CN114540625A - Method for recovering rare earth oxide by using rare earth magnetic material waste - Google Patents
Method for recovering rare earth oxide by using rare earth magnetic material waste Download PDFInfo
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- CN114540625A CN114540625A CN202210185196.0A CN202210185196A CN114540625A CN 114540625 A CN114540625 A CN 114540625A CN 202210185196 A CN202210185196 A CN 202210185196A CN 114540625 A CN114540625 A CN 114540625A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 60
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002699 waste material Substances 0.000 title claims abstract description 25
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 23
- 239000000696 magnetic material Substances 0.000 title claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 80
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000011282 treatment Methods 0.000 claims abstract description 26
- 238000011049 filling Methods 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 38
- 238000001816 cooling Methods 0.000 claims description 29
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 15
- 229910001325 element alloy Inorganic materials 0.000 claims description 6
- 230000000452 restraining effect Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 11
- 238000005192 partition Methods 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- -1 rare earth compounds Chemical class 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000002955 isolation Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011221 initial treatment Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000012716 precipitator Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 101100327917 Caenorhabditis elegans chup-1 gene Proteins 0.000 description 2
- 229910020598 Co Fe Inorganic materials 0.000 description 2
- 229910002519 Co-Fe Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 239000006148 magnetic separator Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0073—Selection or treatment of the reducing gases
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering rare earth oxide by using rare earth magnetic material waste, belonging to the field of rare earth elements. A method for recovering rare earth oxide by using rare earth magnetic material waste comprises the following steps: step (1): crushing a treatment material at least containing rare earth elements and iron group elements, and then carrying out oxidation treatment to obtain oxides; step (2): putting the oxide into a heating device, heating to 360 ℃, filling reducing gas into the heating device, and reducing O in the heating device2Content (c); and (3): heating the heating device, and fully reducing the reducing gas and the oxide of the iron group element at the temperature of 360-1300 ℃ to obtain the iron group elementThe oxide is reduced to an iron group element by the reducing gas. The method can recover the rare earth oxide from the rare earth magnetic material waste, has the advantages of simple operation, low cost, no acid-base continuous circulation, no waste and suitability for continuous operation.
Description
Technical Field
The invention relates to the field of rare earth elements, in particular to a method for recovering rare earth oxide by utilizing rare earth magnetic material waste.
Background
The neodymium iron boron permanent magnet material is widely applied to the fields of national defense war industry, aerospace, medical appliances, computers, electronics, new energy automobile industry and the like due to the excellent magnetic property.
The R-Fe-B permanent magnet produced in the world at present is over thirty million tons, and the waste materials such as magnet scraps, cutting scraps, grinding scraps, ultrafine powder and the like in the manufacturing process account for 20-30% of the input material proportion. Also over time, permanent magnets, which are parts of various products, are becoming obsolete. How to recover various elements contained therein, particularly rare earth elements, in a green manner at low cost is an important technical issue.
The R-Fe-B permanent magnet is commonly used in the fields of electric machinery, medical instruments, toys, packaging, hardware machinery, aerospace and the like, such as a permanent magnet motor, a loudspeaker, a magnetic separator, a computer disk driver, a magnetic resonance imaging equipment instrument and the like.
Samarium cobalt permanent magnet material is one kind of rare earth permanent magnet, and the permanent magnet prepared by mixing rare earth elements of samarium, cobalt and other elements has high magnetic energy product and extremely low temperature coefficient, and the maximum working temperature can reach 350 ℃.
Application No. CN97120123.4 discloses a method for recovering rare earth compounds, which is a method for recovering rare earth compounds, comprising the following steps: (1) primary treatment of the recovered raw materials; (2) leaching the rare earth compound by acid solution; (3) filtering; (4) precipitating a solution containing rare earth metal ions; (5) drying and firing the precipitate; the method is characterized in that: (1) in the primary treatment of the recycled raw materials, the non-metallic inclusions are removed from the alloy waste, leftover materials, defective products, waste products and sludge containing rare earth compounds by a physical screening method; after non-metallic inclusions of oil stains containing rare earth metals are screened and removed by a physical method, the oil stains are heated and incinerated in a common heating furnace in the atmosphere, the heating temperature is more than or equal to 500 ℃, and the heating time is 2-4 hours. (2) The recovered raw materials are put into a material dissolving pool after the primary treatment, proper water is added at the same time, hydrochloric acid is adopted as a leaching solution and is gradually added into the material dissolving pool, the raw materials containing rare earth compounds are leached, water and hydrochloric acid are added after the leaching solution is discharged, the residual raw materials in the pool are leached for the second time, the first treatment time is 10-18 hours, and the second treatment time is 5-10 hours; (3) putting the leached and filtered leaching solution containing rare earth metal ions into a precipitator, heating the solution to 60-90 ℃, injecting an oxalic acid solution into the precipitator by taking the oxalic acid solution as a precipitator, and carrying out precipitation treatment, wherein the oxalic acid solution is also heated to 60-90 ℃; (4) washing the precipitate obtained by precipitation treatment with clear water for 3-4 times, and spin-drying; (5) and (3) placing the washed precipitate containing the rare earth metal in a tunnel furnace for drying and burning, wherein the burning temperature is 800 ℃.
Application No. CN201580016947.4 discloses a method for recovering rare earth elements, specifically discloses the following method: in a method for separating and recovering a rare earth element as an oxide from an iron group element by subjecting an object to be treated containing at least the rare earth element and the iron group element to an oxidation treatment and then subjecting the object to a heat treatment in the presence of carbon, the method is capable of separating the rare earth oxide from the iron group element with low treatment cost and high efficiency, and also capable of suppressing the consumption and damage of a treatment vessel and capable of being repeatedly used for a long period of time. The method of the present invention as a solution to this problem is characterized in that the object to be treated subjected to the oxidation treatment is mixed with petroleum coke as a carbon supply source and stored in a treatment vessel, and the heat treatment is performed at a temperature of 950 to 1150 ℃ (excluding 1150 ℃) in an inert gas atmosphere or in vacuum.
The technical scheme provided by the patent has the following defects:
1. the iron oxide and carbon are solid at temperatures below 1597 ℃, the reaction between the solid and the solid is impossible without contact, the reaction rate is relatively slow even with contact, the diffusion process of the solid-solid reaction is very slow, and the reaction is insufficient.
2. The reaction time of iron oxide with carbon is long.
3. The reaction is incomplete and a large proportion of iron is still mixed with the rare earth oxide in the form of oxide.
4. After the reaction is finished, the rare earth oxide and the carbon powder are not easy to be completely separated by adopting a physical method.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for recovering rare earth oxide by utilizing rare earth magnetic material waste, which can recover rare earth oxide from the rare earth magnetic material waste, and has the advantages of simple operation, low cost, no acid-base continuous circulation, no waste and suitability for continuous operation.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for recovering rare earth oxide by using rare earth magnetic material waste comprises the following steps:
step (1): crushing a treatment material at least containing rare earth elements and iron group elements, and then carrying out oxidation treatment to obtain oxides;
step (2): putting the oxide into a heating device, heating to 360 ℃, filling reducing gas into the heating device, and reducing O in the heating device2Content (c);
and (3): heating the heating device, and fully reducing the reducing gas and the oxide of the iron group element at the temperature of 360-1300 ℃, wherein the oxide of the iron group element is reduced into the iron group element by the reducing gas;
and (4): pouring the material reacted in the step (3) into a cooling device, adding liquid nitrogen into the cooling device, cooling the material reacted in the step (3) by the liquid nitrogen, and cooling to the temperature below 100 ℃; and (4) separating the materials after the reaction in the step (3) to obtain rare earth oxide and iron group element alloy.
Preferably, the reducing gas is NH3Or CO.
Preferably, the particle size of the treated material crushed in the step (1) is less than 0.85 mm.
Preferably, the treatment material containing at least rare earth elements and iron group elements is a material which has been degreased.
Preferably, the heating device can be selected from an atmosphere protection rotary kiln, an atmosphere furnace or a tunnel kiln.
The cooling device comprises a cup body with a cavity, a cup cover and a stirring and separating device; the cup cover is covered at the opening at the top end of the cup body; the top end of the cup cover is provided with a first motor; the stirring and separating device is arranged in the cup body; the stirring and separating device comprises a rotating shaft, an upper belt pulley, a separating disc, a supporting stirring rod and an annular magnetic strip, wherein the upper belt pulley is rotatably connected to the rotating shaft; the top end of the rotating shaft penetrates through the cup cover to be connected with the output end of the first motor, and the bottom end of the rotating shaft penetrates through the middle part of the separating disc to be fixedly connected with the supporting stirring rod; a plurality of feed openings are formed in the separating disc, a material collecting device is arranged between the separating disc and the supporting stirring rod, and materials fall into the material collecting device from the feed openings; the left side and the right side of the top end of the separating disc are respectively provided with a first through hole and a second through hole; the annular magnetic strip passes through the first through hole and the second through hole and is wound between the belt pulley and the supporting stirring rod, and the belt pulley drives the annular magnetic strip to rotate clockwise; the shape of the second through hole is matched with that of the annular magnetic strip; the scraper is arranged on the separating disc and clings to the outer surface of the annular magnetic strip passing through the second through hole; the outer surface of the annular magnetic strip is magnetic, and the inner surface of the annular magnetic strip is nonmagnetic.
Preferably, the material collecting device comprises a collecting bag, a first spring, a boss, a bag restraining ring and a first spring; the boss is fixedly arranged at the joint of the support stirring rod and the rotating shaft; the collecting bag is sleeved outside the rotating shaft, the top end of the collecting bag is connected to the bottom end of the separating disc, the collecting bag is connected to the boss, and the discharging opening is located right above the inner cavity of the collecting bag; the first spring and the bag binding ring are sleeved outside the collecting bag; the first spring is fixedly connected between the bag binding ring and the boss.
Preferably, the separating plate is arranged on the separating disc; the partition plate divides the partition plate into two parts, the first through hole is located on the left side of the partition plate, and the feed opening and the second through hole are located on the right side of the partition plate.
Preferably, the middle part of the rotating shaft is provided with a box body, the middle part of the box body is provided with a third through hole, the belt pulley is provided with a wheel shaft, and the wheel belt pulley is rotatably arranged in the third through hole through the wheel shaft; the aperture of the first through hole is larger than that of the second through hole; the front end of the box body is provided with a first accommodating cavity, and the left inner side wall of the first accommodating cavity is provided with a plurality of first vent holes; the wheel shaft penetrates through the inner side wall of the third through hole and extends into the first accommodating cavity; an impeller is arranged in the first accommodating cavity and is arranged on a wheel shaft; a channel is arranged in the rotating shaft, a plurality of fourth through holes communicated with the channel are formed in the outer side wall of the top end of the rotating shaft, and the fourth through holes are positioned above the cup cover; the channel is positioned above the box body; the breather pipe is arranged between the channel and the first accommodating cavity, and the air flow in the cup body flows into the first accommodating cavity through the first vent hole to drive the impeller to rotate and then flows out of the cup body through the breather pipe, the channel and the fourth vent hole in sequence.
Preferably, a second accommodating cavity is formed in the rear end of the box body, and a second motor is installed in the second accommodating cavity; the wheel shaft penetrates through the inner side wall of the third through hole to extend into the second accommodating cavity, and an output shaft of the second motor is detachably connected with the wheel shaft; a first groove is formed in the end part of an output shaft of the second motor, and a rectangular electromagnet matched with the first groove in shape is arranged in the first groove; a second groove is formed in one end, close to the output shaft of the second motor, of the wheel shaft, the shape of the second groove is matched with that of the rectangular electromagnet, and an iron block adsorbed with the rectangular electromagnet is arranged in the second groove; a second spring is fixedly connected between one side wall of the rectangular electromagnet far away from the iron block and the inner side wall of the first groove.
Preferably, the inner surface of the separating disc is a concave surface which is bent towards the center of the separating disc, and the material on the inner surface of the separating disc can slide down to the feed opening along the concave surface.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) according to the method, the treated material is firstly crushed, then the rare earth element and the iron group element are converted into the oxide, the iron group element is reduced into the iron group element through the reducing gas, and then the iron group element and the rare earth oxide are effectively separated through a physical method.
(2) When the cooling device cools the iron group element and the rare earth oxide, the iron group element and the rare earth oxide can be effectively separated, the oxide is still in the inner cavity of the cooling device, and the iron group element is collected in the collecting bag.
(3) The reducing gas in the method for recovering the rare earth element is NH3Or CO, NH3The method has the advantages that the method reacts with the iron group element oxide to generate nitrogen, water and the iron group element, CO reacts with the iron group element oxide to generate carbon dioxide and the iron group element, the nitrogen and the carbon dioxide are harmless gases, and the method for recycling the rare earth element is green, environment-friendly and pollution-free.
(4) According to the invention, liquid nitrogen is added into the cooling device, when the liquid nitrogen cools the material in the cooling device, the liquid nitrogen is gasified into steam, the steam in the cup body flows into the first accommodating cavity through the first vent hole to drive the impeller to rotate, and then flows out of the cup body through the vent pipe, the channel and the fourth vent hole in sequence, the impeller rotates to drive the belt pulley to rotate, the belt pulley drives the annular magnetic strip to rotate clockwise, and the gasified liquid nitrogen is effectively utilized.
(5) According to the invention, through the arrangement of the supporting stirring rod, the supporting stirring rod is used for stirring materials in the cooling device on one hand, and the annular magnetic strip is spread on the other hand, so that the annular magnetic strip can conveniently rotate, and the annular magnetic strip can adsorb more iron group elements by rotating for one circle.
(6) According to the invention, through the arrangement of the guide isolation U-shaped plate, the guide isolation U-shaped plate prevents the iron group elements from falling out of the collecting bag through the second through holes after the scraper scrapes the iron group elements from the annular magnetic strip.
(7) According to the invention, through the arrangement of the bag bundling ring and the first spring, the bag bundling ring can elastically adjust the containing space of the collecting bag under the driving of the first spring, when more and more iron group element particles fall into the collecting bag, the iron group elements located in the collecting bag push the bag bundling ring downwards, and the bag bundling ring downwards extrudes the first spring, so that the containing space of the collecting bag is enlarged.
(8) According to the invention, through the arrangement of the rectangular electromagnet, the iron block, the second groove, the first groove and the second spring, when the impeller is not driven to rotate by large airflow, the rectangular electromagnet is started, one end of the rectangular electromagnet, which is far away from the second spring, gradually moves from the first groove to the iron block in the second groove for adsorption, so that the connection between the output shaft of the second motor and the wheel shaft is realized, the second motor rotates to drive the belt pulley to rotate clockwise, and the belt pulley drives the annular magnetic strip to rotate, so that the effective separation of iron group elements and rare earth oxides is realized.
Drawings
FIG. 1 is a schematic view of the non-use configuration of the collection bag of the present invention;
FIG. 2 is a schematic cross-sectional view of a collection bag of the present invention in use;
FIG. 3 is a schematic diagram of the structure at A in FIG. 2 according to the present invention;
FIG. 4 is a schematic view of the structure of the separating disk, collecting bag, box body, rotating shaft, annular magnetic strip and separating plate of the present invention;
FIG. 5 is a schematic view of the left side structure of the separating disk, collecting bag, box, rotating shaft, annular magnetic strip and separating plate of the present invention;
FIG. 6 is a right side schematic view of the divider disk, collection bag, cartridge, rotating shaft, annular magnetic strip and divider plate of the present invention;
FIG. 7 is a schematic diagram of the structure of FIG. 6 at C in accordance with the present invention;
FIG. 8 is a schematic structural view of the divider disk, collection bag, bag restraining ring, first through hole and second through hole of the present invention;
FIG. 9 is a schematic structural view of a case, a rotation shaft and a fourth through hole according to the present invention;
FIG. 10 is a schematic diagram of the structure of FIG. 9 at B in accordance with the present invention;
fig. 11 is a schematic structural view of the support stirring rod of the present invention.
The reference numbers in the figures illustrate:
1 cup body, 2 cup covers,
3 stirring and separating device, 301 rotating shaft, 302 belt pulley, 3021 wheel shaft, 3022 second groove, 303 separating disc, 304 bag ring, 305 first spring, 306 supporting stirring rod, 307 annular magnetic strip, 308 collecting bag, 309 first through hole, 310 second through hole, 311 scraping plate, 312 annular boss, 313 minute discharge hole, 314 separating plate,
4 a first motor,
5 box body, 501 third through hole, 502 first containing cavity, 5021 first vent hole, 5023 impeller and 503 second containing cavity
6 channels, 601 a fourth through hole,
7 a vent pipe,
8 second motors, 801 first grooves, 9 rectangular electromagnets, 10 iron blocks, 11 second springs and 12 guide isolation U-shaped plates.
Detailed Description
A method for recovering rare earth oxide by using rare earth magnetic material waste comprises the following steps:
step (1): crushing a treatment material at least containing rare earth elements and iron group elements, and then carrying out oxidation treatment to obtain oxides;
step (2): putting the oxide into a heating device, heating to 360 ℃, filling reducing gas into the heating device, and reducing O in the heating device2Content (c);
and (3): heating the heating device, and fully reducing the reducing gas and the oxide of the iron group element at the temperature of 360-1300 ℃, wherein the oxide of the iron group element is reduced into the iron group element by the reducing gas;
and (4): pouring the material reacted in the step (3) into a cooling device, adding liquid nitrogen into the cooling device, cooling the material reacted in the step (3) by using the liquid nitrogen, and cooling to the temperature below 100 ℃; and (4) separating the materials after the reaction in the step (3) to obtain rare earth oxide and iron group element alloy.
The reducing gas being NH3Or CO.
The granularity of the treated material crushed in the step (1) is less than 0.85 mm.
The particle size of the treatment material is preferably a granular or powdery material having a particle size of 500 μm or less (if the ease of preparation is taken into consideration, the lower limit of the particle size is preferably 1 μm).
The mass content of non-rare earth elements in the treated material is higher than 5 percent.
The treatment material to which the method of the present invention is applied is a treatment material containing at least a rare earth element and an iron group element, and is not particularly limited as long as it contains a rare earth element such as Nd, Pr, Dy, Tb, Sm and an iron group element such as Fe, Co, Ni and the like, and may contain, for example, boron and the like as other elements besides the rare earth element and the iron group element. Specifically, for example, R-Fe-B permanent magnets, heavy rare earth element diffusion sources (including DyFe) for diffusing heavy rare earth elements in R-Fe-B permanent magnets, and alloys of heavy rare earth elements and iron2、DyFe3、TbFe2、TbFe3Such as alloy pieces), and also contains a treatment material of a component (light rare earth element, boron, and the like) derived from the magnet by use.
When the treatment material is an R-Fe-B permanent magnet or an R-Co-Fe permanent magnet, the treatment material may be magnet scraps, magnet machining scraps, or the like discharged in the production process. In order to sufficiently oxidize the object to be treated, the object to be treated is preferably in the form of particles or powder having a particle diameter of 500 μm or less (for example, if the ease of preparation is considered, the lower limit of the particle diameter is preferably 1 μm).
The treated material at least containing rare earth elements and iron group elements is the material which has been degreased.
The processing material at least containing rare earth elements and iron group elements is one or two of R-Co-Fe permanent magnetic materials and R-Fe-B permanent magnetic materials.
Example 1 for recovery of rare earth oxide:
the method comprises the steps of crushing an R-Fe-B permanent magnet material into R-Fe-B fine powder, then carrying out combustion treatment on the R-Fe-B fine powder by using a rotary kiln, carrying out heat preservation reaction for 120 minutes at 800 ℃, and oxidizing rare earth elements and iron group elements in the R-Fe-B fine powder into oxides, wherein the mass of the rare earth oxides accounts for 40.3%.
Putting 12g of oxide into an experimental atmosphere protection rotary kiln, heating to 360 ℃, and starting to charge NH into the atmosphere protection rotary kiln3When atmosphere protects O in the rotary kiln2After the content is less than 16 percent, the temperature is continuously increased to 850 ℃, and the reaction is carried out at 850 ℃ 6After 0 minute, stopping charging NH3 until the iron group element oxide is completely reduced; and pouring the reacted materials into a cooling device, adding liquid nitrogen into the cooling device, cooling the reacted materials by the liquid nitrogen, and separating the rare earth oxide from the iron group element alloy particles. 4.8g of metal and 4.82g of oxide were separated. The yield of rare earth elements is 98.2%.
Example 2 for recovery of rare earth oxide
The irregular lump material of the R-Fe-B permanent magnet material is firstly crushed into a material with the thickness less than 0.85mm by a high-speed crusher, then the material is combusted by a rotary kiln, the temperature is kept at 800 ℃ for reaction for 120 minutes, the material is oxidized into oxide, wherein the mass of the oxide of iron accounts for 74.36%.
100kg of oxide is put into an atmosphere protection rotary kiln, after the temperature is raised to 360 ℃, NH begins to be filled3When atmosphere protects O in the rotary kiln2After the content is lower than 16 percent, the temperature is continuously increased to 850 ℃, the reaction is carried out for 80 minutes at 850 ℃, and NH charging is stopped after the iron group element oxide is completely reduced3。NH3The filling amount is 382L/min. And pouring the treated material into a cooling device, filling liquid nitrogen to cool the treated material, and separating rare earth oxide from iron group element alloy particles. 52kg of metal and 36.2kg of oxide were obtained. The yield of rare earth elements is 98.5%.
Example 3 for recovery of rare earth oxide
Crushing the R-Fe-B grinding powder into fine powder, then carrying out combustion treatment by using a rotary kiln, carrying out heat preservation reaction at 850 ℃ for 120 minutes, and oxidizing the material into oxide, wherein the mass of the oxide of the iron is 73.28%.
100kg of oxide is put into an atmosphere protection rotary kiln, the temperature is raised to 360 ℃, and NH begins to be filled3When atmosphere protects O in the rotary kiln2After the content is lower than 16 percent, the temperature is continuously increased to 1300 ℃, the reaction is carried out for 30 minutes at 1300 ℃, and NH charging is stopped after the iron group element oxide is completely reduced3；NH3The charging rate is 390L/min; and pouring the treated material into a cooling device, filling liquid nitrogen to cool the treated material, and separating rare earth oxide from iron group element alloy particles. After separation, obtain50.3kg of metal, 36.5kg of oxide and 98.5% of rare earth element yield.
The iron group elements refer to partial elements in the 4 th period of the periodic table, comprise Fe, Co and Ni 3 elements, and belong to transition group elements.
The cooling device comprises a cup body 1 with a cavity, a cup cover 2 and a stirring and separating device 3; the cup cover 2 covers the opening at the top end of the cup body 1; the top end of the cup cover 2 is provided with a first motor 4; the stirring and separating device 3 is arranged in the cup body 1; the stirring and separating device 3 comprises a rotating shaft 301, an upper belt pulley 302 rotatably connected to the rotating shaft 301, a separating disc 303 fixedly arranged on the rotating shaft 301 and positioned below the belt pulley 302, a supporting stirring rod 306 and an annular magnetic strip 307; the top end of the rotating shaft 301 penetrates through the cup cover 2 to be connected with the output end of the first motor 4, and the bottom end of the rotating shaft penetrates through the middle part of the separating disc 303 to be fixedly connected with the supporting stirring rod 306; a plurality of feed openings 313 are formed in the separating disc 303, a material collecting device is arranged between the separating disc 303 and the supporting stirring rod 306, and materials fall into the material collecting device from the feed openings 313; the left side and the right side of the top end of the separating disc 303 are respectively provided with a first through hole 309 and a second through hole 310; the annular magnetic strip 307 passes through the first through hole 309 and the second through hole 310 and is wound between the belt pulley 302 and the support stirring rod 306, and the belt pulley 302 drives the annular magnetic strip 307 to rotate clockwise; the second through hole 310 matches the shape of the annular magnetic strip 307; a scraper 311 is arranged on the separating disc 303 and is tightly attached to the outer surface of the annular magnetic strip 307 passing through the second through hole 310; the outer surface of the annular magnetic strip 307 is magnetic and the inner surface is nonmagnetic.
The material collection device comprises a collection bag 308, a first spring 305, a boss 312, a bag restraining ring 304, and a first spring 305; the boss 312 is fixedly arranged at the joint of the support stirring rod 306 and the rotating shaft 301; the collecting bag 308 is sleeved outside the rotating shaft 301, the top end of the collecting bag 308 is connected to the bottom end of the separating disc 303, the collecting bag 308 is connected to the boss 312, and the discharging opening 313 is positioned right above the inner cavity of the collecting bag 308; the first spring 305 and the bag restraining ring 304 are sleeved outside the collection bag 308; the first spring 305 is fixedly connected between the bag-restraining ring 304 and the boss 312, and the bag-restraining ring 304 is driven by the first spring 305 to dynamically adjust the accommodating space of the collecting bag 308.
The partition plate 314 is arranged on the partition plate 303; the partition plate 314 divides the partition plate 303 into two, the first through hole 309 is located on the left side of the partition plate 314, and the feed opening 313 and the second through hole 310 are located on the right side of the partition plate 314.
A box body 5 is arranged in the middle of the rotating shaft 301, a third through hole 501 is formed in the middle of the box body 5, a wheel shaft 3021 is arranged on the belt pulley 302, and the belt pulley 302 is rotatably installed in the third through hole 501 through the wheel shaft 3021; the first through hole 309 has a larger aperture than the second through hole 310; a first accommodating cavity 502 is formed in the front end of the box body 5, and a plurality of first vent holes 5021 are formed in the left inner side wall of the first accommodating cavity 502; the axle 3021 extends into the first accommodating cavity 502 through the inner side wall of the third through hole 501; an impeller 5023 is arranged in the first accommodating cavity 502, and the impeller 5023 is mounted on a wheel shaft 3021; a channel 6 is arranged in the rotating shaft 301, a plurality of fourth through holes 601 communicated with the channel 6 are formed in the outer side wall of the top end of the rotating shaft 301, and the fourth through holes 601 are located above the cup cover 2; the channel 6 is positioned above the box body 5; a vent pipe 7 is arranged between the channel 6 and the first accommodating cavity 502, and the air flow in the cup body 1 flows into the first accommodating cavity 502 through the first vent hole 5021 to drive the impeller 5023 to rotate, and then flows out of the cup body 1 through the vent pipe 7, the channel 6 and the fourth through hole 601 in sequence.
A second accommodating cavity 503 is formed in the rear end of the box body 5, and a second motor 8 is installed in the second accommodating cavity 503; the axle 3021 extends into the second accommodating cavity 503 through the inner side wall of the third through hole 501, and the output shaft of the second motor 8 is detachably connected with the axle 3021; a first groove 801 is formed in the end portion of an output shaft of the second motor 8, and a rectangular electromagnet 9 matched with the first groove 801 in shape is arranged in the first groove 801; a second groove 3022 is formed in one end, close to the output shaft of the second motor 8, of the wheel shaft 3021, the shape of the second groove 3022 is matched with that of the rectangular electromagnet 9, and an iron block 10 adsorbed with the rectangular electromagnet 9 is arranged in the second groove 3022; a second spring 11 is fixedly connected between one side wall of the rectangular electromagnet 9 far away from the iron block 10 and the inner side wall of the first groove 801.
A guiding isolation U-shaped plate 12 matched with the annular magnetic strip 307 in shape is arranged at the second through hole 310; the inner wall of the annular magnetic strip 307 is tightly attached to the inner wall of the isolation U-shaped plate 10.
The inner surface of the separating disc 303 is a concave surface which is bent towards the center of the separating disc 303, and materials on the inner surface of the separating disc 303 can slide down to the blanking port 313 along the concave surface.
The cup cover 2 is a sealing cover.
The support agitator bars 306 comprise a plurality of agitator bars and a plurality of support bars; two adjacent stirring rods are connected with each other, and the supporting rod is fixedly connected between the two adjacent stirring rods; one end of the stirring rod, which is far away from the stirring rod connected with the stirring rod, is provided with a rotating wheel, and the rotating wheel can reduce the friction between the belt pulley 302 and the end part of the stirring rod; the bracing piece plays the effect of supporting two adjacent puddlers on the one hand, and on the other hand, when axis of rotation 301 rotated, the bracing piece was driven and is rotated, and the bracing piece can play the effect of stirring.
The pulley 302 rotates in two ways:
firstly, when the liquid nitrogen cools the material in the cooling device, the liquid nitrogen is gasified into steam due to the high temperature of the cooled material, the steam in the cup body 1 flows into the first accommodating cavity 502 through the first vent hole 5021 to drive the impeller 5023 to rotate, and then flows out of the cup body 1 through the vent pipe 7, the channel 6 and the fourth through hole 601 in sequence; the rotation of the impeller 5023 drives the pulley 302 to rotate clockwise, and the pulley 302 drives the annular magnetic strip 307 to rotate clockwise.
Secondly, when the impeller 5023 does not have large airflow to drive the impeller 5023 to rotate, the rectangular electromagnet 9 is started, one end, far away from the second spring 11, of the rectangular electromagnet 9 gradually moves from the first groove 801 to the second groove 3022 to be adsorbed by the iron block 10, the connection between the output shaft of the second motor 8 and the wheel shaft 3021 is achieved, the second motor 8 rotates to drive the belt pulley 302 to rotate clockwise, and the belt pulley 302 drives the annular magnetic strip 307 to rotate clockwise.
The using step of the cooling device comprises the following steps:
pouring the reacted materials into the cup body 1, and then pouring liquid nitrogen into a cooling device; start first motor 4, first motor 4 drives puddler 306 and rotates, puddler 306 stirs the material in to cup 1, make cup 1's material fully contact with the liquid nitrogen, realize rapid cooling, pivoted belt pulley 302 drives annular magnetic stripe 307 clockwise rotation, adsorb at annular magnetic stripe 307 surface with the adsorbed material of magnet mutually, scraper blade 311 will be with the adsorbed material of magnet mutually scrape off from annular magnetic stripe 307 surface, the material that is scraped off falls into to collecting bag 308 in through feed opening 313, along with the increase of material in collecting bag 308, the material promotes to restraint bag ring 304 downstream, restraint bag ring 304 extrusion spring 305, the space grow that collecting bag 308 above restraint bag ring 304 held the material. The material not collected in the collection bag 308 is rare earth oxide.
Claims (10)
1. A method for recovering rare earth oxide by using rare earth magnetic material waste is characterized by comprising the following steps: the method comprises the following steps:
step (1): crushing a treatment material at least containing rare earth elements and iron group elements, and then carrying out oxidation treatment to obtain oxides;
step (2): putting the oxide into a heating device, heating to 360 ℃, filling reducing gas into the heating device, and reducing O in the heating device2Content (c);
and (3): heating the heating device, and fully reducing the reducing gas and the oxide of the iron group element at the temperature of 360-1300 ℃, wherein the oxide of the iron group element is reduced into the iron group element by the reducing gas;
and (4): pouring the material reacted in the step (3) into a cooling device, adding liquid nitrogen into the cooling device, cooling the material reacted in the step (3) by the liquid nitrogen, and cooling to the temperature below 100 ℃; and (4) separating the materials after the reaction in the step (3) to obtain rare earth oxide and iron group element alloy.
2. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 1, wherein: the reducing gas being NH3Or CO.
3. The method for recovering rare earth oxide from rare earth magnetic material waste according to claim 1, wherein: the granularity of the treated material crushed in the step (1) is less than 0.85 mm.
4. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 1, wherein: the treated material at least containing rare earth elements and iron group elements is the material which has been degreased.
5. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 1, wherein: the cooling device comprises a cup body (1) with a cavity, a cup cover (2) and a stirring and separating device (3);
the cup cover (2) covers the opening at the top end of the cup body (1); a first motor (4) is arranged at the top end of the cup cover (2); the stirring and separating device (3) is arranged in the cup body (1);
the stirring and separating device (3) comprises a rotating shaft (301), an upper belt pulley (302) rotatably connected to the rotating shaft (301), a separating disc (303) fixedly arranged on the rotating shaft (301) and positioned below the belt pulley (302), a supporting stirring rod (306) and an annular magnetic strip (307);
the top end of the rotating shaft (301) penetrates through the cup cover (2) to be connected with the output end of the first motor (4), and the bottom end of the rotating shaft penetrates through the middle part of the separating disc (303) to be fixedly connected with the supporting stirring rod (306);
a plurality of feed openings (313) are formed in the separating disc (303), a material collecting device is arranged between the separating disc (303) and the supporting stirring rod (306), and materials fall into the material collecting device from the feed openings (313);
the left side and the right side of the top end of the separating disc (303) are respectively provided with a first through hole (309) and a second through hole (310);
the annular magnetic strip (307) passes through the first through hole (309) and the second through hole (310) and is wound between the belt pulley (302) and the supporting stirring rod (306), and the belt pulley (302) drives the annular magnetic strip (307) to rotate clockwise;
the second through hole (310) is matched with the shape of the annular magnetic strip (307); the scraper (311) is arranged on the separating disc (303) and is tightly attached to the outer surface of the annular magnetic strip (307) passing through the second through hole (310); the outer surface of the annular magnetic strip (307) is magnetic, and the inner surface is nonmagnetic.
6. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 5, wherein: the material collecting device comprises a collecting bag (308), a first spring (305), a boss (312), a bag binding ring (304) and a first spring (305);
the boss (312) is fixedly arranged at the joint of the support stirring rod (306) and the rotating shaft (301);
the collecting bag (308) is sleeved outside the rotating shaft (301), the top end of the collecting bag (308) is connected to the bottom end of the separating disc (303), the collecting bag (308) is connected to the boss (312), and the discharge port (313) is positioned right above the inner cavity of the collecting bag (308);
the first spring (305) and the bag-binding ring (304) are sleeved outside the collecting bag (308); the first spring (305) is fixedly connected between the bag restraining ring (304) and the boss (312).
7. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 5, wherein: a separation plate (314) is arranged on the separation disc (303); the separating plate (314) divides the separating disc (303) into two parts, the first through hole (309) is positioned at the left side of the separating plate (314), and the feed opening (313) and the second through hole (310) are both positioned at the right side of the separating plate (314).
8. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 5, wherein: a box body (5) is arranged in the middle of the rotating shaft (301), a third through hole (501) is formed in the middle of the box body (5), a wheel shaft (3021) is arranged on the belt pulley (302), and the wheel belt pulley (302) is rotatably installed in the third through hole (501) through the wheel shaft (3021);
the aperture of the first through hole (309) is larger than that of the second through hole (310);
a first accommodating cavity (502) is formed in the front end of the box body (5), and a plurality of first vent holes (5021) are formed in the left inner side wall of the first accommodating cavity (502);
the wheel shaft (3021) penetrates through the inner side wall of the third through hole (501) and extends into the first accommodating cavity (502);
an impeller (5023) is arranged in the first accommodating cavity (502), and the impeller (5023) is mounted on a wheel shaft (3021);
a channel (6) is arranged in the rotating shaft (301), a plurality of fourth through holes (601) communicated with the channel (6) are formed in the outer side wall of the top end of the rotating shaft (301), and the fourth through holes (601) are positioned above the cup cover (2);
the channel (6) is positioned above the box body (5);
a vent pipe (7) is arranged between the channel (6) and the first accommodating cavity (502), and air flow in the cup body (1) flows into the first accommodating cavity (502) through the first vent hole (5021) to drive the impeller (5023) to rotate and then flows out of the cup body (1) through the vent pipe (7), the channel (6) and the fourth through hole (601) in sequence.
9. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 8, wherein: a second accommodating cavity (503) is formed in the rear end of the box body (5), and a second motor (8) is installed in the second accommodating cavity (503);
the wheel shaft (3021) penetrates through the inner side wall of the third through hole (501) and extends into the second accommodating cavity (503), and the output shaft of the second motor (8) is detachably connected with the wheel shaft (3021);
a first groove (801) is formed in the end portion of an output shaft of the second motor (8), and a rectangular electromagnet (9) matched with the first groove in shape is arranged in the first groove (801);
a second groove (3022) is formed in one end, close to the output shaft of the second motor (8), of the wheel shaft (3021), the second groove (3022) is matched with the rectangular electromagnet (9) in shape, and an iron block (10) adsorbed to the rectangular electromagnet (9) is arranged in the second groove (3022);
a second spring (11) is fixedly connected between one side wall of the rectangular electromagnet (9) far away from the iron block (10) and the inner side wall of the first groove (801).
10. The method for recovering rare earth oxide from waste material of rare earth magnetic material as claimed in claim 5, wherein: the inner surface of the separating disc (303) is a concave surface which is bent towards the center of the separating disc (303), and materials on the inner surface of the separating disc (303) can slide down to the blanking port (313) along the concave surface.
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