CN106044833A - Method for recovering rare earth fluoride from electrode scrap reclaimed material and slag of rare earth - Google Patents
Method for recovering rare earth fluoride from electrode scrap reclaimed material and slag of rare earth Download PDFInfo
- Publication number
- CN106044833A CN106044833A CN201610396411.6A CN201610396411A CN106044833A CN 106044833 A CN106044833 A CN 106044833A CN 201610396411 A CN201610396411 A CN 201610396411A CN 106044833 A CN106044833 A CN 106044833A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- slag
- electrolysis
- fluoride
- reclaimed materials
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 64
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 41
- 239000002893 slag Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 30
- -1 rare earth fluoride Chemical class 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 238000007885 magnetic separation Methods 0.000 claims abstract description 7
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims abstract description 4
- 239000000706 filtrate Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 6
- 238000007667 floating Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910016468 DyF3 Inorganic materials 0.000 description 1
- 229910017557 NdF3 Inorganic materials 0.000 description 1
- 229910019322 PrF3 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering rare earth fluoride from an electrode scrap reclaimed material and slag of rare earth. The electrode scrap reclaimed material and the slag of the rare earth are taken as raw materials, the massive raw materials are sieved, non-rare-earth impurity blocks are removed, and the materials are subjected to sieving, ball milling and magnetic separation; the materials with most iron removed after magnetic separation are mixed with lithium fluoride; the mixture is heated to be melted until a melted liquid reaches a sufficient liquid level; the melted liquid is stirred and subjected to slag removal through filtering; a filtrate after slag removal is subjected to electrolytic impurity removal, slag is fished after an anode effect occurs in electrolysis, and a supernatant is subjected to cyclic electrolysis; the obtained supernatant is detected and is weighed and packaged after reaching the standard, and the final recovery product is obtained. Rare earth fluoride can be extracted conveniently and effectively from the electrode scrap reclaimed material and the slag of the rare earth, resources are saved, pollution is reduced, and the method has the characteristics of simple process and low cost.
Description
Technical field
The present invention relates to a kind of rare-earth smelting technology, particularly one and reclaim dilute from rare earth electrode scrap reclaimed materials and slag
The method of soil fluoride.
Background technology
Rare earth, as a kind of mineral resources, also exists serious environmental pollution and ecological disruption in recovery process, therefore,
Recovering rare earth from the trade waste containing rare earth element, sustainable development and protection environment to China's rare earth resources have weight
The meaning wanted.After since the nineties in last century, rare earth permanent-magnetic material develops rapidly, as downstream wind-powered electricity generation, the electricity of rare earth permanent magnet product
Mechanical, electrical electrical automobile is developed faster, the demand that the existence of the high performance magnet causing rare earth permanent magnet to be representative is huge, thus
Create developing rapidly of this industry of rare earth metal as the main raw material of rare earth permanent-magnetic material.Rare earth metal is processed
Journey defines substantial amounts of waste material, most importantly Rare Earth Electrolysis slag.Its content of rare earth is higher, wherein NdF3、PrF3、DyF3
Content by weight 70～80%, 15～20%, 2～5%.Meanwhile, waste material is mainly based on rare earth fluoride, and fluoride is the most steady
Fixed the most disposable, bargain price is high, and yield is low, and equivalent recovery handling per ton is up to 8.5 ten thousand yuan.So, exploitation is from rare earth
The reutilization technology of recovering rare earth fluoride in electrode scrap reclaimed materials and slag, has huge realistic meaning and economic benefit.
Consult at present and find no about the literary composition of recovering rare earth fluoride methods from rare earth electrode scrap reclaimed materials and slag
Offering, the present invention has originality.
Summary of the invention
It is an object of the invention to provide a kind of side of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag
Method, to economize on resources, reduces and pollutes.
In order to reach above-mentioned purpose, the solution of the present invention is:
A kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag, with rare earth electrode scrap reclaimed materials and stove
Slag is raw material, sequentially includes the following steps:
The first step, by block stock after sieving, by non-rare earth bulk Impurity removals such as graphite block and anode screw rods, sieve,
Ball milling, magnetic separation；
Second step, the raw material removing major part ferrum after the above-mentioned choosing of magnetic separation excessively is mixed by certain weight ratio with lithium fluoride；
3rd step, carries out mixture heating uniform temperature and makes it melt, continue to enough liquid levels；
4th step, carries out splash bar, filtering residue to above-mentioned fused solution；
5th step, carries out being electrolysed remove impurity by the filtrate after above-mentioned filtering residue, and electrolysis is dragged for slag after there is anode effect, carried out by supernatant
Cyclic electrolysis；
6th step, the supernatant that will obtain, detects, crosses and claim packaging, be i.e. finally to reclaim product after reaching standard.
Further, in the described first step, block stock is after sieving, the particle size distribution after sieving 0.1～1mm it
Between.
Further, in described second step, the mass ratio that raw material mixes with lithium fluoride is 1:1～1:1.2.
Further, in described 3rd step, heating-up temperature is 1200 DEG C～1400 DEG C, and charging rate is 1 ± 0.2kg/
5min hour, beating arc acc power was 50-70kw, and liquid level keeps electrolysis normal level of liquid.
Further, in described 4th step, the aperture in filtering residue spoon hole is 0.5-0.7mm, and often heating 1h filtering residue is once, including
Furnace bottom slagging scorification and the floating carbon dust of liquid level, stirring: 1 time/half an hour.
Further, in described 5th step, electrolysis temperature exceeds electrolytic metal temperature 100-150 DEG C, and liquid level keeps electrolysis
Standard liquid level；Supernatant is scooped out, carries out re-electrolysis；So cyclic electrolysis, electrolysis is due to the many needs of waste material impurity more every time
Change electrolytic furnace to carry out being electrolysed remove impurity.
Further, in described 6th step, standard is Fe≤1000ppm in reclaimed materials, Si≤1000ppm, Al≤
1000ppm, Ca≤500ppm, Na≤500ppm.
Use after such scheme, the present invention by rare earth electrode scrap reclaimed materials and slag sieves, ball milling, magnetic separation,
Obtain the less waste material of iron content, mix with lithium fluoride, add heat fusing, through filtering, obtain the less supernatant of impurity, will obtain
Supernatant be placed in clean electrolytic furnace and be electrolysed, during electrolysis, floating carbon dust and the body refuse sunk to the bottom are dragged for
Going out, the supernatant obtained proceeds electrolysis, drags for slag, and so electrolysis 2-3 time, obtains supernatant and detect, qualified after incite somebody to action back
Receipts rare earth fluoride is packed, and obtains the rare earth fluoride of recoverable.The present invention can facilitate and effectively reclaim from rare earth electrode scrap
Material and slag purify rare earth fluoride, has saved resource, decreased pollution, had the advantages that technique is simple, with low cost.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Coordinate shown in Fig. 1, the following technique specifically processing rare earth electrode scrap reclaimed materials and slag with one present invention is done into
One step describes in detail, but is not intended as limiting the scope of the invention.
Taking 300 kg rare earth electrode scrap reclaimed materials and slags (neodymium), after general-purpose crusher in crushing, 5mm coarse net is sieved through sieve.
Powder ball mill grinding after sieving, the mean diameter of final rare earth electrode scrap reclaimed materials and slag (neodymium) powder is 0.1-1
mm。
Above-mentioned rare earth electrode scrap reclaimed materials and slag (neodymium) powder, lithium fluoride and rare earth electrode scrap is mixed with industry lithium fluoride
Reclaimed materials and the mass ratio 1.15:1 of slag (neodymium) powder.In electrolytic furnace, beat arc add heat fusing, liquid level temperature 1200-1400
DEG C, liquid level reaches electrolysis liquid surface.
Not slag mud and the floating graphite chip of putting into of liquid level of furnace bottom are salvaged clean, takes out supernatant in clean electrolysis
Stove is electrolysed, and electrolysis temperature controls at 1060 ± 20 DEG C, during furnace bottom there will be body refuse, liquid level also have graphite bits, often
Half an hour, drags for once, electrolysis to anode effect, scoops out supernatant.
The supernatant obtained is scooped out and carries out being electrolysed for the second time at clean electrolytic furnace, maintain normal electrolysis, electrolysis temperature
Control at 1060 ± 20 DEG C, during furnace bottom there will be body refuse, liquid level also have graphite bits, per half an hour, drags for once, electrolysis
To anode effect, scoop out supernatant.
Obtain supernatant detect non-rare earth rare earth impurities, respectively Fe≤1000ppm, Si≤1000ppm, Al≤
1000ppm, Ca≤500ppm, Na≤500ppm, reach me and take charge of use requirement, can not carry out next step electrolysis remove impurity.Weigh
Obtain 183kg rare earth fluoride.
The above is the detailed description of the invention of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as
The protection model of the present invention is used.
Claims (7)
1. the method for recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag, it is characterised in that with the useless electricity of rare earth
Pole reclaimed materials and slag are raw material, sequentially include the following steps:
The first step, by block stock after sieving, by non-rare earth bulk Impurity removal, sieve, ball milling, magnetic separation；
Second step, the raw material removing major part ferrum after the above-mentioned choosing of magnetic separation excessively mixes with lithium fluoride；
3rd step, carries out heating by mixture and makes it melt, and continues to enough liquid levels；
4th step, carries out splash bar, filtering residue to above-mentioned fused solution；
5th step, carries out being electrolysed remove impurity by the filtrate after above-mentioned filtering residue, and electrolysis is dragged for slag after there is anode effect, carried out by supernatant
Cyclic electrolysis；
6th step, the supernatant that will obtain, detects, crosses and claim packaging, be i.e. finally to reclaim product after reaching standard.
2. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in the described first step, block stock is after sieving, and the particle size distribution after sieving is between 0.1～1mm.
3. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in described second step, the mass ratio that raw material mixes with lithium fluoride is 1:1～1:1.2.
4. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in described 3rd step, heating-up temperature is 1200 DEG C～1400 DEG C, and charging rate is 1 ± 0.2kg/5min hour,
Beating arc acc power is 50-70kw, and liquid level keeps electrolysis normal level of liquid.
5. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in described 4th step, the aperture in filtering residue spoon hole is 0.5-0.7mm, and often heating 1h filtering residue is once, ties including furnace bottom
Slag and the floating carbon dust of liquid level, stirring: 1 time/half an hour.
6. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in described 5th step, electrolysis temperature exceeds electrolytic metal temperature 100-150 DEG C, and liquid level keeps electrolysis titer
Face；Supernatant is scooped out, carries out re-electrolysis；So cyclic electrolysis, electrolysis needs to change electrolysis owing to waste material impurity every time
Stove carries out being electrolysed remove impurity.
7. according to a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and slag described in claim 1,
It is characterized in that: in described 6th step, standard is Fe≤1000ppm in reclaimed materials, Si≤1000ppm, Al≤1000ppm, Ca
≤ 500ppm, Na≤500ppm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610396411.6A CN106044833B (en) | 2016-06-07 | 2016-06-07 | A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610396411.6A CN106044833B (en) | 2016-06-07 | 2016-06-07 | A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker |
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| Publication Number | Publication Date |
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| CN106044833A true CN106044833A (en) | 2016-10-26 |
| CN106044833B CN106044833B (en) | 2017-10-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487089A (en) * | 2019-01-07 | 2019-03-19 | 江西理工大学 | A kind of method of rare earth fluoride molten-salt electrolysis Slag treatment |
| CN111876795A (en) * | 2020-07-28 | 2020-11-03 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
| CN113061756A (en) * | 2021-03-17 | 2021-07-02 | 赣州齐畅新材料有限公司 | Method for extracting rare earth from rare earth organic slag |
| CN113265552A (en) * | 2021-04-30 | 2021-08-17 | 福建省长汀金龙稀土有限公司 | Preparation method of rare earth holmium copper alloy for magnetic refrigeration |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109487089A (en) * | 2019-01-07 | 2019-03-19 | 江西理工大学 | A kind of method of rare earth fluoride molten-salt electrolysis Slag treatment |
| CN111876795A (en) * | 2020-07-28 | 2020-11-03 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
| CN111876795B (en) * | 2020-07-28 | 2022-12-06 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
| CN113061756A (en) * | 2021-03-17 | 2021-07-02 | 赣州齐畅新材料有限公司 | Method for extracting rare earth from rare earth organic slag |
| CN113265552A (en) * | 2021-04-30 | 2021-08-17 | 福建省长汀金龙稀土有限公司 | Preparation method of rare earth holmium copper alloy for magnetic refrigeration |
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| CN106044833B (en) | 2017-10-27 |
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