CN107119200A - A kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element - Google Patents
A kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element Download PDFInfo
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- CN107119200A CN107119200A CN201710283226.0A CN201710283226A CN107119200A CN 107119200 A CN107119200 A CN 107119200A CN 201710283226 A CN201710283226 A CN 201710283226A CN 107119200 A CN107119200 A CN 107119200A
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- mischmetal
- rare earth
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- old
- fluorescent material
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 47
- 229910001122 Mischmetal Inorganic materials 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004411 aluminium Substances 0.000 claims abstract description 19
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 230000002000 scavenging effect Effects 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 27
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 230000003750 conditioning effect Effects 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 238000003916 acid precipitation Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 238000005189 flocculation Methods 0.000 claims description 2
- 230000016615 flocculation Effects 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 14
- 229910052684 Cerium Inorganic materials 0.000 abstract description 5
- 229910052693 Europium Inorganic materials 0.000 abstract description 5
- 229910052771 Terbium Inorganic materials 0.000 abstract description 5
- 229910052788 barium Inorganic materials 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 229910052727 yttrium Inorganic materials 0.000 abstract description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 230000001698 pyrogenic effect Effects 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003672 processing method Methods 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910001940 europium oxide Inorganic materials 0.000 description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 229910003451 terbium oxide Inorganic materials 0.000 description 2
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 235000021180 meal component Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Classifications
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element, be calcined by low-temperature reduction, water logging removal of impurities, filtrate containing rare earth purification except aluminium, scavenging solution rare-earth precipitation reclaim processing step, waste and old mischmetal fluorescent material is handled by the way of wet method is combined using pyrogenic process.Realize the efficient removal and Y, Eu, Tb, Ce high efficiente callback of the impurity element such as aluminium, silicon, barium in waste and old mischmetal fluorescent material.This method is the processing method that a kind of environment-friendly, technique is simple, resource comprehensive utilization rate is high, energy consumption is low.Solve green powder in fluorescent RE powder, blue powder and reclaim difficult problem, with higher economic value.
Description
Technical field
The present invention relates to resource circulation utilization field, more particularly to a kind of waste and old mischmetal fluorescent material high efficiente callback rare earth
The method of element.
Background technology
According to statistics, the production capacity of rare-earth trichromatic fluorescent powder in 2014 is about 10000 tons, and waste and old mischmetal fluorescent material is about
5000 tons, main component is yittrium oxide 24%, cerium oxide 4.2%, europium oxide 2.3%, terbium oxide 2.6% and aluminum oxide
55.6%, respectively containing 130 tons of 1200 tons of yittrium oxide, 210 tons of cerium oxide, 106 tons of europium oxide and terbium oxide.Because discarded fluorescence
Waste meal component in lamp lamp powder and the production of lamp powder is complicated, and the rate that is recycled is relatively low, so most of useless powder and discarded glimmering
Light lamp is all burned with house refuse or landfill disposal is fallen.So processing can cause severe contamination to environment.Therefore, to waste and old
Fluorescent material carries out rare earth synthetical recovery, regeneration, can increase to the making full use of of China's rare earth resources, reduce energy resource consumption, solution
The problem of certainly China's per capita resources are poorer, the also protection to environment is respectively provided with significance.
The recycling for discarding fluorescent RE powder has both direction at present：One is the recovering rare earth from fluorescent material；Two
It is the separation of fluorescent RE powder.The technology of use has flotation partition method, high pressure digestion method, alkali process method etc..But at present these
There is high energy consumption, cost in method.
The content of the invention
Based on the problems of prior art, it is an object of the invention to provide a kind of waste and old mischmetal fluorescent material is efficient
The method of recovering rare earth element, can with better simply technique, at lower cost with energy consumption from waste and old mischmetal fluorescent material it is high
Imitate recovering rare earth element.
The purpose of the present invention is achieved through the following technical solutions：
Embodiment of the present invention also provides a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element, including
Following steps：
The first step, low-temperature reduction roasting：
Waste and old mischmetal fluorescent material, sodium sulfite, the concentrated sulfuric acid and water are mixed after mixing thoroughly, are placed in low temperature in Muffle furnace and roast
Burning obtains roasting material；
Second step, water logging removal of impurities：
The roasting material that the first step is obtained is levigate, then water logging under mechanical stirring, and filter residue is filtrated to get after water logging
With filtrate containing rare earth；
3rd step, the purification of filtrate containing rare earth removes aluminium：
By second step obtain described in filtrate containing rare earth with conditioning agent adjust pH value, then under agitation add flocculant remove
Aluminium, filtering, is purified liquid and filter residue containing aluminium；Wherein, the conditioning agent uses ammonium hydrogen carbonate, or ammoniacal liquor and sodium carbonate is mixed
Close solution；
4th step, scavenging solution rare-earth precipitation is reclaimed：
The scavenging solution addition oxalic acid that 3rd step is obtained precipitates rare earth element under stirring and obtains mischmetal,
Then the obtained mischmetal is precipitated and dries, calcines, that is, obtain mischmetal.
As seen from the above technical solution provided by the invention, waste and old mischmetal fluorescence provided in an embodiment of the present invention
The method of powder high efficiente callback rare earth element, its advantage is：The inventive method is by low-temperature bake, water logging removal of impurities, containing rare earth
Filtrate purification is realized to be combined with wet method using pyrogenic process and handles waste and old mix except several processing steps such as aluminium, scavenging solution rare-earth precipitation
Fluorescent RE powder is closed, effective recovery has been carried out to Y, Eu, Tb, Ce in waste and old mischmetal fluorescent material, is one and cleans, simply
Process route, energy consumption low feature high with resource comprehensive utilization rate.Compared with prior art, method of the invention is solved
The problem that high price rare earth element hardly possible is leached, reclaimed in waste and old mischmetal fluorescent material, leaching rate of Y, Eu, Tb, Ce is up to 95%
More than；Solve influence of the impurity element to recovering rare earth in re dip solution, Al, Si, Ba clearance respectively up to 98%,
92%th, more than 99%；Using NH3-CO3 2-System conditioning agent pH value, adds a small amount of flocculant and removes aluminium, solve prevailing technology and add
Alkali/acid for adjusting pH value removal of impurity metal and aluminium can cause to generate a large amount of colloids, the very poor phenomenon of strainability.This method design is closed
Manage, make full use of the property of each element and compound under given conditions, realize efficiently separating for each element, can be efficiently waste and old
The rare earth element such as Y, Eu, Tb, Ce in mischmetal fluorescent material, is one brand-new with very high economic benefit and the value of environmental protection
Process route, and during without " three wastes " discharge, it is environment-friendly, suitable for industrial applications.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the flow chart of waste and old mixed fluorescent powder synthetical recovery rare earth element method provided in an embodiment of the present invention.
Embodiment
With reference to the particular content of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made,
Belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element (referring to figure
1), be it is a kind of design advantages of simple, can high efficiency extraction Waste fluorescent powder rare earth elements, method low in the pollution of the environment, including with
Lower step：
The first step, low-temperature reduction roasting：
Waste and old mischmetal fluorescent material, sodium sulfite, the concentrated sulfuric acid and water are mixed after mixing thoroughly, are placed in low temperature in Muffle furnace and roast
Burning obtains roasting material；
Second step, water logging removal of impurities：
The roasting material that the first step is obtained is levigate, then water logging under mechanical stirring, is filtrated to get after water logging containing dilute
Native filtrate and filter residue；
3rd step, the purification of filtrate containing rare earth removes aluminium：
By second step obtain described in filtrate containing rare earth with conditioning agent adjust pH value, then under agitation add flocculant remove
Aluminium, filtering, is purified liquid and filter residue containing aluminium；Wherein, the conditioning agent uses ammonium hydrogen carbonate, or ammoniacal liquor and sodium carbonate is mixed
Close solution；
4th step, scavenging solution rare-earth precipitation is reclaimed：
The scavenging solution addition oxalic acid that 3rd step is obtained precipitates rare earth element under stirring and obtains mischmetal,
Then the obtained mischmetal is precipitated and dries, calcines, that is, obtain mischmetal.
In the first step of the above method, sodium sulfite addition for waste and old mischmetal fluorescent material weight 1.5%~
4.0%, the mass percentage concentration of the concentrated sulfuric acid is 98%, and the addition of the concentrated sulfuric acid is the 80% of waste and old mischmetal fluorescent material weight
~130%, the addition of water is the 5%~10% of waste and old mischmetal fluorescent material weight, and low-temperature bake temperature is 150~250
DEG C, roasting time is 0.5~2 hour.High price rare earth element can be converted into the low oxide beneficial to acidleach in the step,
Laid the foundation for follow-up efficiently leach.
In the second step of the above method, the roasting material that the first step is obtained is levigate to 100~200 mesh, then adds water
Leach, the liquid-solid ratio of water and the roasting material is 3：1~6：1, reaction temperature is room temperature~80 DEG C, and the reaction time is 2h~5h,
Mechanical agitation speed is 60~150r/min.The total rare earth leaching rate of the step is more than 95%, other impurity gold such as silicon, barium
Category clearance is respectively greater than 92% and 99%.
In 3rd step of the above method, by second step obtain described in filtrate containing rare earth with regulation solution adjust pH value to
2.5~3.5, flocculant addition (being added with reference to filtrate volume) is 0.2~1vt%, and reaction temperature is normal temperature, and the reaction time is
30~60min, the mixing speed of flocculation is 60~150r/min.NH is used in the step3-CO3 2-System adjusts pH value, a side
Face can make aluminum precipitation completely, on the other hand can substantially improve solution strainability, and aluminium clearance is dilute more than 98% during being somebody's turn to do
Earth elements loss late is less than 0.5%.
In the above method, flocculant can be using conventional flocculant, in the flocculants such as acrylamide, Sodium Polyacrylate
It is any.
In 4th step of the above method, the scavenging solution that the 3rd step is obtained adds oxalic acid precipitation rare earth element, oxalic acid
For 2~8 times of theoretical value, (theoretical value is the data drawn by experiment to addition, and the theoretical value precipitates dilute in scavenging solution completely
The amount of the required precipitating reagent of soil), the reaction time is 2~6h, and reaction temperature is normal temperature, and mixing speed is 60~150r/min.Should
In step, rare earth element rate of deposition is more than 97%, realizes the high efficiente callback of rare earth.
The method of the present invention is specifically described in further detail with reference to specific embodiment.
Embodiment：
The present embodiment provides a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element, its specific steps bag
Include：
Step 1) waste and old mischmetal fluorescent material, sodium sulfite, the concentrated sulfuric acid, water are pressed 100：2：110：5 mass ratioes are mixed
Mix thoroughly, be subsequently placed in low-temperature bake in Muffle furnace and obtain roasting material, sintering temperature is 200 DEG C, and roasting time is 1.5 hours；
Step 2) by step 1) in obtained roasting material it is levigate to 200 mesh, the then water logging in the case of mechanical agitation, liquid
Admittedly than 4：1, reaction temperature is 60 DEG C, and the reaction time is 3h, and mixing speed is 100r/min.It is filtrated to get after the completion of reaction containing dilute
Native filtrate and filter residue.Total rare earth leaching rate is more than 95% in the step, and other foreign metal clearance difference such as silicon, barium are big
In 92% and 99%；
Step 3) by step 2) in obtained filtrate containing rare earth with conditioning agent, (i.e. ammonium hydrogen carbonate or ammoniacal liquor+sodium carbonate are mixed
Close solution) regulation pH value is to 3.0, and flocculant addition is that (flocculant includes but is not limited to acrylamide, polypropylene to 0.5vt%
The conventional flocculant such as sour sodium), reaction temperature is normal temperature, and the reaction time is 50min, and mixing speed is 100r/min, filtering, is obtained
Aluminium clearance is more than 98% in scavenging solution and filter residue containing aluminium, the step, and rare earth element loss late is less than 0.5%；
Step 4) by step 3) in obtained scavenging solution add oxalic acid precipitation rare earth element, consumption of oxalic acid is 4 times of theoretical value,
Reaction time is 3h, and reaction temperature is normal temperature, and mixing speed is 100r/min, then precipitates the mischmetal obtained after precipitation
Dry, calcine, that is, the mischmetal being recycled.The step rare earth elements rate of deposition is more than 97%, realizes the height of rare earth
Effect is reclaimed.
The present invention method be calcined by low-temperature reduction, water logging removal of impurities, filtrate containing rare earth purification except aluminium, scavenging solution rare earth sink
Formed sediment the processing step reclaimed, and waste and old mischmetal fluorescent material is handled by the way of wet method is combined using pyrogenic process.Realize waste and old
The efficient removal of the impurity element such as aluminium, silicon, barium and Y, Eu, Tb, Ce high efficiente callback in mischmetal fluorescent material.This method is
The processing method that a kind of environment-friendly, technique is simple, resource comprehensive utilization rate is high, energy consumption is low.Solve green in fluorescent RE powder
Powder, blue powder reclaim difficult problem, with higher economic value.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (6)
1. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element, it is characterised in that comprise the following steps：
The first step, low-temperature reduction roasting：
Waste and old mischmetal fluorescent material, sodium sulfite, the concentrated sulfuric acid and water are mixed after mixing thoroughly, are placed in low-temperature bake in Muffle furnace and obtain
To roasting material；
Second step, water logging removal of impurities：
The roasting material that the first step is obtained is levigate, then water logging under mechanical stirring, is filtrated to get after water logging containing rare earth filter
Liquid and filter residue；
3rd step, the purification of filtrate containing rare earth removes aluminium：
By second step obtain described in filtrate containing rare earth with conditioning agent adjust pH value, then under agitation add flocculant remove aluminium,
Filtering, is purified liquid and filter residue containing aluminium；Wherein, the conditioning agent uses ammonium hydrogen carbonate, or ammoniacal liquor and sodium carbonate mixing
Solution；
4th step, scavenging solution rare-earth precipitation is reclaimed：
The scavenging solution addition oxalic acid that 3rd step is obtained precipitates rare earth element under stirring and obtains mischmetal, then
Obtained mischmetal precipitation is dried, calcined, that is, obtains mischmetal.
2. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element according to claim 1, its feature
It is, in the first step of methods described, sodium sulfite addition is the 1.5%~4.0% of waste and old mischmetal fluorescent material weight,
The mass percentage concentration of the concentrated sulfuric acid is 98%, the addition of the concentrated sulfuric acid for waste and old mischmetal fluorescent material weight 80%~
130%, the addition of water is the 5%~10% of waste and old mischmetal fluorescent material weight, and low-temperature bake temperature is 150~250 DEG C,
Roasting time is 0.5~2 hour.
3. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element according to claim 1 or 2, it is special
Levy and be, in the second step of methods described, the roasting material that the first step is obtained is levigate to 100~200 mesh, and then add water leaching
Go out, the liquid-solid ratio of water and the roasting material is 3：1~6：1, reaction temperature is room temperature~80 DEG C, and the reaction time is 2h~5h, machine
Tool mixing speed is 60~150r/min.
4. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element according to claim 1, its feature
Be, in the 3rd step of methods described, by second step obtain described in filtrate containing rare earth with conditioning agent adjust pH value to 2.5~
3.5, flocculant addition is 0.2~1vt%, and reaction temperature is normal temperature, and the reaction time is 30~60min, the stirring speed of flocculation
Spend for 60~150r/min.
5. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element according to claim 1 or 4, it is special
Levy and be, the flocculant uses any in acrylamide, Sodium Polyacrylate.
6. a kind of method of waste and old mischmetal fluorescent material high efficiente callback rare earth element according to claim 1,2 or 4, its
It is characterised by, in the 4th step of methods described, the scavenging solution that the 3rd step is obtained adds oxalic acid precipitation rare earth element, oxalic acid
Addition is 2~8 times of theoretical value, and the reaction time is 2~6h, and reaction temperature is normal temperature, and mixing speed is 60~150r/min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710283226.0A CN107119200B (en) | 2017-04-26 | 2017-04-26 | A kind of method of waste and old mischmetal fluorescent powder high efficiente callback rare earth element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710283226.0A CN107119200B (en) | 2017-04-26 | 2017-04-26 | A kind of method of waste and old mischmetal fluorescent powder high efficiente callback rare earth element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107119200A true CN107119200A (en) | 2017-09-01 |
| CN107119200B CN107119200B (en) | 2019-02-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710283226.0A Expired - Fee Related CN107119200B (en) | 2017-04-26 | 2017-04-26 | A kind of method of waste and old mischmetal fluorescent powder high efficiente callback rare earth element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107119200B (en) |
Cited By (5)
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| CN108004410A (en) * | 2017-12-15 | 2018-05-08 | 清远先导材料有限公司 | A kind of extracting method of rare earth silicate crystals element |
| CN108913918A (en) * | 2018-07-09 | 2018-11-30 | 武汉工程大学 | A method of utilizing extremely dilute earth solution recovering rare earth of weathered superficial leaching rare-earth ore Situ Leaching |
| CN113136495A (en) * | 2021-04-28 | 2021-07-20 | 江西理工大学 | Method for pre-enriching rare earth elements in waste fluorescent powder |
| CN114703366A (en) * | 2022-04-24 | 2022-07-05 | 中南大学 | Method for treating waste CRT fluorescent powder by concentrated sulfuric acid directional transformation |
| CN114854990A (en) * | 2022-04-24 | 2022-08-05 | 中南大学 | Method for recovering rare earth from waste CRT fluorescent powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108004410A (en) * | 2017-12-15 | 2018-05-08 | 清远先导材料有限公司 | A kind of extracting method of rare earth silicate crystals element |
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| CN108913918A (en) * | 2018-07-09 | 2018-11-30 | 武汉工程大学 | A method of utilizing extremely dilute earth solution recovering rare earth of weathered superficial leaching rare-earth ore Situ Leaching |
| CN113136495A (en) * | 2021-04-28 | 2021-07-20 | 江西理工大学 | Method for pre-enriching rare earth elements in waste fluorescent powder |
| CN114703366A (en) * | 2022-04-24 | 2022-07-05 | 中南大学 | Method for treating waste CRT fluorescent powder by concentrated sulfuric acid directional transformation |
| CN114854990A (en) * | 2022-04-24 | 2022-08-05 | 中南大学 | Method for recovering rare earth from waste CRT fluorescent powder |
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| CN107119200B (en) | 2019-02-01 |
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