WO2012137727A1 - Procédé de séparation et de récupération de terres rares - Google Patents

Procédé de séparation et de récupération de terres rares Download PDF

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WO2012137727A1
WO2012137727A1 PCT/JP2012/058914 JP2012058914W WO2012137727A1 WO 2012137727 A1 WO2012137727 A1 WO 2012137727A1 JP 2012058914 W JP2012058914 W JP 2012058914W WO 2012137727 A1 WO2012137727 A1 WO 2012137727A1
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rare earth
earth elements
separating
group
chloride
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PCT/JP2012/058914
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English (en)
Japanese (ja)
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山本　浩貴
克佳 古澤
哲也 宇田
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株式会社日立製作所
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Priority to CN201280013131.2A priority Critical patent/CN103443304B/zh
Publication of WO2012137727A1 publication Critical patent/WO2012137727A1/fr

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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/253—Halides
    • C01F17/259—Oxyhalides
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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

Definitions

  • the present invention relates to a technique for separating and collecting rare earth elements, and more particularly to a method for separating and collecting rare earth elements from a composition containing a plurality of types of rare earth elements.
  • rare earth magnets used in rotating electrical machines such as drive motors for hybrid vehicles and compressors for air conditioners are required to have a high coercive force even in high temperature environments (eg, about 200 ° C).
  • high temperature environments eg, about 200 ° C.
  • rare earth magnets used in rotating electrical machines such as drive motors for hybrid vehicles and compressors for air conditioners are required to have a high coercive force even in high temperature environments (eg, about 200 ° C).
  • high temperature environments eg, about 200 ° C
  • rare earth magnets In addition to neodymium, iron, and boron It contains a lot of expensive and heavy heavy rare earth elements (for example, dysprosium).
  • Rare earth magnets are indispensable now, and demand is expected to increase in the future.
  • rare earth elements are difficult and expensive to separate and purify single elements
  • development of technologies and alternative materials for reducing the amount of use while maintaining the performance of magnets has been intensively studied.
  • Patent Document 1 discloses a divalent trivalent mixture in which the average valence of two or more rare earth ions is 2 or more and 3 or less by halogenating a rare earth element in a mixture containing a plurality of rare earth elements or compounds thereof. Producing a mixture containing a rare earth halide which is not dissolved in an aqueous solution or an organic solvent, and then utilizing the difference in properties between the divalent rare earth halide and the trivalent rare earth halide, There has been proposed a rare earth element separation method characterized by separating elements into at least two groups. According to Patent Document 1, it is said that the separation factor between rare earth elements can be dramatically increased, and mutual separation can be performed more efficiently than in the conventional method.
  • steps such as acid dissolution, filtration, precipitation removal of impurities, concentration, neutralization, and drying, which are essential for conventional wet methods, can be omitted. It is said that the cost can be greatly reduced.
  • Patent Document 2 discloses a method for recovering a rare earth element from a material containing a rare earth element and an iron group element, and a rare earth element such as a rare earth magnet scrap or sludge is added to a gaseous or molten iron chloride. Select a rare earth element as a chloride from the substance by contacting a substance containing an iron group element and proceeding the chlorination reaction of the rare earth element in the substance while maintaining the metallic state of the iron group element in the substance. There has been proposed a method for recovering a rare earth element characterized by having a step of recovering automatically.
  • Patent Document 2 it is possible to extract and separate only high-purity rare earth components from materials containing rare earth elements and iron group elements, such as rare earth magnet scraps or sludges, especially wastes, and thus lower cost rare earth elements. It is said that the magnet recycling law can be established.
  • JP 2001-303149 A Japanese Patent Laid-Open No. 2003-73754
  • rare earth elements such as neodymium and dysprosium, which are rare earth magnet raw materials, are unevenly distributed on the earth, and technologies for separating, recovering and recycling rare earth elements from the viewpoint of ensuring the stability of raw materials and effective use of resources. Is becoming more important than before.
  • an object of the present invention is to provide a method capable of separating and recovering rare earth elements with higher yield than the prior art.
  • One aspect of the present invention is a method for separating and recovering a plurality of types of rare earth elements, wherein a chemical reaction is performed in the presence of an oxygen source with respect to a mixture containing a halide of the types of rare earth elements.
  • the rare earth halide means a fluoride, chloride, bromide or iodide of a rare earth element, and is represented by the general chemical formula REX 3 (RE: rare earth element, X: halogen element). .
  • the rare earth oxyhalide is represented by the general chemical formula REOX (O: oxygen).
  • Another embodiment of the present invention is a method for separating and recovering a plurality of types of rare earth elements, wherein a chemical reaction is performed in the presence of a halogen source on a mixture containing the oxides of the plurality of types of rare earth elements.
  • a step of separating the first group of rare earth elements and the second group of rare earth elements by solid-liquid separation of the solid phase To provide a method of separating and recovering that rare earth elements.
  • the present invention can add the following improvements and changes to the above-described rare earth element separation and recovery methods (I) and (II).
  • the halogen is chlorine.
  • the neodymium is contained as the rare earth element of the first group, and dysprosium is contained as the rare earth element of the second group.
  • Still another embodiment of the present invention is a method for separating and recovering a plurality of kinds of rare earth elements, wherein the compound containing the plurality of kinds of rare earth elements, iron, and boron is chlorinated using iron chloride.
  • the first group of rare earth element rare earth chlorides and the second group rare earth element rare earth oxychlorides are chemically reacted with the mixture of the rare earth element chlorides in the presence of an oxygen source.
  • a method for separating and recovering rare earth elements comprising a step of separating two groups of rare earth elements.
  • Still another aspect of the present invention is a method for separating and recovering a plurality of types of rare earth elements, and a step of subjecting the compound containing the plurality of types of rare earth elements, iron, and boron to a roasting treatment; A step of immersing the roasted compound in an acid to selectively leaching the plurality of rare earth elements, a step of generating a precipitate of the plurality of rare earth elements from an acid leaching solution, and the precipitation Forming a mixture of the plurality of rare earth oxides from the product, and chemically reacting the mixture of the plurality of rare earth oxides in the presence of a chlorine source with the rare earth oxide of the first group.
  • the present invention can add the following improvements and changes to the above-described rare earth element separation and recovery methods (III) and (IV).
  • (Iii) The neodymium and dysprosium are included as the plurality of kinds of rare earth elements.
  • the rare earth chloride is neodymium chloride, and the rare earth oxychloride is dysprosium oxychloride.
  • rare earth elements for example, neodymium, dysprosium, etc.
  • waste of rare earth magnets for example, non-use, defective products, sludge, etc.
  • the separated rare earth elements are recycled as raw materials. be able to. This can contribute to effective utilization of resources and stable securing of rare earth materials.
  • 2 is a chart showing an example of a powder X-ray diffraction pattern obtained in Example 1.
  • 5 is a graph showing the relationship between the Nd concentration ratio (Nd / (Nd + Dy)) obtained from FIG. 4 and the distillation temperature.
  • Figure 1 shows the equilibrium of the neodymium-oxygen-chlorine (Nd-O-Cl) chemical potential diagram and the dysprosium-oxygen-chlorine (Dy-O-Cl) chemical potential diagram at 727 ° C (1000 K). It is a state diagram.
  • a solid line is a chemical potential diagram of neodymium
  • a broken line is a chemical potential diagram of dysprosium.
  • the oxide (RE 2 O 3 ) is stable in the region where the oxygen potential is high and the chlorine potential is low
  • the chloride (REC1) is used in the region where the chlorine potential is high and the oxygen potential is low.
  • the metal (RE) is stable in the region where the oxygen potential is low and the chlorine potential is low. Further, a stable region of oxychloride (REOCl) exists between the stable region of oxide and the stable region of chloride.
  • neodymium is stable in trivalent chloride (NdCl 3 ), and dysprosium is stable in dysprosium oxychloride (DyOCl). Accordingly, if the potential of chlorine and oxygen can be controlled so as to fall within this ABCDE region, neodymium chloride and dysprosium oxychloride can coexist.
  • examples of the oxygen source include moisture adsorbed on chlorides, oxides that may be present on the surface of the crucible, oxygen gas that cannot be removed by exhaust using a rotary pump or the like, and the like.
  • oxygen is fixed as MgO, so the three-phase equilibrium point (point F) of Mg / MgCl 2 / MgO. ) Can control the potential of the system.
  • Mg, MgCl 2 , NdCl 3 , and DyOCl mainly remain as residues after the completion of the reaction.
  • Mg and MgCl 2 have a high vapor pressure, and therefore can be discharged out of the system by exhausting / distilling with a rotary pump or the like.
  • NdCl 3 and DyOCl remain in the crucible.
  • the separation process (procedure) of rare earth elements and other elements is basically the same as the process disclosed in Patent Document 2, but is specifically as follows. As described above, it is preferable to use waste (for example, non-use, defective products, sludge, etc.) as the rare earth magnet for element separation, and it should be in powder form from the viewpoint of separation and recovery efficiency (chemical reaction efficiency). Is preferred. In the following, separation of rare earth magnets from sludge powder will be described as an example.
  • FIG. 2 is a schematic cross-sectional view showing a state immediately after the separation step in an example of a distillation apparatus used in the separation step of rare earth elements and other elements.
  • the distillation apparatus 20 is a cylindrical vertical electric furnace having two vertical heaters (upper heater 1, lower heater 2, thermocouples 3, 3 ′) on the outer periphery of a vertical furnace core tube 4.
  • the core tube 4 has an exhaust port 5, a gas introduction port 6, and an upper lid 7 so that the inside can be exhausted and replaced with gas.
  • the exhaust port 5 is connected to a rotary pump or the like (not shown).
  • FIG. 2 although the bottomed core tube 4 was illustrated, the structure sealed with a lower cover may be sufficient.
  • the installation location of the exhaust port 5 and the gas introduction port 6 is not particularly limited.
  • a high temperature side recovery unit 8 is installed in the region of the lower heater 2, and a low temperature side recovery unit 9 is disposed in the region of the upper heater 1.
  • the crucible 10 containing the material to be separated by distillation is installed at the bottom of the high temperature side recovery unit 8.
  • the sludge powder dried using a dryer or the like is crushed. Thereafter, the crushed sludge powder, graphite powder, and iron dichloride (FeCl 2 ) in excess of the stoichiometric amount are mixed and filled in the crucible 10.
  • the crucible 10 is installed at the bottom of the high temperature side recovery unit 8 and inserted into the core tube 4 of the distillation apparatus 20.
  • the inside of the furnace tube 4 is evacuated and replaced with an inert gas such as argon gas, and then heated at 700 to 900 ° C. while flowing an inert gas.
  • the mixed material in the crucible 10 chemically reacts, and a mixture of rare earth chloride, unreacted iron dichloride, iron or an iron group element alloy is obtained in the crucible 10 (mixture containing chloride).
  • Generating step The oxygen component fixed in the rare earth magnet sludge powder is gasified by the graphite powder (carbon component), and the generated gas is discharged out of the system by the flowing inert gas.
  • the obtained rare earth chloride, iron dichloride, iron or iron group element alloy mixture is subjected to distillation separation by heating while reducing pressure with a rotary pump.
  • the temperature of the upper heater 1 (maximum temperature of the low temperature side recovery unit 9) is maintained at 400 to 500 ° C
  • the temperature of the lower heater 2 (maximum temperature of the high temperature side recovery unit 8) is maintained at 700 to 1100 ° C. It is preferable.
  • a condensed phase of iron dichloride is formed in the low temperature side recovery unit 9
  • a condensed phase of rare earth chloride is formed in the high temperature side recovery unit 8
  • iron and iron group elements are contained in the crucible 10.
  • the alloy remains as a residue (step of separating a mixture of chlorides of a plurality of rare earth elements).
  • a mixture of a plurality of types of rare earth chlorides is obtained.
  • a mixture of neodymium chloride and dysprosium chloride is obtained.
  • the charged crucible 10 is installed at the bottom of the high temperature side recovery unit 8 and inserted into the reactor core tube 4 of the distillation apparatus 20.
  • the inside of the furnace core tube 4 is evacuated and replaced with an inert gas such as argon gas, and then heated at 700 to 900 ° C. for 6 to 24 hours while flowing an inert gas.
  • an inert gas such as argon gas
  • the mixed material in the crucible 10 chemically reacts, and dysprosium oxychloride and magnesium chloride are obtained as products in the crucible 10
  • neodymium chloride and magnesium metal are obtained as unreacted materials (first reaction).
  • distillation separation is performed by evacuating with a rotary pump while keeping the furnace body at a high temperature.
  • the temperature of the upper heater 1 is preferably maintained at 400 to 500 ° C.
  • the temperature of the lower heater 2 is preferably maintained at 900 to 1100 ° C.
  • a condensed phase 12 of magnesium metal and a condensed phase 13 of magnesium chloride are formed in the low-temperature side recovery section 9, and neodymium chloride and dysprosium oxychloride remain as main residual components in the crucible 10. To do.
  • the distillation apparatus 20 is cooled to room temperature.
  • the residue remaining in the crucible 10 is poured into pure water and stirred.
  • neodymium chloride is preferentially dissolved and extracted in pure water, and dysprosium oxychloride remains as a solid phase residue (rare earth chloride is extracted into the liquid phase and the rare earth oxychloride is dissolved in the solid phase. As a process).
  • neodymium can be concentrated in the liquid phase.
  • the liquid phase from which the neodymium chloride is extracted and the solid phase of the remaining dysprosium oxychloride are subjected to solid-liquid separation (step of separating the first group of rare earth elements and the second group of rare earth elements). Thereby, neodymium and dysprosium can be separated.
  • a precipitant eg, ammonium carbonate ((NH 4 ) 2 CO 3 ), ammonium hydrogen carbonate (NH 4 HCO 3 ), sodium carbonate (Na 2 CO 3 ), sodium bicarbonate (NaHCO 3 ), oxalic acid ((COOH) 2 ), sodium oxalate ((COONa) 2 ), ammonium hydroxide (NH 4 OH), etc.
  • a soluble neodymium salt precipitate is formed. The precipitate is filtered and dried, and then neodymium oxide can be recovered by baking at about 900 ° C. in the atmosphere.
  • the solid phase dysprosium oxychloride obtained above is dissolved in an acid (dilute hydrochloric acid, dilute nitric acid, etc.), adjusted to pH in the aqueous solution, and then precipitated with a precipitant (for example, ammonium carbonate (( NH 4 ) 2 CO 3 ), ammonium bicarbonate (NH 4 HCO 3 ), sodium carbonate (Na 2 CO 3 ), sodium bicarbonate (NaHCO 3 ), oxalic acid ((COOH) 2 ), sodium oxalate ((COONa 2 ), ammonium hydroxide (NH 4 OH), etc.) is added to form a dysprosium salt precipitate which is sparingly soluble in water. After the precipitate is filtered and dried, dysprosium oxide can be recovered by baking at about 900 ° C. in the atmosphere.
  • a precipitant for example, ammonium carbonate (( NH 4 ) 2 CO 3 ), ammonium bicarbonate (NH 4 HCO
  • the neodymium oxide and dysprosium oxide recovered above can be reduced to metal neodymium and metal dysprosium by performing molten salt electrolysis using a fluoride bath or the like. These rare earth metals can be reused as raw materials for rare earth magnets.
  • Example 1 Separation and recovery from rare earth oxide mixtures were studied. Neodymium oxide (Nd 2 O 3 ) powder and dysprosium oxide (Dy 2 O 3 ) powder were used as starting materials for the rare earth oxide, and anhydrous dysprosium chloride (DyCl 3 ) powder was used as the starting material for the chlorine source .
  • starting powder reagents 3N grades manufactured by Kojundo Chemical Laboratory Co., Ltd. were used. Weigh and mix 2.5 mmol (0.84 g) Nd 2 O 3 powder, 2.5 mmol (0.93 g) Dy 2 O 3 powder, and 5.0 mmol (1.34 g) DyCl 3 powder in a drying chamber. The reaction vessel was charged and sealed under a nitrogen atmosphere. Sealing was performed by capping a stainless steel reaction vessel and welding with argon.
  • FIG. 3 is a chart showing an example of a powder X-ray diffraction pattern obtained in Example 1.
  • NdCl 3 .6H 2 O and DyOCl were identified from the X-ray diffraction pattern of the powder after the chemical reaction, but Nd 2 used as a starting material for the rare earth oxide and chlorine source. O 3 , Dy 2 O 3 , and DyCl 3 peaks were not observed. That is, it was confirmed that the mixed powder of the rare earth oxide and the chlorine source was changed into a mixture of the rare earth chloride and the rare earth oxo chloride by the chemical reaction by the heat treatment. In addition, although neodymium chloride became hexahydrate, it is thought that this was adsorbed after sampling from the reaction container and before powder X-ray diffraction measurement.
  • the Nd component and the Dy component were quantitatively analyzed by ICP-AES method (inductively coupled plasma emission spectrometry) for the non-turbid filtrate.
  • ICP-AES method inductively coupled plasma emission spectrometry
  • the Nd concentration was 900 mg / L and the Dy concentration was 700 mg / L.
  • Nd and Dy are eluted in an equivalent manner.
  • Example 2 Separation and recovery from rare earth chloride mixtures were studied.
  • 2.5 g each of NdCl 3 powder and DyCl 3 powder was weighed in a drying chamber, and 5.0 g of Mg powder was weighed and filled in a crucible 10 made of molybdenum.
  • the distillation apparatus 20 was heated to 300 ° C. and held for 12 hours or longer. After the raw material powder and the inside of the furnace core tube 4 were dried by heating under vacuum, argon gas was introduced to bring the system to atmospheric pressure. In order to remove excess oxygen remaining in the reactor core tube 4 and the gas inlet 6 as much as possible, the operation of exhausting and introducing gas was further repeated five times. After introducing argon gas, the gas stream was maintained. Thereafter, the temperature of the lower heater 2 was set to 800 ° C. and the temperature of the upper heater 1 was set to 400 ° C. for 6 hours under an argon stream atmosphere, and the raw material powder was chemically reacted.
  • the rotary pump was evacuated for 3 hours while maintaining the temperature as it was, and an excess Mg that was supposed to remain in the crucible 10 and MgCl 2 as a reaction product were subjected to distillation separation.
  • the distillation apparatus 20 was cooled to room temperature while being evacuated to vacuum. According to the same procedure, when the temperature of the lower heater 2 is 900 ° C. and the temperature of the upper heater 1 is 450 ° C., and the temperature of the lower heater 2 is 1000 ° C. and the temperature of the upper heater 1 is 500 ° C. The case was done separately.
  • the crucible 10 was taken out from the distillation apparatus 20 and sampled.
  • the residue in the crucible 10 was weighed out to 0.5 g, quickly poured into 50 mL of pure water, and stirred with a stirrer for 24 hours.
  • the distillation temperature maximum temperature of the high temperature side recovery unit 8
  • the distillation temperature was 800 ° C. and 900 ° C.
  • the distillation temperature was 1000 ° C., no bubbles were observed and no residue was observed.
  • FIG. 4 is a graph showing the relationship between the concentration of rare earth elements (Nd, Dy) dissolved in water and the distillation temperature.
  • FIG. 5 is a graph showing the relationship between the Nd concentration ratio (Nd / (Nd + Dy)) obtained from FIG. 4 and the distillation temperature.
  • Nd concentration ratio
  • the charged composition of the rare earth chloride is 2.5 g of NdCl 3 and DyCl 3 (that is, the charged molar ratio of Nd element and Dy element is 49:51). From).
  • Nd chloride is remarkably dissolved in water, and Dy oxychloride is less soluble in water than Nd chloride and tends to remain as a solid phase. That is, it was confirmed that neodymium and dysprosium can be separated efficiently.
  • Example 3 We studied the separation and recovery of rare earth elements from waste materials of rare earth magnets (RE 2 Fe 14 B) containing neodymium, dysprosium, praseodymium, iron and boron.
  • the mass composition of the rare earth magnet used was 61.2% Fe-23.1% Nd-3.5% Dy-2.0% Pr-1.0% B.
  • the waste magnet is a defective product because cracks, chips, etc. occur after nickel plating in the manufacturing process.
  • the waste magnet was roughly pulverized by heating at 800 ° C. in a hydrogen atmosphere using an electric furnace. As described above, the waste magnet was nickel-plated. However, since the nickel-plated film can be peeled off by the hydrogen pulverization step, the peeled-off plated film was separated from the magnet powder by sieving.
  • the obtained magnetic powder was mixed with FeCl 2 powder as a chlorine source and placed in an iron crucible 10 and placed in the distillation apparatus 20 shown in FIG.
  • the Inconel furnace core tube 4 is evacuated with a rotary pump and then replaced with argon gas.
  • the temperature of the lower heater 2 is set to 800 ° C.
  • the temperature of the upper heater 1 is set to 400 ° C., and maintained for 10 to 15 hours. Reaction was performed. Thereafter, the temperature of the lower heater 2 was raised to 1000 ° C., the temperature of the upper heater 1 was raised to 500 ° C., and vacuum distillation was performed for 3 hours while exhausting with a rotary pump. After vacuum distillation, the furnace core tube 4 was cooled in the furnace while maintaining a vacuum.
  • the condensate adhesion state of the high temperature side recovery unit 8 and the low temperature side recovery unit 9 was observed, and the high temperature side recovery unit 8 had a light purple powder or light green powder in the region of 800 to 500 ° C.
  • the white powdery substance was condensed, and the orange powdery substance was condensed in the low temperature side recovery unit 9 at a temperature lower than 500 ° C. It was observed that these condensed substances absorb moisture in a short time when left in a general room.
  • the condensed substances in the region of 800 to 500 ° C are mainly composed of compounds of rare earth elements (neodymium, praseodymium, dysprosium). It was confirmed that the content was 98%.
  • neodymium, praseodymium and dysprosium can be separated from each other.

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Abstract

La présente invention concerne un procédé permettant de séparer et de récupérer des terres rares avec un rendement supérieur à celui des techniques conventionnelles. Ledit procédé de séparation et de récupération de terres rares, grâce auquel de multiples sortes de terres rares sont séparées et récupérées, consiste à : atteindre un équilibre chimique entre des halogénures de terres rares du groupe 1 et des oxyhalogénures de terres rares du groupe 2, en faisant réagir chimiquement un mélange contenant des halogénures des multiples sortes de terres rares en présence d'une source d'oxygène, ou en faisant réagir chimiquement un mélange contenant des oxydes des multiples sortes de terres rares en présence d'une source d'halogène ; verser les halogénures de terres rares et les oxyhalogénures de terres rares dans de l'eau pour y dissoudre sélectivement les halogénures de terres rares et extraire ainsi les halogénures de terres rares dans une phase liquide tout en laissant les oxyhalogénures de terres rares sous la forme d'une phase solide ; et soumettre la phase liquide qui contient les halogénures de terres rares extraits et la phase solide des oxyhalogénures de terres rares à une séparation solide/liquide pour séparer ainsi les terres rares du groupe 1 des terres rares du groupe 2.
PCT/JP2012/058914 2011-04-08 2012-04-02 Procédé de séparation et de récupération de terres rares WO2012137727A1 (fr)

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JP2011086004A JP5401497B2 (ja) 2011-04-08 2011-04-08 希土類元素の分離回収方法
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Cited By (9)

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JP2013087318A (ja) * 2011-10-17 2013-05-13 Chiyoda Kako Kensetsu Kk 目的物質の分離・回収方法及び分離・回収システム
JP2013087317A (ja) * 2011-10-17 2013-05-13 Chiyoda Kako Kensetsu Kk 目的物質の分離・回収方法及び分離・回収システム
CN103225023A (zh) * 2013-04-26 2013-07-31 连云港市丽港稀土实业有限公司 一种从稀土渣中浸出回收稀土元素的方法
WO2014057922A1 (fr) * 2012-10-10 2014-04-17 日立金属株式会社 Procédé et dispositif de séparation d'éléments de terres rares
WO2014057541A1 (fr) * 2012-10-10 2014-04-17 株式会社日立製作所 Procédé et dispositif pour séparer des éléments de terres rares
US20140356258A1 (en) * 2012-01-06 2014-12-04 Hitachi Metals, Ltd. Method for Separating and Recovering Rare-Earth Elements
WO2015019433A1 (fr) * 2013-08-07 2015-02-12 株式会社日立製作所 Appareil de séparation et de récupération des terres rares
WO2015019434A1 (fr) * 2013-08-07 2015-02-12 株式会社日立製作所 Appareil de séparation et de récupération de terres rares
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IL248600A0 (en) 2016-10-30 2017-02-01 Yeda Res & Dev A method for obtaining platinum group metals from spent catalysts
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WO2022003694A1 (fr) * 2020-07-01 2022-01-06 Yeda Research And Development Co. Ltd. Récupération de métaux des terres rares à partir d'alliages ferromagnétiques

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JP2013087318A (ja) * 2011-10-17 2013-05-13 Chiyoda Kako Kensetsu Kk 目的物質の分離・回収方法及び分離・回収システム
US20140356258A1 (en) * 2012-01-06 2014-12-04 Hitachi Metals, Ltd. Method for Separating and Recovering Rare-Earth Elements
US9376736B2 (en) * 2012-01-06 2016-06-28 Hitachi Metals, Ltd. Method for separating and recovering rare-earth elements
WO2014057922A1 (fr) * 2012-10-10 2014-04-17 日立金属株式会社 Procédé et dispositif de séparation d'éléments de terres rares
WO2014057541A1 (fr) * 2012-10-10 2014-04-17 株式会社日立製作所 Procédé et dispositif pour séparer des éléments de terres rares
JP5967210B2 (ja) * 2012-10-10 2016-08-10 日立金属株式会社 希土類元素の分離方法および分離装置
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WO2015019433A1 (fr) * 2013-08-07 2015-02-12 株式会社日立製作所 Appareil de séparation et de récupération des terres rares
WO2015019434A1 (fr) * 2013-08-07 2015-02-12 株式会社日立製作所 Appareil de séparation et de récupération de terres rares
WO2015118621A1 (fr) * 2014-02-05 2015-08-13 株式会社日立製作所 Procédé et appareil pour la séparation d'éléments des terres rares
CN106062222A (zh) * 2014-02-05 2016-10-26 株式会社日立制作所 稀土元素的分离方法及分离装置
JPWO2015118621A1 (ja) * 2014-02-05 2017-03-23 株式会社日立製作所 希土類元素の分離方法および分離装置
CN106062222B (zh) * 2014-02-05 2017-09-26 株式会社日立制作所 稀土元素的分离方法及分离装置

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