CN106044833B - A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker - Google Patents
A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker Download PDFInfo
- Publication number
- CN106044833B CN106044833B CN201610396411.6A CN201610396411A CN106044833B CN 106044833 B CN106044833 B CN 106044833B CN 201610396411 A CN201610396411 A CN 201610396411A CN 106044833 B CN106044833 B CN 106044833B
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- China
- Prior art keywords
- rare earth
- electrolysis
- reclaimed materials
- clinker
- fluoride
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- 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
- 239000000463 material Substances 0.000 title claims abstract description 28
- -1 rare earth fluoride Chemical class 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000007885 magnetic separation Methods 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 238000004806 packaging method and process 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
- 239000000203 mixture 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
- 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
- 230000008859 change Effects 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 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
- 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
- 230000008901 benefit Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration 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
- 230000008569 process Effects 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
Abstract
The present invention discloses a kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker, using rare earth electrode scrap reclaimed materials and clinker as raw material, by block stock after sieving, non-rare earth bulk impurity is removed, sieving, ball milling, magnetic separation；The above-mentioned raw material for crossing the most of iron of removing after magnetic separation choosing is mixed with lithium fluoride；Melt it mixture progress heating, continue to enough liquid levels；Splash bar, filter residue are carried out to above-mentioned fused solution；Filtrate after above-mentioned filter residue is subjected to electrolysis removal of impurities, electrolysis occurs dragging for slag after anode effect, and supernatant is carried out into cyclic electrolysis；By obtained supernatant, detected, reach and title packaging is crossed after standard, be final recovery product.The present invention can be facilitated effectively purifies rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker, has saved resource, has reduced pollution, with technique it is simple, it is with low cost the characteristics of.
Description
Technical field
The present invention relates to a kind of rare-earth smelting technology, particularly one kind reclaims dilute from rare earth electrode scrap reclaimed materials and clinker
The method of native fluoride.
Background technology
Rare earth has serious environmental pollution and ecological disruption as a kind of mineral resources in recovery process, therefore,
The recovering rare earth from the trade waste containing rare earth element, sustainable development and environmental protection to China's rare earth resources have weight
The meaning wanted.After rare earth permanent-magnetic material is developed rapidly since the nineties in last century, downstream wind-powered electricity generation, the electricity of rare earth permanent magnet product are used as
Mechanical, electrical electrical automobile is developed faster, the demand for causing the presence for the high performance magnet that rare earth permanent magnet is representative huge, so that
Create and developed rapidly as this industry of rare earth metal of rare earth permanent-magnetic material main raw material.Rare earth metal is processed
Substantial amounts of waste material, most importantly Rare Earth Electrolysis slag are formd in journey.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 extremely steady
Fixed not disposable, bargain price is high, and yield is low, and equivalent recovery handling per ton is up to 8.5 ten thousand yuan.So, develop from rare earth
The reutilization technology of recovering rare earth fluoride in electrode scrap reclaimed materials and clinker, with huge realistic meaning and economic benefit.
The text found no on the recovering rare earth fluoride methods from rare earth electrode scrap reclaimed materials and clinker is consulted at present
Offer, the present invention has originality.
The content of the invention
It is an object of the invention to provide a kind of side of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker
Method, to economize on resources, reduces pollution.
In order to reach above-mentioned purpose, solution of the invention is：
A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker, with rare earth electrode scrap reclaimed materials
It is raw material with clinker, carries out according to the following steps：
The first step, by block stock after sieving, the non-rare earth bulk impurity such as graphite block and anode screw rod is removed, mistake
Sieve, ball milling, magnetic separation；
Second step, the above-mentioned raw material for crossing the most of iron of removing after magnetic separation choosing is mixed with lithium fluoride by certain weight ratio；
3rd step, mixture is carried out into heating certain temperature melts it, continues to enough liquid levels；
4th step, splash bar, filter residue are carried out to above-mentioned fused solution；
5th step, carries out electrolysis removal of impurities, electrolysis occurs dragging for slag after anode effect, by supernatant by the filtrate after above-mentioned filter residue
Carry out cyclic electrolysis；
6th step, obtained supernatant is detected, reaches and title packaging is crossed after standard, is final recovery product.
Further, in the first step block stock after sieving, size distribution after sieving 0.1~1mm it
Between.
Further, in the second step, the mass ratio that raw material is mixed with lithium fluoride is 1:1~1:1.2.
Further, in the 3rd step, heating-up temperature is 1200 DEG C~1400 DEG C, and charging rate is 1 ± 0.2kg/
5min hours, arc acc power is beaten for 50-70kw, and liquid level keeps electrolysis normal level of liquid.
Further, in the 4th step, the aperture in filter residue spoon hole is 0.5-0.7mm, often heats 1h filter residues once, including
Furnace bottom slagging and liquid level floating carbon dust, stirring：1 time/half an hour.
Further, in the 5th step, electrolysis temperature is higher by 100-150 DEG C of electrolytic metal temperature, and liquid level keeps electrolysis
Standard liquid level；Supernatant is scooped out, re-electrolysis is carried out；Such cyclic electrolysis, electrolysis due to needing more waste material impurity more every time
Change electrolytic furnace and carry out electrolysis removal of impurities.
Further, in the 6th step, standard be reclaimed materials in Fe≤1000ppm, Si≤1000ppm, Al≤
1000ppm, Ca≤500ppm, Na≤500ppm.
After such scheme, the present invention by being sieved to rare earth electrode scrap reclaimed materials and clinker, ball milling, magnetic separation,
The less waste material of iron content is obtained, is mixed with lithium fluoride, heating fusing, by filtering, obtains the less supernatant of impurity, will obtained
Supernatant be placed in clean electrolytic furnace and be electrolysed, the carbon dust of floating and the body refuse sunk to the bottom are dragged for during electrolysis
Go out, obtained supernatant proceeds to be electrolysed, drags for slag, so electrolysis 2-3 time, obtain supernatant and detected, it is qualified after by time
Rare earth fluoride packaging is received, the rare earth fluoride of recoverable is obtained.The present invention can facilitate effective from the recovery of rare earth electrode scrap
Material and clinker in purify rare earth fluoride, saved resource, reduced pollution, with technique it is simple, it is with low cost the characteristics of.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
Coordinate shown in Fig. 1, following techniques with specific a processing rare earth electrode scrap reclaimed materials and clinker the present invention is done into
One step is described in detail, but is not intended as limiting the scope of the invention.
Take 300 kg rare earth electrode scrap reclaimed materials and clinker（Neodymium）, after general-purpose crusher in crushing, 5mm coarse nets are sieved through sieve.
Powder ball mill grinding after sieving, final rare earth electrode scrap reclaimed materials and clinker（Neodymium）The average grain diameter of powder is 0.1-1
mm。
Above-mentioned rare earth electrode scrap reclaimed materials and clinker are mixed with industrial lithium fluoride（Neodymium）Powder, lithium fluoride and rare earth electrode scrap
Reclaimed materials and clinker（Neodymium）The mass ratio 1.15 of powder:1.Arc heating fusing, liquid level temperature 1200-1400 are played in electrolytic furnace
DEG C, liquid level reaches electrolysis liquid surface.
Not slag mud and the liquid level floating of furnace bottom are put into graphite chip and salvage clean, supernatant is taken out in clean electrolysis
Stove is electrolysed, and electrolysis temperature is controlled at 1060 ± 20 DEG C, during furnace bottom occur body refuse, liquid level also has graphite bits, often
Half an hour is dragged for once, and anode effect is arrived in electrolysis, scoops out supernatant.
Obtained supernatant is scooped out and carries out second of electrolysis in clean electrolytic furnace, normal electrolysis, electrolysis temperature is maintained
Control at 1060 ± 20 DEG C, during furnace bottom occur body refuse, liquid level also has graphite bits, is dragged for once per half an hour, is electrolysed
To anode effect, supernatant is scooped out.
Obtain supernatant and detect non-rare earth rare earth impurities, respectively Fe≤1000ppm, Si≤1000ppm, Al≤
1000ppm, Ca≤500ppm, Na≤500ppm, reach that I takes charge of use requirement, can be without next one-step electrolysis removal of impurities.Weigh
Obtain 183kg rare earth fluorides.
Described above is the embodiment 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, some improvements and modifications can also be made, these improvements and modifications are also considered as
The protection model of the present invention is used.
Claims (7)
1. a kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker, it is characterised in that with the useless electricity of rare earth
Pole reclaimed materials and clinker are raw material, are carried out according to the following steps：
The first step, by block stock after sieving, non-rare earth bulk impurity is removed, sieving, ball milling, magnetic separation；
Second step, the above-mentioned raw material for crossing the most of iron of removing after magnetic separation choosing is mixed with lithium fluoride；
3rd step, melts it mixture progress heating, continues to enough liquid levels；
4th step, is stirred, filter residue to above-mentioned fused solution；
5th step, electrolysis removal of impurities is carried out by the filtrate after above-mentioned filter residue, and electrolysis occurs dragging for slag after anode effect, supernatant is carried out
Cyclic electrolysis；
6th step, obtained supernatant is detected, reaches and title packaging is crossed after standard, is final recovery product.
2. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In the first step, block stock is after sieving, and the size distribution after sieving is between 0.1~1mm.
3. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In the second step, the mass ratio that raw material is mixed with lithium fluoride is 1:1~1:1.2.
4. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In 3rd step, heating-up temperature is 1200 DEG C~1400 DEG C, and charging rate is 1 ± 0.2kg/5min hours,
It is 50-70kw to beat arc acc power, and liquid level keeps electrolysis normal level of liquid.
5. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In 4th step, the aperture in filter residue spoon hole is 0.5-0.7mm, often heats 1h filter residues once, including furnace bottom knot
Slag and liquid level floating carbon dust, stirring：1 time/half an hour.
6. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In 5th step, electrolysis temperature is higher by 100-150 DEG C of electrolytic metal temperature, and liquid level keeps electrolysis titer
Face；Supernatant is scooped out, re-electrolysis is carried out；Such cyclic electrolysis, every time electrolysis is electrolysed more due to needing to change waste material impurity
Stove carries out electrolysis removal of impurities.
7. a kind of method of recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker according to claim 1,
It is characterized in that：In 6th step, standard is Fe≤1000ppm, Si≤1000ppm, Al≤1000ppm, Ca in reclaimed materials
≤ 500ppm, Na≤500ppm.
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| Application Number | Priority Date | Filing Date | Title |
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| 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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| 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 CN106044833A (en) | 2016-10-26 |
| CN106044833B true CN106044833B (en) | 2017-10-27 |
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Families Citing this family (4)
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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 |
| 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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Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee after: Fujian Jinlong Rare Earth Co.,Ltd. Address before: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. |