to operate, and implements recycling of the rare earth fluorescent powder waste.
Description
Technical field
The present invention relates to the method for environment protection and secondary resource comprehensive reutilization, particularly ultrasonic-sub-molten salt method reclaims the method for fluorescent RE powder waste material middle-weight rare earths element.
Background technology
Rare earth is non-renewable grand strategy resource, because of many-sided characteristics such as its good light, electricity, magnetic, has been widely used in a plurality of fields such as electronic information, metallurgical machinery, petrochemical complex, energy environment, defence and military.Fluorescent RE powder has been widely used in the products such as plasm TV, semiconductor lighting photodiode, rare-earth fluorescent light, mobile phone and computer as important luminescent material.These products are finally discarded by the human consumer with the form of solid waste, and discarded arbitrarily or improper processing contains the solid waste of fluorescent RE powder, contaminate environment not only, and cause the waste of rare earth resources.Though China is the abundantest country of rare earth resources, along with the domestic rare earth consumers demand of China increases, the influence of factor such as cheap outlet and long-term gopher in a large number, China's rare earth reserves fall sharply.Therefore, reclaim the REE in the fluorescent RE powder waste material, the aspects such as Sustainable development, save energy and protection environment for China's rare earth resources all have great importance.
In recent years, there is the investigator to adopt technology such as solid direct extraction, supercritical extraction, hydrometallurgy, flotation process from the fluorescent RE powder waste material, to reclaim REE.R. (The Journal of Supercritical Fluids such as Shimizu; 2005; 33; 235) Tributyl phosphate salt, nitric acid and water are mixed with the supercritical extraction solvent according to a certain percentage in CO 2 medium; Adopting supercritical extraction technique to reclaim rare earth element y and Eu in the rare-earth trichromatic fluorescent powder waste material, is that acid is dissolved the rare-earth trichromatic fluorescent powder waste material with extraction separation process combines together on this technological essence, exist reaction conditions very harshness, cost recovery high, be prone to cause shortcoming such as second environmental pollution.Ni Haiyong (CN 101307391 A) adopts KOH or NaOH high-temperature fusion fluorescent RE powder waste material, obtains the alkali fusion thing, through obtaining containing the mishmetal throw out of rare earth element y, Eu, Ce, Tb behind filtration, acidleach, the oxalic acid precipitation; This method needs high-temperature calcination, and energy consumption is too high, and production cost is too high.Mei Guangjun etc. (CN 102312098 A) adopt mineral acids (example hydrochloric acid, nitric acid or sulfuric acid) the dissolving technology that combines with extracting and separating, recovery rare earth element y and Eu from the fluorescent RE powder waste material; But this method only relates to the recycling of rare earth element y and Eu, is prone to cause the waste of other REEs.
The inventor at first handles the fluorescent RE powder waste material through ultrasonic-sub-molten salt method, obtains the rare-earth enrichment slag; The rare-earth enrichment slag successively through acidleach, ammonia precipitation process, acid dissolve, oxalic acid precipitation and high-temperature calcination obtain rare earth oxide.Used in the present invention ultrasonic-Ya fused salt method do not appear in the newspapers in the rare earth secondary resource field of recycling as yet.
Summary of the invention
The purpose of this invention is to provide a kind ofly have that industrial operability, with low cost, operation are simple, the rare earth secondary resource treatment technology of advantages such as non-rare earth impurity content is low in the products therefrom.
Inferior fused salt of the present invention is meant high concentration alkali/multi-element, inorganic salts solution; Be the unconventional medium that is in the aqueous solution and fused salt intermediate state, good reaction, stalling characteristic such as have good physico-chemical property and high activity quotient, high reaction activities such as low-steam pressure, boiling point height, good fluidity, separation function is adjustable.(turbulent waves. inferior fused salt is produced alumina process silicon component physio-chemical study, Xi'an University of Architecture and Technology, 2008).
Principle of the present invention is because the generation of a large amount of active oxygen negative ions is arranged in the inferior fused-salt medium; Make mineral lattice produce distortion; Increase reactive behavior, thermodynamics and kinetics is strengthened reaction, makes inferior fused-salt medium have very strong resolving power to mineral; And the multiple action such as HTHP of UW also can produce mechanical stirring to reaction medium, cause because of cavitation moment improves the chemical reaction effect.
Provided by the present invention ultrasonic-sub-molten salt method reclaims the method for fluorescent RE powder waste material middle-weight rare earths element, may further comprise the steps:
1) the fluorescent RE powder waste material is put into the inferior fused salt liquid phase medium of alkaline; In the reaction kettle that ultrasonic and water vapor condensation reflux are housed, react; Ultrasonic frequency is 20 ~ 40KHz, and temperature of reaction is 200 ~ 400 ℃, and the reaction times is 1 ~ 6h; Obtain containing alkali lye, alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the acid solution, and add ydrogen peroxide 50 as solubility promoter, the ydrogen peroxide 50 add-on is the per 10 g fluorescent RE powder waste materials of 1 ~ 2mL; Temperature is 60 ~ 85 ℃, and extraction time is 1 ~ 3h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and acid solution is 1:10 ~ 1:20g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9 ~ 10, filters, and obtains precipitation of hydroxide;
5) precipitation of hydroxide with the step 4) gained adds acid fluid dissolves, and regulating the pH value is 1.5 ~ 3.0, adds 50 ~ 100g/L oxalic acid solution, and the mole number of oxalic acid is 1.0 ~ 1.5 times of fluorescent RE powder waste material; Be incubated 0.5 ~ 2h down at 80 ~ 90 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 900 ~ 1000 ℃ of calcining 0.5 ~ 2h down, obtains rare earth oxide.
Press such scheme, the fluorescent RE powder waste material of described step 1) is rare-earth trichromatic fluorescent powder waste material, cathode tube fluorescent material waste material, rare-earth trichromatic fluorescent powder rouge and powder waste material, rare-earth trichromatic fluorescent powder blue powder waste material or the green powder waste material of rare-earth trichromatic fluorescent powder.
Press such scheme, the highly basic of described step 1) is sodium hydroxide, Pottasium Hydroxide or rubidium hydroxide.
Press such scheme, the weight ratio of the highly basic of described step 1) and fluorescent RE powder waste material is 2:1 ~ 10:1.
Press such scheme, the acid solution of described step 3) and step 5) is nitric acid, hydrochloric acid or sulfuric acid.
Advantage of the present invention and characteristics are:
1, the present invention adopts ultrasonic-sub-molten salt method to reclaim the method for fluorescent RE powder waste material middle-weight rare earths element, and reaction conditions is gentle, and industrial implementation is workable;
2, agents useful for same wide material sources of the present invention are cheap, and this method flow process is simple;
3, in the present invention, adopt methods such as ultrasonic-Ya fused salt, ammonia precipitation process, oxalic acid precipitation, can remove a large amount of non-rare earth impurities, improve rare earth oxide purity.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Specific embodiment of the present invention is described in down, but embodiment of the present invention is not limited thereto at present.
Embodiment 1
1) gets the inferior fused salt liquid phase medium that 10g rare-earth trichromatic fluorescent powder waste material is put into sodium hydroxide; The quality of sodium hydroxide is 20g, in the reaction kettle that ultrasonic and water vapor condensation reflux are housed, reacts, and ultrasonic frequency is 20KHz; Temperature of reaction is 200 ℃; Reaction times is 1h, obtains containing alkali lye, and alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the hydrochloric acid soln of 10mol/L, and add the 1mL ydrogen peroxide 50 as solubility promoter, and temperature is 60 ℃, extraction time is 1h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and hydrochloric acid soln is 1:10g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9, filters, and obtains precipitation of hydroxide;
5) with adding 10mol/L nitric acid 30mL in the precipitation of hydroxide of step 4) gained, dissolve, regulating the pH value is 1.5, adds the oxalic acid solution of 50g/L, and the mole number of oxalic acid is 1.0 times of fluorescent RE powder waste material; Be incubated 0.5h down at 80 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 900 ℃ of calcining 0.5h down, obtains rare earth oxide.
Detect through XRF, non-rare earth impurity content is 1.7wt% in the rare earth oxide.
Embodiment 2
1) gets the inferior fused salt liquid phase medium that 10g cathode tube fluorescent material waste material is put into Pottasium Hydroxide; The quality of Pottasium Hydroxide is 60g, in the reaction kettle that ultrasonic and water vapor condensation reflux are housed, reacts, and ultrasonic frequency is 30KHz; Temperature of reaction is 350 ℃; Reaction times is 3h, obtains containing alkali lye, and alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the 10mol/L salpeter solution, and add the 1.5mL ydrogen peroxide 50 as solubility promoter, and temperature is 70 ℃, extraction time is 2h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and salpeter solution is 1:15g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9.5, filters, and obtains precipitation of hydroxide;
5) with adding 10mol/L nitric acid 30mL in the precipitation of hydroxide of step 4) gained, regulating the pH value is 2.0, adds the oxalic acid solution of 70g/L, and the mole number of oxalic acid is 1.5 times of fluorescent RE powder waste material; Be incubated 1h down at 85 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 950 ℃ of calcining 1h down, obtains rare earth oxide.
Detect through XRF, non-rare earth impurity content is 1.2wt% in the rare earth oxide.
Embodiment 3
1) gets the inferior fused salt liquid phase medium that 10g rare-earth trichromatic fluorescent powder rouge and powder waste material is put into rubidium hydroxide; Wherein the quality of rubidium hydroxide is 100g, in the reaction kettle that ultrasonic and water vapor condensation reflux are housed, reacts, and ultrasonic frequency is 30KHz; Temperature of reaction is 400 ℃; Reaction times is 6h, obtains containing alkali lye, and alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the 10mol/L sulphuric acid soln, and add the 2mL ydrogen peroxide 50 as solubility promoter, and temperature is 70 ℃, extraction time is 2h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and sulphuric acid soln is 1:18g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9.5, filters, and obtains precipitation of hydroxide;
5) with adding 10mol/L sulfuric acid 30mL in the precipitation of hydroxide of step 4) gained, dissolve, regulating the pH value is 2.0, adds the oxalic acid solution of 70g/L, and the mole number of oxalic acid is 1.2 times of fluorescent RE powder waste material; Be incubated 1h down at 85 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 950 ℃ of calcining 1h down, obtains rare earth oxide.
Detect through XRF, non-rare earth impurity content is 0.2wt% in the rare earth oxide.
Embodiment 4
1) gets the inferior fused salt liquid phase medium that 10g rare-earth trichromatic fluorescent powder blue powder waste material is put into sodium hydroxide; The quality of sodium hydroxide is 80g, in the reaction kettle that ultrasonic and water vapor condensation reflux are housed, reacts, and ultrasonic frequency is 40KHz; Temperature of reaction is 300 ℃; Reaction times is 5h, obtains containing alkali lye, and alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the 10mol/L hydrochloric acid soln, and add the 1mL ydrogen peroxide 50 as solubility promoter, and temperature is 85 ℃, extraction time is 3h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and acid solution is 1:20g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9, filters, and obtains precipitation of hydroxide;
5) with adding 10mol/L hydrochloric acid 30mL in the precipitation of hydroxide of step 4) gained, dissolve, regulating the pH value is 2.0, adds the oxalic acid solution of 50g/L, and the mole number of oxalic acid is 1.0 times of fluorescent RE powder waste material; Be incubated 2h down at 80 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 950 ℃ of calcining 2h down, obtains rare earth oxide.
Detect through XRF, non-rare earth impurity content is 1.3wt% in the rare earth oxide.
Embodiment 5
1) gets the inferior fused salt liquid phase medium that the green powder waste material of 10g rare-earth trichromatic fluorescent powder is put into sodium hydroxide; The quality of sodium hydroxide is 50g, in the reaction kettle that ultrasonic and water vapor condensation reflux are housed, reacts, and ultrasonic frequency is 40KHz; Temperature of reaction is 400 ℃; Reaction times is 6h, obtains containing alkali lye, and alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the 10mol/L hydrochloric acid soln, and add the 2mL ydrogen peroxide 50 as solubility promoter, and temperature is 85 ℃, extraction time is 3h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and acid solution is 1:20g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 10, filters, and obtains precipitation of hydroxide;
5) with adding 10mol/L sulfuric acid 30mL in the precipitation of hydroxide of step 4) gained, dissolve, regulating the pH value is 3.0, adds the oxalic acid solution of 100g/L, and the mole number of oxalic acid is 1.0 times of fluorescent RE powder waste material; Be incubated 2h down at 90 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 1000 ℃ of calcining 2h down, obtains rare earth oxide.
Detect through XRF, non-rare earth impurity content is 2.4wt% in the rare earth oxide.
Claims (5)
1. ultrasonic-sub-molten salt method reclaims the method for fluorescent RE powder waste material middle-weight rare earths element, it is characterized in that this method may further comprise the steps:
1) the fluorescent RE powder waste material is put into the inferior fused salt liquid phase medium of alkaline; In the reaction kettle that ultrasonic and water vapor condensation reflux are housed, react; Ultrasonic frequency is 20 ~ 40KHz, and temperature of reaction is 200 ~ 400 ℃, and the reaction times is 1 ~ 6h; Obtain containing alkali lye, alkali dissolves the reaction product mixture of thing and rare-earth enrichment slag;
2) reaction product mixture that step 1) is obtained is filtered, and obtains alkaline filtrate and rare-earth enrichment slag;
3) with step 2) the rare-earth enrichment slag of gained immerses in the acid solution, and add ydrogen peroxide 50 as solubility promoter, the ydrogen peroxide 50 add-on is the per 10 g fluorescent RE powder waste materials of 1 ~ 2mL; Temperature is 60 ~ 85 ℃, and extraction time is 1 ~ 3h, obtains rare earth feed liquid; The solid-to-liquid ratio of described rare-earth enrichment slag and acid solution is 1:10 ~ 1:20g/mL;
4) add ammoniacal liquor in the rare earth feed liquid with the step 3) gained, the pH value is adjusted to 9 ~ 10, filters, and obtains precipitation of hydroxide;
5) precipitation of hydroxide with the step 4) gained adds acid fluid dissolves, and regulating the pH value is 1.5 ~ 3.0, adds 50 ~ 100g/L oxalic acid solution, and the mole number of oxalic acid is 1.0 ~ 1.5 times of fluorescent RE powder waste material; Be incubated 0.5 ~ 2h down at 80 ~ 90 ℃, filter, obtain the rare-earth oxalate deposition;
6) rare-earth oxalate with the step 5) gained is deposited in 900 ~ 1000 ℃ of calcining 0.5 ~ 2h down, obtains rare earth oxide.
2. method according to claim 1 is characterized in that: the fluorescent RE powder waste material of described step 1) is rare-earth trichromatic fluorescent powder waste material, cathode tube fluorescent material waste material, rare-earth trichromatic fluorescent powder rouge and powder waste material, rare-earth trichromatic fluorescent powder blue powder waste material or the green powder waste material of rare-earth trichromatic fluorescent powder.
3. method according to claim 1 is characterized in that: the highly basic of described step 1) is sodium hydroxide, Pottasium Hydroxide or rubidium hydroxide.
4. method according to claim 1 is characterized in that: the weight ratio of the highly basic of described step 1) and fluorescent RE powder waste material is 2:1 ~ 10:1.
5. method according to claim 1 is characterized in that: the acid solution of described step 3) and step 5) is nitric acid, hydrochloric acid or sulfuric acid.
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| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN105296758A (en) * | 2015-11-03 | 2016-02-03 | 苏州优康通信设备有限公司 | Extracting method for noble metal on optical device |
| CN106995884A (en) * | 2016-01-25 | 2017-08-01 | 安徽工业大学 | A kind of method of the Extraction of rare earth element from waste phosphor powder |
| CN107513620A (en) * | 2017-08-30 | 2017-12-26 | 赣州齐畅新材料有限公司 | A kind of process of the Extraction of rare earth oxide from fluorescent powder scrap |
| CN108517426A (en) * | 2018-05-15 | 2018-09-11 | 北京工业大学 | The method that the CRT fluorescent powder middle rare earth that gives up under a kind of temperate condition efficiently separates recycling |
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| CN114425486A (en) * | 2022-01-26 | 2022-05-03 | 江西理工大学 | Method for recovering rare earth elements in waste fluorescent powder through ultrasonic enhanced flotation |
| CN114774718A (en) * | 2022-04-21 | 2022-07-22 | 江西理工大学 | Method for recovering rare earth elements in rare earth molten salt electrolytic slag by using sub-molten salt method |
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| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN105296758A (en) * | 2015-11-03 | 2016-02-03 | 苏州优康通信设备有限公司 | Extracting method for noble metal on optical device |
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| CN107513620B (en) * | 2017-08-30 | 2021-07-09 | 赣州齐畅新材料有限公司 | Process method for extracting rare earth oxide from fluorescent powder waste |
| CN108686668B (en) * | 2018-05-15 | 2021-03-02 | 北京工业大学 | Method for selectively recycling yttrium in CRT fluorescent powder for doping preparation of ternary composite oxide catalyst |
| CN108517426B (en) * | 2018-05-15 | 2020-02-04 | 北京工业大学 | Method for efficiently separating and recycling rare earth in waste CRT fluorescent powder under mild condition |
| CN108686668A (en) * | 2018-05-15 | 2018-10-23 | 北京工业大学 | Yttrium is used for the method that doping prepares ternary compound oxides catalyst in a kind of selective recovery CRT fluorescent powders |
| CN108517426A (en) * | 2018-05-15 | 2018-09-11 | 北京工业大学 | The method that the CRT fluorescent powder middle rare earth that gives up under a kind of temperate condition efficiently separates recycling |
| CN111040819A (en) * | 2018-10-12 | 2020-04-21 | 国家能源投资集团有限责任公司 | Ash removal method for solid carbonaceous material |
| CN112695213A (en) * | 2020-12-03 | 2021-04-23 | 北京工业大学 | Method for extracting rare earth from waste FCC catalyst by acid leaching coupling photoreduction |
| CN114425486A (en) * | 2022-01-26 | 2022-05-03 | 江西理工大学 | Method for recovering rare earth elements in waste fluorescent powder through ultrasonic enhanced flotation |
| CN114774718A (en) * | 2022-04-21 | 2022-07-22 | 江西理工大学 | Method for recovering rare earth elements in rare earth molten salt electrolytic slag by using sub-molten salt method |
| CN114774718B (en) * | 2022-04-21 | 2023-10-27 | 江西理工大学 | Method for recycling rare earth elements in rare earth molten salt electrolysis slag by sub-molten salt method |
| CN115418504A (en) * | 2022-08-25 | 2022-12-02 | 萍乡鑫森新材料有限责任公司 | Method for extracting rare earth from rare earth organic slag |
| CN115948122A (en) * | 2023-01-05 | 2023-04-11 | 包头稀土研究院 | Method for regenerating fluorine-containing rare earth polishing powder |
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Application publication date: 20121219 |