CN105838878A - Method for recovering rare earth from waste cathode ray tube fluorescent powder through microbial leaching - Google Patents
Method for recovering rare earth from waste cathode ray tube fluorescent powder through microbial leaching Download PDFInfo
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- CN105838878A CN105838878A CN201610421514.3A CN201610421514A CN105838878A CN 105838878 A CN105838878 A CN 105838878A CN 201610421514 A CN201610421514 A CN 201610421514A CN 105838878 A CN105838878 A CN 105838878A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/18—Extraction of metal compounds from ores or concentrates by wet processes with the aid of microorganisms or enzymes, e.g. bacteria or algae
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention relates to a method for recovering rare earth from waste cathode ray tube fluorescent powder through microbial leaching. The method is characterized by comprising the steps of (a), performing pretreatment: drying fluorescent powder until constant weight is achieved, and grinding the dried fluorescent powder with constant weight into fine powder with a grinding instrument for standby application; (b), performing microbe selection and culturing: selecting funguses or bacteria as leaching microbes, and selecting liquid cane sugar culture mediums and beef extract peptone culture mediums as culture mediums for separately culturing the funguses and the bacteria; (c), performing leaching treatment: adding levigated fluorescent powder into the culture mediums containing strains, putting the culture mediums with the levigated fluorescent powder into a vibrating culturing box, performing culturing for some time, performing filtration, obtaining waste slags, collecting thalli, and decomposing the thalli so as to obtain a leaching solution containing rare-earth elements. Through the adoption of the method, not only can the innocent treatment of the waste fluorescent powder be realized, but also rare earth resources can be recovered.
Description
Technical field
The invention belongs to hazardous waste process and field of comprehensive utilization, utilize the useless negative electrode of microorganism wet method extraction to penetrate particularly to one
The method of spool (CRT) fluorescent material rare earth element.
Background technology
CRT fluorescent material is to scribble fluorescent RE powder according to a fixed structure on the inner surface of cathode ray tube panel glass.China is cloudy
Extreme ray pipe (CRT) display production and application big country, CRT yield accounts for about the 60% of whole world total output.According to statistics, China
There are about 400,000,000 CRT television sets, nearly 20,000,000 computers.Along with the quickening of electronic product renewal speed, new display
Substitute traditional CRT monitor, cause increasing CRT monitor to be eliminated.According to estimates, annual TV and computer
Superseded quantity all more than 5,000,000, and its quantity is continuously increased with the rate of increase of annual 25% to 30%.
In discarded CRT, fluorescent material contains rare earth element (mainly yttrium (Y) and europium (Eu)) and the heavy metal such as zinc, lead, as
After the most mishandling entrance environment, environment is existed and threatens greatly.Rare earth metal enters in environment, and rare earth heavy metal generally has
There is acute or chronic toxicity, enter soil or animals and plants therein can be caused the biggest harm by water body, the Environmental Toxicological of rare earth element
Problem receives significant attention.On the other hand, fluorescent material is the rare earth resources of preciousness containing Y and Eu, if can be by rare earth
Metal is separated containing rare earth waste from various, the protection to China's environment, and the cycling and reutilization of rare earth resources has important
Realistic meaning.
Recovery and treatment method about useless CRT fluorescent material rare earth resources mainly uses acidleach, the most again side such as extract and separate at present
Method, separates and recovers rare earth metal yttrium and europium from waste phosphor powder.Owing to the occurrence status of different fluorescent material middle rare earth is different,
And non-rare earth composition is the most different；Although the research reclaiming fluorescent material middle rare earth achieves certain achievement, but it is multiple often to there is technique
The problem such as miscellaneous, rare earth yield is low, cost is high, economic benefit is low, the content of waste phosphor powder middle rare earth component is the most relatively low,
Need to use the reagent such as acid to remove substantial amounts of impurity during recovering rare earth, secondary pollution to a greater extent may be caused.
Therefore, the most green, the research processing the useless CRT fluorescent material rare earth elements of recovery of low cost, it has also become research of technique in the industry
Focus.
Summary of the invention
The present invention is to provide the method that one utilizes microorganism extraction to reclaim useless cathode ray tube (CRT) fluorescent material rare earth.The party
Method theory based on microorganism ecology, utilizes larger molecular organics secreted in growth of microorganism or growth course to verify glimmering
In light powder, the material containing rare earth dissolves, and ionic state rare earth element absorbs the effect such as (absorption) or chelating, reaches to separate back
Receiving the purpose of rare earth element, the method has green, low cost, secondary stain few advantage.
Present disclosure is: utilize the method that useless cathode ray tube (CRT) fluorescent material rare earth is reclaimed in microorganism extraction, including
The following step:
A, pre-treatment: being mixed by waste phosphor powder, drying to constant weight, fine powder worn into by ground instrument.
B, microorganism are chosen and are cultivated: select fungus and antibacterial for extraction microorganism；Culture medium selects liquid sugar culture medium and cattle
Meat extract protein culture medium cultivates fungus and antibacterial respectively.
C, extraction process: joined by levigate fluorescent material in the culture medium of strain, when putting into cultivation one section in vibration culture oven
After between, filter, waste, collect thalline, obtain containing yttrium, the lixiviating solution of europium.
Bacillus cereus, aspergillus niger, penicillium sp are chosen in microorganism of the present invention.
Strain is preferably added in culture medium 1～3d by step c of the present invention extraction processing method, then adds levigate fluorescent material.
In present disclosure, it is as follows that the extraction of step c processes concrete grammar: the waste phosphor powder after levigate is joined sterilizing good
Fluid medium in, be concurrently accessed microorganism, strain access amount is the 0.5%～5% of culture volume；Adding of waste phosphor powder
Enter amount be mass ratio be the amount of 1%～20% culture medium, temperature be 20～40 DEG C, rotating speed be 100～180r/min vibration trainings
Support 7～30d；Taking-up culture bottle is through 2～5min sonic oscillations, standing to supernatant becomes clarification, takes out upper strata bacterium
Body thing, extraction supernatant, by 0.22 μm membrane filtration, is collected filtrate, is obtained containing yttrium, the lysate of europium.
It is as follows that step c extraction of the present invention processes preferred version: microorganism being linked in the fluid medium that sterilizing is good, strain connects
Enter that amount is culture volume 0.5%～5%；Temperature be 20～40 DEG C, rotating speed be 100～180r/min vibrations cultivate 1～
3d, then add levigate after waste phosphor powder, addition be mass ratio be the amount of 1%～20% culture medium, in temperature be
20-40 DEG C, rotating speed be 100-180r/min vibration cultivate 7-30d；Take out culture bottle through 2～5min sonic oscillations,
Standing becomes clarification to supernatant, taking out upper strata thalline thing, extraction supernatant, by 0.22 μm membrane filtration, was collected
Filtrate, obtains containing yttrium, the lysate of europium.
The present invention utilizes the method that useless cathode ray tube (CRT) fluorescent material rare earth is reclaimed in microorganism extraction, still further comprise with
Lower step: the thalline material on filter membrane is put into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h, the flying dust obtained
Use 10% dilute nitric acid dissolution, obtain containing yttrium, the lysate of europium.
In present disclosure: key component and the mass percent of described waste phosphor powder consist of (in terms of oxide): Y2O3
8%～30%, ZnO 20%～45%, Eu2O31%～2%, Al2O36%～8%, S 15%～20%, Si2O33%～5%,
Remaining is K2O、Na2O、PbO、MgO、Co3O4、Fe2O3Deng.
Compared with prior art, the present invention has features and a beneficial effect:
(1) present invention is from raw material waste phosphor powder, through the extraction effect of microorganism, it is achieved the dissolution of rare earth element, separates
And enrichment method, obtain concentration higher be that further purification has provided to obtain condition containing rare earth element solution, by extraction after
The big reduction of content of residue heavy metal, be possible not only to realize the harmless treatment of this waste phosphor powder, at the same time it can also be realize
The recovery of rare earth resources.
(2) use the present invention, turn waste into wealth, beneficially the comprehensive utilization of Environmental capacity, environmental conservation, beneficially resource, prepare work
Skill is simple, practical.
Detailed description of the invention
Embodiment 1: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and 200 mesh worn into by ground instrument
Fine powder.With aspergillus niger for extraction bacterial strain, culture medium is multitudinous sugar liquors culture medium, accesses ready after the sterilized process of culture medium
Aspergillus niger bacterium solution 5mL (a total of about 750 mycelium pellets) in the 500mL triangular flask equipped with the multitudinous sugar culture-medium of 250mL,
It is simultaneously introduced the fluorescent material 1.25g that sterilizing is good.Temperature be 30 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.Take out triangle
Bottle, through 2min sonic oscillation, stands and treats that liquid is clarified, and takes out upper strata thalline, takes supernatant and passes through 0.22 μm membrane filtration,
Collect filtrate 230mL；Thalline material on filter membrane is put into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h,
The flying dust obtained 10% dilute nitric acid dissolution, obtains containing yttrium, the lysate of europium；Inductively-coupled plasma spectrometer analytical solution
With the element such as yttrium, europium in sample before reaction (solid uses HNO3/HClO4/HF method to clear up)；Result show about 70% yttrium,
The europium of 88% enters solution.
Embodiment 2: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and 200 mesh worn into by ground instrument
Fine powder.With aspergillus niger for extraction bacterial strain, culture medium is multitudinous sugar liquors culture medium, accesses ready after the sterilized process of culture medium
Aspergillus niger bacterium solution 5mL (a total of about 750 mycelium pellets) in the 500mL triangular flask equipped with the multitudinous sugar culture-medium of 250mL,
It is simultaneously introduced the fluorescent material 3.75g that sterilizing is good.Temperature be 30 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.Take out triangle
Bottle, through 2min sonic oscillation, stands and treats that liquid is clarified, and takes out upper strata thalline, takes supernatant and passes through 0.22 μm membrane filtration,
Collect filtrate 225mL；Thalline material on filter membrane is put into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h,
The flying dust obtained 10% dilute nitric acid dissolution, obtains containing yttrium, the lysate of europium；Analyze molten with inductively-coupled plasma spectrometer
The element such as yttrium, europium in sample (solid uses HNO3/HClO4/HF method to clear up) before liquid and reaction；Result shows about 80%
Yttrium, the europium of 85% enter solution.
Embodiment 3: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and 200 mesh worn into by ground instrument
Fine powder.With aspergillus niger for extraction bacterial strain, culture medium is multitudinous sugar liquors culture medium, accesses ready after the sterilized process of culture medium
Aspergillus niger bacterium solution 5mL (a total of about 750 mycelium pellets) in the 500mL triangular flask equipped with the multitudinous sugar culture-medium of 250mL,
Temperature be 30 DEG C, rotating speed be that 170r/min vibration is cultivated；After Aspergillus Niger Growth 3d, add the fluorescent material 1.25 that sterilizing is good
g.Temperature be 30 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.Take out triangular flask through 2min sonic oscillation, standing
Treat that liquid is clarified, take out upper strata thalline, take supernatant by 0.22 μm membrane filtration, collection filtrate 224mL；Will filter
Thalline material on film puts into 105 DEG C of drying in Muffle furnace, and then at 500 DEG C of calcination 5h, the flying dust obtained is with 10% dilute nitre
Acid is dissolved, and obtains containing yttrium, the lysate of europium；With sample (solid before inductively-coupled plasma spectrometer analytical solution and reaction
Use HNO3/HClO4/HF method clear up) in the element such as yttrium, europium；Result shows that the yttrium of about 85%, the europium of 90% enter solution.
Embodiment 4: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and 200 mesh worn into by ground instrument
Fine powder.With aspergillus niger for extraction bacterial strain, culture medium is multitudinous sugar liquors culture medium, accesses ready after the sterilized process of culture medium
Aspergillus niger bacterium solution 5mL (a total of about 750 mycelium pellets) in the 500mL triangular flask equipped with the multitudinous sugar culture-medium of 250mL,
Temperature be 30 DEG C, rotating speed be that 170r/min vibration is cultivated；After Aspergillus Niger Growth 3d, add the fluorescent material 3.75 that sterilizing is good
g.Temperature be 30 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.Take out triangular flask through 2min sonic oscillation, standing
Treat that liquid is clarified, take out upper strata thalline, take supernatant by 0.22 μm membrane filtration, collection filtrate 221mL；Will filter
Thalline material on film puts into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h, and the flying dust obtained 10% dust technology
Dissolve, obtain containing yttrium, the lysate of europium；With sample before inductively-coupled plasma spectrometer solution and reaction, (solid uses
HNO3/HClO4/HF method is cleared up) in the element such as yttrium, europium；Result shows that the yttrium of about 88%, the europium of 92% enter solution.
Embodiment 5: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and 200 mesh worn into by ground instrument
Fine powder.With penicillium sp for extraction bacterial strain, culture medium is multitudinous sugar liquors culture medium, accesses ready green grass or young crops after the sterilized process of culture medium
Bacterium solution 5mL (a total of about 750 mycelium pellets), in the 500mL triangular flask equipped with the multitudinous sugar culture-medium of 250mL, adds simultaneously
Enter the fluorescent material 1.25g that sterilizing is good.Temperature be 30 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.Taking-up triangular flask passes through
2min sonic oscillation, stands and treats that liquid is clarified, and takes out upper strata thalline, takes supernatant by 0.22 μm membrane filtration, collection
Filtrate 240mL；Thalline material on filter membrane is put into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h,
The flying dust arrived 10% dilute nitric acid dissolution, obtains containing yttrium, the lysate of europium；Inductively-coupled plasma spectrometer analytical solution and
The element such as yttrium, europium in sample (solid uses HNO3/HClO4/HF method to clear up) before reaction；Result show about 68% yttrium,
The europium of 81% enters solution.
Embodiment 6: one utilizes the method for useless cathode ray tube (CRT) the fluorescent material rare earth of microorganism extraction.In the present embodiment,
Waste phosphor powder comes from useless cathode ray tube, first fluorescent material is dried 24h to constant weight at 80 DEG C, and ground instrument wears into 200
Mesh fine powder.With bacillus cereus for extraction bacterial strain, culture medium is beef extract-peptone fluid medium, after the sterilized process of culture medium
(in bacterium solution, antibacterial number is more than 10 to access ready bacillus liquid 5mL7/ mL) in the 500mL equipped with 250mL culture medium
In triangular flask, it is simultaneously introduced the fluorescent material 1.25g that sterilizing is good.Temperature be 37 DEG C, rotating speed be that 7d is cultivated in 170r/min vibration.
Take out triangular flask standing and treat that liquid is clarified, take supernatant by 0.22 μm membrane filtration, collection filtrate 235mL；Will filter
Thalline material on film puts into 105 DEG C of drying in Muffle furnace, then at 500 DEG C of calcination 5h, and the flying dust obtained 10% dust technology
Dissolve, obtain containing yttrium, the lysate of europium；Before inductively-coupled plasma spectrometer analytical solution and reaction, (solid uses sample
HNO3/HClO4/HF method is cleared up) in the element such as yttrium, europium；Result shows that the yttrium of about 68%, the europium of 81% enter solution.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but in the present invention
On the basis of, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore, not
Deviate these modifications or improvements on the basis of spirit of the present invention, belong to the scope of protection of present invention.
Claims (6)
1. one kind utilizes the method that useless cathodic ray-tube fluorescent powder rare earth is reclaimed in microorganism extraction, it is characterised in that comprise the following steps:
A, pretreatment: drying fluorescent material to constant weight, it is stand-by that fine powder worn into by ground instrument；
B, microorganism are chosen and are cultivated: select fungus or antibacterial to select liquid sugar culture medium and cattle for extraction microorganism, culture medium
Meat extract protein culture medium cultivates fungus and antibacterial respectively；
C, extraction process: joined by levigate fluorescent material in the culture medium of strain, when putting into cultivation one section in vibration culture oven
After between, filtering, waste, collect thalline, thalline is cleared up, and i.e. obtains the lixiviating solution containing rare earth element.
The method utilizing microorganism extraction to reclaim useless cathodic ray-tube fluorescent powder rare earth the most according to claim 1, its characteristic exists
In: bacillus cereus, aspergillus niger, penicillium sp are chosen in described microorganism.
The method utilizing microorganism extraction to reclaim useless cathodic ray-tube fluorescent powder rare earth the most according to claim 1, its characteristic exists
In: described step c extraction processing method, also first strain can be added in culture medium 1～3d, then add levigate fluorescent material.
The method utilizing microorganism extraction to reclaim useless cathodic ray-tube fluorescent powder rare earth the most according to claim 1, its characteristic exists
In, it is as follows that described step c extraction processes concrete grammar: the waste phosphor powder after levigate is joined the liquid culture that sterilizing is good
In base, being concurrently accessed microorganism, strain access amount is the 0.5%～5% of culture volume；The addition of waste phosphor powder is
Mass ratio is the amount of 1%～20% culture medium, temperature be 20～40 DEG C, rotating speed be 100～180r/min vibrations cultivate 7～
30d；Take out culture bottle and treat that liquid is clarified through 2～5min sonic oscillations, standing, take out upper strata thalline thing, in extraction
Clear liquid passes through 0.22 μm membrane filtration, collects filtrate, obtains the lysate containing rare earth element.
The method utilizing microorganism extraction to reclaim useless cathodic ray-tube fluorescent powder rare earth the most according to claim 3, its characteristic exists
In, it is as follows that described step c extraction processes concrete grammar: microorganism being linked in the fluid medium that sterilizing is good, strain connects
Enter that amount is culture volume 0.5%～5%；Temperature be 20～40 DEG C, rotating speed be that 100～180r/min vibrations are cultivated
1～3d, then add levigate after waste phosphor powder, addition be mass ratio be the amount of 1%～20% culture medium, in temperature
Degree is 20-40 DEG C, rotating speed is that 7-30d is cultivated in 100-180r/min vibration；Take out culture bottle ultrasonic through 2～5min
Vibration, stands and treats that liquid is clarified, and takes out upper strata thalline thing, and extraction supernatant, by 0.22 μm membrane filtration, is collected and filtered
Liquid, obtains the lysate containing rare earth element.
6. the method utilizing the microorganism useless cathodic ray-tube fluorescent powder rare earth of extraction recovery described in claim 1-5, it is characterised in that
Still further comprise following steps: the solid matter on filter membrane is put into 105 DEG C of drying in Muffle furnace together with upper strata thalline,
Then at 500 DEG C of calcination 5h, the flying dust obtained 10% dilute nitric acid dissolution, obtain the lysate containing rare earth element.
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Cited By (7)
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| CN108754188A (en) * | 2018-07-01 | 2018-11-06 | 广西那神晞途环保科技有限公司 | Application and sandworm culture rare-earth precipitation liquid of the sandworm culture in precipitating rare earth |
| CN109402390A (en) * | 2018-11-12 | 2019-03-01 | 江西理工大学 | A method of utilizing bacillus subtilis spore recovering rare earth ion |
| CN109554547A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A method of utilizing indium in aspergillus niger Bioleaching waste liquid crystal display |
| CN109863254A (en) * | 2016-11-03 | 2019-06-07 | 新技术管理创新公司 | The method for recycling metal |
| CN110373549A (en) * | 2019-09-04 | 2019-10-25 | 贵州理工学院 | A kind of method of the dump leaching leaching slag of acidolysis containing rare earth recovering rare earth |
| CN113046554A (en) * | 2021-03-09 | 2021-06-29 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN114231740A (en) * | 2021-12-14 | 2022-03-25 | 内蒙古科技大学 | Method for decomposing monazite by using compound microorganisms |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108754188A (en) * | 2018-07-01 | 2018-11-06 | 广西那神晞途环保科技有限公司 | Application and sandworm culture rare-earth precipitation liquid of the sandworm culture in precipitating rare earth |
| CN109402390A (en) * | 2018-11-12 | 2019-03-01 | 江西理工大学 | A method of utilizing bacillus subtilis spore recovering rare earth ion |
| CN109402390B (en) * | 2018-11-12 | 2020-02-07 | 江西理工大学 | Method for recovering rare earth ions by utilizing bacillus subtilis spores |
| CN109554547A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A method of utilizing indium in aspergillus niger Bioleaching waste liquid crystal display |
| CN109554547B (en) * | 2018-12-14 | 2020-08-18 | 华南理工大学 | Method for leaching indium in liquid crystal display by aspergillus niger organisms |
| CN110373549A (en) * | 2019-09-04 | 2019-10-25 | 贵州理工学院 | A kind of method of the dump leaching leaching slag of acidolysis containing rare earth recovering rare earth |
| CN113046554A (en) * | 2021-03-09 | 2021-06-29 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN113046554B (en) * | 2021-03-09 | 2022-03-11 | 中南大学 | Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism |
| CN114231740A (en) * | 2021-12-14 | 2022-03-25 | 内蒙古科技大学 | Method for decomposing monazite by using compound microorganisms |
| CN114231740B (en) * | 2021-12-14 | 2023-07-14 | 内蒙古科技大学 | Method for decomposing monazite by utilizing composite microorganisms |
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