CN115232971A - Method for recycling rare earth from neodymium iron boron chamfer mud - Google Patents
Method for recycling rare earth from neodymium iron boron chamfer mud Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 122
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 40
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 34
- 238000004064 recycling Methods 0.000 title abstract description 5
- 238000007885 magnetic separation Methods 0.000 claims abstract description 132
- 229910001021 Ferroalloy Inorganic materials 0.000 claims abstract description 30
- 239000002699 waste material Substances 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 239000002893 slag Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims description 65
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 37
- 230000005291 magnetic effect Effects 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 15
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 24
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000004744 fabric Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 238000004537 pulping Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 230000008719 thickening Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000006246 high-intensity magnetic separator Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000006148 magnetic separator Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 rare earth hydroxide Chemical class 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical group [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for recovering rare earth from neodymium iron boron chamfer mud, and belongs to the technical field of rare earth resource recovery. According to the invention, a mechanical purification processing technology (sequentially carrying out size mixing, slag separation, low-intensity magnetic separation and high-intensity magnetic separation on the waste) is adopted, the rare earth ferroalloy in the neodymium iron boron chamfer mud can be recovered on a large scale without smelting the waste, the process flow is simple, the production scale is large, the power consumption is low, the enrichment efficiency of the rare earth ferroalloy is high, the efficient and green recycling of the rare earth ferroalloy in the neodymium iron boron chamfer mud is realized, and the recovery cost of rare earth resources is greatly reduced. Compared with the traditional chemical sorting enrichment method, the method provided by the invention has the advantages that the recycled rare earth ferroalloy has few carbon, silicon and other non-rare earth impurities, the rare earth oxide recovery rate is high, the product performance is stable, the hydrochloric acid consumption in the later rare earth elemental substance preparation process of the rare earth ferroalloy by preferential dissolution can be greatly reduced, the rare earth recovery cost is reduced, the method is green and pollution-free, and the economic benefit is good.
Description
Technical Field
The invention relates to the technical field of rare earth resource recovery, in particular to a method for recovering rare earth from neodymium iron boron chamfer mud.
Background
Neodymium iron boron is used as a third-generation rare earth permanent magnet, wherein the content of rare earth elements is about 30 percent, neodymium accounts for about 90 percent, and the balance is praseodymium, dysprosium, gadolinium and the like, has the characteristics of excellent storage property, light weight, small volume and the like, and is widely applied in the fields of national defense and military industry, aerospace, medical appliances, electronics, computers, new energy automobile industry and the like.
The neodymium iron boron waste materials comprise invalid neodymium iron boron magnets and oil sludge, leftover materials and the like generated in the production and processing processes of neodymium iron boron. At present, the method for recycling the neodymium iron boron waste mainly comprises the following steps: hydrometallurgical methods (using roasting oxidation-hydrochloric acid dissolution-decomposition impurity removal-extraction separation-precipitation roasting), fluoride precipitation, sulfuric acid-double salt precipitation, total dissolution using hydrochloric acid as solvent, oxidation roasting-hydrochloric acid dissolution, etc. However, the neodymium iron boron chamfer mud contains more impurity elements such as carbon, silicon, aluminum and the like, the content of the rare earth is relatively low (the total content of the rare earth elements is 2-4 wt%), and the recovery method for recovering the rare earth has the problems of low rare earth recovery rate, difficulty in solid-liquid two-phase filtration and separation and high production cost.
The magnetic separation has the characteristics of low acid consumption (even no acid is added), and simple operation, and is more and more widely applied to the recovery of rare earth in neodymium iron boron waste. For example, chinese patent CN108866357A discloses a method for recovering rare earth from low-grade NFB waste, which comprises vacuum induction melting of neodymium iron boron material, hydrolysis of mother alloy, and magnetic separation of rare earth hydroxide and iron-based alloy powder, wherein the recovery rate of rare earth elements can reach 99.9%. However, the magnetic separation method requires vacuum induction melting of the waste materials, and has high energy consumption and high recovery cost.
Disclosure of Invention
In view of this, the invention aims to provide a method for recovering rare earth from neodymium iron boron chamfer mud, and the method provided by the invention does not need vacuum induction melting, and is low in energy consumption and recovery cost.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recovering rare earth from neodymium iron boron chamfer mud, which comprises the following steps:
pulping the neodymium iron boron chamfer mud by using water to obtain waste pulp;
carrying out slag separation treatment on the waste slurry to obtain slag-removed slurry;
performing low-intensity magnetic separation on the slag-removed slurry to obtain low-intensity magnetic separation rare earth iron alloy and low-intensity magnetic separation tailing slurry; the magnetic field intensity of the low-intensity magnetic separation is 2000-3000 Gs;
carrying out strong magnetic separation on the low-intensity magnetic separation tailing slurry to obtain rare-earth iron alloy with strong magnetic separation; the magnetic field intensity of the strong magnetic separation is 10000-15 kGs.
Preferably, the solid content of the neodymium iron boron waste slurry is 50-70 wt%.
Preferably, the slag separation treatment is carried out by using a slag separation sieve, and the aperture of the slag separation sieve is 2-5 mm.
Preferably, the method further comprises the following steps of: and adding water into the deslagging slurry for dilution.
Preferably, the solid content of the diluted slurry obtained by dilution is 20-30 wt%
Preferably, the strong magnetic separation is pulse strong magnetic separation, the pulse stroke of the pulse strong magnetic separation is 6-12 mm, and the frequency of impact is 120-220 r/min.
Preferably, the equipment adopted by the strong magnetic separation is a vertical ring pulsating high-gradient strong magnetic machine.
Preferably, the magnetic separation device further comprises: and concentrating and dehydrating the wet low-intensity magnetic separation rare earth iron alloy obtained by low-intensity magnetic separation to obtain the low-intensity magnetic separation rare earth iron alloy.
Preferably, after the strong magnetic separation, the method further comprises the following steps: and concentrating and dehydrating the wet-strength magnetic separation rare earth iron alloy obtained by the strong magnetic separation to obtain the strong magnetic separation rare earth iron alloy.
The invention provides a method for recovering rare earth from neodymium iron boron chamfer mud, which comprises the following steps: slurrying the neodymium iron boron chamfer angle with water to obtain waste slurry; carrying out slag separation treatment on the waste slurry to obtain slag-removed slurry; carrying out low-intensity magnetic separation on the slag-removed slurry to obtain a low-intensity magnetic separation rare earth iron alloy and a low-intensity magnetic separation tailing slurry; the magnetic field intensity of the low-intensity magnetic separation is 2000-3000 Gs; carrying out strong magnetic separation on the low-intensity magnetic separation tailing slurry to obtain a rare-earth iron alloy with strong magnetic separation; the magnetic field intensity of the strong magnetic separation is 10000-15 kGs. According to the invention, a mechanical purification processing technology (sequentially carrying out size mixing, slag separation, low-intensity magnetic separation and high-intensity magnetic separation on the waste) is adopted, the rare earth ferroalloy in the neodymium iron boron chamfer mud can be recovered on a large scale without smelting the waste, the process flow is simple, the production scale is large, the power consumption is low, the enrichment efficiency of the rare earth ferroalloy is high, the efficient and green recycling of the rare earth ferroalloy in the neodymium iron boron chamfer mud is realized, and the recovery cost of rare earth resources is greatly reduced. Compared with the traditional chemical sorting enrichment method, the method provided by the invention has the advantages that the recycled rare earth ferroalloy has few non-rare earth impurities such as carbon, silicon, aluminum and the like without magnetism, the recovery rate of rare earth oxide is high, the consumption of hydrochloric acid in the later rare earth ferroalloy preferential dissolution rare earth simple substance preparation process can be greatly reduced, the rare earth recovery cost is reduced, the method is green and pollution-free, and the economic benefit is good. As shown in the test results of the embodiment, after the treatment by the method provided by the invention, the rare earth yield is over 95 percent, the total amount of residual rare earth oxides in the tailings is below 0.2 percent, and the rare earth recovery rate is high.
Detailed Description
The invention provides a method for recovering rare earth from neodymium iron boron chamfer mud, which comprises the following steps:
pulping the neodymium iron boron chamfer mud by using water to obtain waste slurry;
carrying out slag separation treatment on the waste slurry to obtain slag-removed slurry;
carrying out low-intensity magnetic separation on the slag-removed slurry to obtain a low-intensity magnetic separation rare earth iron alloy and a low-intensity magnetic separation tailing slurry; the magnetic field intensity of the low-intensity magnetic separation is 2000-3000 Gs;
carrying out strong magnetic separation on the low-intensity magnetic separation tailing slurry to obtain a rare-earth iron alloy with strong magnetic separation; the magnetic field intensity of the strong magnetic separation is 10000-15 kGs.
In the present invention, unless otherwise specified, all the raw material components are commercially available products well known to those skilled in the art.
The method utilizes water to carry out pulping on the neodymium iron boron chamfer mud to obtain the waste slurry. In the invention, the total content of rare earth oxides in the neodymium iron boron chamfer mud is preferably 2-4 wt%, more preferably 2.5-3.5 wt%, and further preferably 3wt%. In the present invention, the slurrying is preferably carried out under stirring conditions; the stirring speed and time are not particularly limited in the invention, and the stirring is carried out until no agglomeration or precipitation occurs. In the invention, the solid content of the waste neodymium iron boron slurry is preferably 50 to 70wt%, more preferably 55 to 65wt%, and even more preferably 60 to 65wt%. In the invention, the purpose of the slurry is to separate the doped and wrapped rare earth ferroalloy from non-rare earth impurities such as silicon-aluminum-carbon and the like, thereby laying a foundation for subsequent magnetic separation.
After the waste slurry is obtained, the invention carries out slag separation treatment on the waste slurry to obtain slag-removed slurry. In the invention, the slag separation treatment is carried out by using a slag separation sieve, and the aperture of the slag separation sieve is preferably 2-5 mm, and more preferably 3-4 mm; the slag separating screen is preferably a cylindrical slag separating screen. In the invention, the purpose of the slag separation treatment is to remove substances such as plastics, wood chips and other non-rare earth wastes in the waste slurry.
After obtaining the slag-removing slurry, carrying out low-intensity magnetic separation on the slag-removing slurry to obtain a low-intensity magnetic separation rare earth iron alloy and a low-intensity magnetic separation tailing slurry. Before the low-intensity magnetic separation, water is preferably added into the slag-removed slurry for dilution, and the obtained diluted slurry is subjected to low-intensity magnetic separation. In the present invention, the solid content of the dilute slurry is preferably 20 to 30wt%, more preferably 25 to 30wt%. After the diluted slurry is obtained, the diluted slurry is subjected to low-intensity magnetic separation to obtain a low-intensity magnetic separation rare earth iron alloy and low-intensity magnetic separation tailing slurry. In the invention, the magnetic field intensity of the weak magnetic separation is 2000-3000 Gs, preferably 2300-3000 Gs, and more preferably 2500-3000 Gs. In the present invention, the low-intensity magnetic separation is preferably performed using a permanent magnet drum magnetic separator. In the present invention, the purpose of the low-intensity magnetic separation is to recover a ferromagnetic rare-earth iron alloy (i.e., a low-intensity magnetic separation rare-earth iron alloy).
In the present invention, after the low-intensity magnetic separation, the method preferably further comprises: and concentrating and dehydrating the wet low-intensity magnetic separation rare earth iron alloy obtained by low-intensity magnetic separation to obtain the low-intensity magnetic separation rare earth iron alloy. The concentration condition is not particularly limited, and the concentration is carried out until the solid content of the obtained concentrated solution is 45-65 wt%, and the solid content of the concentrated solution is more preferably 50-60 wt%; in the present invention, the concentration is preferably performed in a thickening tank. In the invention, the dehydration is preferably vacuum dehydration, and the vacuum dehydration is particularly preferably that the concentrated solution obtained by concentration is placed on a filter cloth under the condition of negative pressure, the rare earth ferroalloy solid phase is left on the filter cloth, and the separation of the solid phase and the liquid phase is realized by the infiltration of water through the filter cloth; the pressure of the negative pressure is preferably 0.04-0.08 MPa; the dewatering is preferably carried out in a vacuum dewatering screen; the water content of the dehydrated low-intensity magnetic separation rare earth iron alloy is preferably 8-13 wt%. In the invention, the total content of rare earth oxides in the low-intensity magnetic separation rare earth iron alloy is preferably 8-12 wt%.
After the low-intensity magnetic separation tailing slurry is obtained, the low-intensity magnetic separation tailing slurry is subjected to strong magnetic separation to obtain rare-earth iron alloy with strong magnetic separation. In the invention, the solid content of the low-intensity magnetic separation tailings slurry is preferably 20-25 wt%, more preferably 21-24 wt%, and even more preferably 22-23 wt%. In the invention, the magnetic field intensity of the strong magnetic separation is preferably 10000-15 kGs, preferably 12000-15 kGs; the magnetic medium is preferably a magnetic bar medium; the high-intensity magnetic separation is preferably pulse high-intensity magnetic separation, and the pulse stroke of the pulse high-intensity magnetic separation is preferably 6-12 mm, and more preferably 8-10 mm; the frequency of the pulse strong magnetic separation is preferably 120-220 r/min, and more preferably 150-200 r/min; the equipment adopted by the pulse strong magnetic separation is preferably a vertical ring pulse high-gradient strong magnetic machine. In the invention, the purpose of the pulse strong magnetic separation is to further recover the residual rare earth ferroalloy material in the tailings obtained by the weak magnetic separation. The invention adopts the vertical-ring pulsating high-gradient high-intensity magnetic separator for strong magnetic separation, the vertical-ring pulsating high-gradient high-intensity magnetic separator has the advantages that the background magnetic field intensity is high (the magnetic field intensity can be adjusted from 0 to 1.8 Tesla), the gradient is high, the pulse can repeatedly wash and screen nonmagnetic minerals in magnetic materials, impurities are removed to the greatest extent, and finally the purity of rare earth ferroalloy in the magnetic materials is greatly improved; the gap between the diameter of the magnetic medium and the magnetic medium can be matched according to the particle size of the material, so that the effect of recovering the magnetic material is effectively achieved, and the phenomenon of material inclusion is avoided. In a specific embodiment of the present invention, the magnetic medium used for the strong magnetic separation is preferably a rod medium, and the diameter of the rod medium is preferably 1.0 to 2.0mm, and more preferably 1.5 to 2.0mm.
In the present invention, it is preferable that the method further comprises, after the strong magnetic separation: and concentrating and dehydrating the wet-strength magnetic separation rare earth iron alloy obtained by the strong magnetic separation to obtain the strong magnetic separation rare earth iron alloy. The concentration condition is not particularly limited, and the concentration is carried out until the solid content of the obtained concentrated solution is 45-65 wt%, and the solid content of the concentrated solution is more effectively 50-60 wt%; in the present invention, the concentration is preferably performed in a thickening tank. In the invention, the dehydration is preferably vacuum dehydration, and the vacuum dehydration is particularly preferably that the concentrated solution obtained by concentration is placed on a filter cloth under the condition of negative pressure, the rare earth ferroalloy solid phase is left on the filter cloth, and the separation of the solid phase and the liquid phase is realized by the infiltration of water through the filter cloth; the pressure of the negative pressure is preferably 0.04-0.08 MPa; in a particular embodiment of the invention, the dewatering is preferably carried out in a vacuum dewatering screen; the water content of the dehydrated highly magnetic rare earth iron alloy is preferably 8 to 13wt%, and more preferably 10 to 12wt%.
In the present invention, the total content of rare earth oxides in the strongly magnetic rare earth iron alloy is preferably 6.0 to 8.0wt%. In the invention, the water obtained by settling the dehydrated water phase can be recycled, the recovery cost of the rare earth is greatly reduced, the method is green and pollution-free, the efficient and green recovery and utilization of the rare earth in the neodymium iron boron chamfer mud are realized, and the economic benefit is improved for related industries. Moreover, the method provided by the invention has the advantages of simple flow, large production scale, low power consumption, high recovery efficiency, good mineral separation environment and high economic benefit. And the whole production process belongs to physical ore dressing, no chemical substance is used, and the environmental protection pressure is reduced for enterprises of related departments.
In the present invention, the weakly magnetically sorted rare earth iron alloy and the strongly sorted rare earth iron alloy are preferably separated from the rare earth oxide by acid dissolution.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Adding 5kg of neodymium iron boron chamfering mud rare earth waste (total rare earth amount (TREO) is 2.66wt%, main rare earth elements are praseodymium oxide 23.95% and neodymium oxide 70.87%) and water into stirring equipment, and pulping under the stirring condition to obtain waste pulp with the solid content of 65wt%.
The composition of rare earth elements in the neodymium iron boron chamfering pug rare earth waste is shown in table 1.
TABLE 1 rare earth element composition (wt%) in neodymium iron boron chamfer mud rare earth waste
Note: the contents in table 1 are the contents of the corresponding rare earth oxides.
(2) And (3) placing the waste slurry into a cylindrical slag separation sieve (with the aperture of 2-5 mm) for slag separation treatment to obtain slag-removed slurry which is used as a magnetic separation feed stock.
(3) Diluting the slag-removing slurry to a solid content of 30wt% by using water, placing the obtained diluted slurry in a permanent magnet drum type magnetic separator, and carrying out low-intensity magnetic separation (mainly used for recovering strong magnetic rare earth ferroalloy) under the condition of 2300Gs to obtain wet low-intensity magnetic separation rare earth ferroalloy and low-intensity magnetic separation tailing slurry. Respectively sampling the wet low-intensity magnetic separation rare-earth ferroalloy and the low-intensity magnetic separation tailing slurry, concentrating the slurry in a thickening tank until the solid content is 50-60 wt%, dehydrating the slurry in a vacuum dehydration sieve (0.04-0.08 MPa) until the water content is 8-13 wt%, and then drying the slurry to respectively obtain the low-intensity magnetic separation rare-earth ferroalloy and the low-intensity magnetic separation tailing; respectively analyzing the total content of rare earth oxides and the rare earth partition condition in the low-intensity magnetic separation rare earth ferroalloy and the low-intensity magnetic separation tailings, and analyzing the results: 1055g of rare earth iron alloy subjected to low intensity magnetic separation, wherein the total content of rare earth oxides (TREO) is 10.66wt%, and the recovery rate of rare earth is 84.58%; 3945g of tailing slurry subjected to low-intensity magnetic separation, wherein the total content (TREO) of residual rare earth oxides is 0.52wt%.
(4) And (3) placing the tailings slurry subjected to low-intensity magnetic separation in a vertical-ring pulsating high-gradient strong magnetic machine, and performing a pulsating magnetic field under the conditions that the magnetic field intensity is 12000Gs, the magnetic medium is a 2.0mm rod medium, the pulsation stroke is 8mm, and the stroke frequency is 180r/min to obtain the rare earth iron alloy subjected to high-intensity magnetic separation and the tailings slurry subjected to pulsating magnetic field magnetic separation. Respectively sampling the strong magnetic separation rare earth ferroalloy and the tailing slurry subjected to magnetic separation by a pulsating magnetic field, concentrating the slurry in a thickening tank until the solid content is 50-60 wt%, dehydrating the slurry in a vacuum dehydration sieve (0.04-0.08 MPa) until the water content is 8-13 wt%, drying the slurry, and respectively analyzing the total content of rare earth oxides and the rare earth distribution condition in the obtained strong magnetic separation rare earth ferroalloy and the tailings subjected to magnetic separation by a rare earth analyzer, wherein the analysis result is as follows: 660.79g of strongly magnetic separation rare earth iron alloy, 2.21wt% of TREO and 10.98% of rare earth recovery rate; the strong magnetic separation tailings are 3284.21g, and the TREO is 0.18wt%.
(5) By combining the step (3) and the step (4), 1715.79g of the total amount of the recycled rare earth ferroalloy, 7.41wt% of TREO, 95.56% of the rare earth yield and 0.18wt% of the total content of the residual rare earth oxide in the discharged end tailings (namely the strong magnetic separation tailings) can be obtained.
Example 2
A recycled rare earth ferroalloy was prepared as in example 1, differing from example 1 only in that:
in the step (4), the magnetic field intensity is 15000Gs, the magnetic medium is a 1.5mm rod medium, the strongly magnetic separation rare earth iron alloy 775.59g, the TREO is 1.95wt%, and the rare earth recovery rate is 11.37%; 3169.41g of strong magnetic separation tailings, and 0.17wt% of TREO.
In the step (5), the total amount of the recycled rare earth ferroalloy is 1830.59g, TREO is 6.97wt%, the rare earth yield is 95.95%, and the residual TREO in the discharged final tailings is 0.17wt%.
Example 3
A recycled rare earth ferroalloy was prepared as in example 1, differing from example 1 only in that:
in the step (3), the magnetic field intensity is 3000Gs, the low-intensity magnetic separation rare earth iron alloy is 1138.50g, the TREO is 10.02wt%, and the rare earth recovery rate is 85.77%; 3861.5g of tailing slurry subjected to low-intensity magnetic separation, and the residual TREO is 0.49wt%.
In the step (4), 478.83g of strongly magnetic separation rare earth iron alloy, 2.61wt% of TREO and 9.39% of rare earth recovery rate are obtained; 3382.67g of tailings after the strong magnetic separation, and 0.19wt% of TREO.
In the step (5), the total amount of the recycled rare earth ferroalloy is 1617.33g, the TREO is 7.83wt%, the rare earth yield is 95.17%, and the residual TREO in the discharged final tailings is 0.19wt%.
Example 4
A recycled rare earth ferroalloy was prepared according to example 3, differing from example 3 only in that:
in the step (4), the magnetic field intensity is 15000Gs, the magnetic medium is a 1.5mm rod medium, the strongly magnetic separation rare earth iron alloy is 873.86g, the TREO is 1.55wt%, and the rare earth recovery rate is 10.18%; 2987.64g of strong magnetic separation tailings and 0.178wt% of TREO.
In the step (5), the total amount of the recycled rare earth iron alloy is 2012.36g, the TREO is 6.34wt%, the rare earth yield is 95.96%, and the residual TREO in the discharged final tailings is 0.18wt%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for recovering rare earth from neodymium iron boron chamfer mud is characterized by comprising the following steps:
slurrying the neodymium iron boron chamfer angle with water to obtain waste slurry;
carrying out slag separation treatment on the waste slurry to obtain slag-removed slurry;
carrying out low-intensity magnetic separation on the slag-removed slurry to obtain a low-intensity magnetic separation rare earth iron alloy and a low-intensity magnetic separation tailing slurry; the magnetic field intensity of the low-intensity magnetic separation is 2000-3000 Gs;
carrying out strong magnetic separation on the low-intensity magnetic separation tailing slurry to obtain a rare-earth iron alloy with strong magnetic separation; the magnetic field intensity of the strong magnetic separation is 10000-15 kGs.
2. The method according to claim 1, wherein the solid content of the neodymium iron boron waste slurry is 50-70 wt%.
3. The method according to claim 1, wherein the slag removal treatment is performed by using a slag removal screen having a pore size of 2 to 5mm.
4. The method of claim 1, further comprising, prior to the low intensity magnetic separation: and adding water into the deslagging slurry for dilution.
5. The method according to claim 4, wherein the diluted slurry obtained by the dilution has a solid content of 20 to 30wt%.
6. The method according to claim 1, wherein the strong magnetic separation is pulsed strong magnetic separation, the pulse stroke of the pulsed strong magnetic separation is 6-12 mm, and the number of pulses is 120-220 r/min.
7. The method according to claim 1 or 6, wherein the equipment adopted by the strong magnetic separation is a vertical ring pulsating high gradient strong magnetic machine.
8. The method of claim 1, further comprising, after the low intensity magnetic separation: and concentrating and dehydrating the wet low-intensity magnetic separation rare-earth iron alloy obtained by low-intensity magnetic separation to obtain the low-intensity magnetic separation rare-earth iron alloy.
9. The method of claim 1, further comprising, after said high magnetic separation: and concentrating and dehydrating the wet-strength magnetic separation rare-earth ferroalloy obtained by strong magnetic separation to obtain the strong magnetic separation rare-earth ferroalloy.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102994756A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for enriching rare earth elements from red mud |
| CN104894363A (en) * | 2015-06-24 | 2015-09-09 | 东北大学 | Method for using low-grade niobium concentrate to produce niobium-iron alloy and rare earth double sulfate salt |
| CN206008984U (en) * | 2016-07-04 | 2017-03-15 | 艺利磁铁（天津）有限公司 | A kind of magnetized rare earth machine of multi-angle |
| WO2017163094A1 (en) * | 2016-03-25 | 2017-09-28 | Fakon Vállalkozási Kft. | Process for processing red mud and producing rare-earth metal salts |
| CN111871594A (en) * | 2020-06-30 | 2020-11-03 | 中国地质科学院矿产综合利用研究所 | Mineral processing technology for recovering phosphorus and rare earth from vanadium titano-magnetite |
| CN112458295A (en) * | 2020-10-28 | 2021-03-09 | 赣州金环磁选设备有限公司 | Efficient mineral processing method for recycling iron blast furnace ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994756A (en) * | 2012-09-29 | 2013-03-27 | 贵州绿水青山环保科技有限公司 | Method for enriching rare earth elements from red mud |
| CN104894363A (en) * | 2015-06-24 | 2015-09-09 | 东北大学 | Method for using low-grade niobium concentrate to produce niobium-iron alloy and rare earth double sulfate salt |
| WO2017163094A1 (en) * | 2016-03-25 | 2017-09-28 | Fakon Vállalkozási Kft. | Process for processing red mud and producing rare-earth metal salts |
| CN206008984U (en) * | 2016-07-04 | 2017-03-15 | 艺利磁铁（天津）有限公司 | A kind of magnetized rare earth machine of multi-angle |
| CN111871594A (en) * | 2020-06-30 | 2020-11-03 | 中国地质科学院矿产综合利用研究所 | Mineral processing technology for recovering phosphorus and rare earth from vanadium titano-magnetite |
| CN112458295A (en) * | 2020-10-28 | 2021-03-09 | 赣州金环磁选设备有限公司 | Efficient mineral processing method for recycling iron blast furnace ash |
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