WO2003078671A1 - Procede pour recuperer un element utile dans les rebuts de terres rares alliees a des metaux de transition - Google Patents

Procede pour recuperer un element utile dans les rebuts de terres rares alliees a des metaux de transition Download PDF

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Publication number
WO2003078671A1
WO2003078671A1 PCT/JP2003/003238 JP0303238W WO03078671A1 WO 2003078671 A1 WO2003078671 A1 WO 2003078671A1 JP 0303238 W JP0303238 W JP 0303238W WO 03078671 A1 WO03078671 A1 WO 03078671A1
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Prior art keywords
rare earth
scrap
precipitate
mineral acid
acid
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PCT/JP2003/003238
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English (en)
Japanese (ja)
Inventor
Hiroshi Ohrai
Hideo Yokoi
Original Assignee
Santoku Corporation
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Application filed by Santoku Corporation filed Critical Santoku Corporation
Priority to JP2003576661A priority Critical patent/JP4287749B2/ja
Priority to AU2003221047A priority patent/AU2003221047A1/en
Publication of WO2003078671A1 publication Critical patent/WO2003078671A1/fr

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Definitions

  • the present invention relates to a method for recovering useful elements that can economically and safely recover useful elements such as rare earth elements from rare earth transition alloy scrap.
  • rare earth-transition metal alloys include rare earth-copartite and rare earth-iron-boron permanent magnets.
  • the magnet usually contains, for example, about 30 to 35% by weight of a rare earth element such as Nd, Pr, and Dy, about 60 to 65% by weight of iron, and 1 to 2% by weight of boron.
  • An alloy containing A1 etc. (hereinafter sometimes referred to as a rare-earth iron-based alloy) is used as a raw material, compacted after pulverization and then sintered to form a sintered magnet, or kneaded with resin. I have.
  • scraps such as a large amount of alloy scraps and polishing scraps in the process of powder frame, molding, sintering, cutting or grinding unnecessary parts, inspection etc. Occurs and accounts for 30-40% of the product weight.
  • a scrap in which powder such as polishing waste is in a slurry state with a polishing liquid or water is hereinafter referred to as sludge in particular.
  • waste is inevitably generated in terms of the loss of the molten slag, the production yield, and the milling yield. Approximately 30% by weight of these scrap components are expensive and useful rare earth elements, and their recovery is strongly demanded from the viewpoints of effective use of resources and economy.
  • the (1) acid dissolving method is a method of dissolving the entire amount of scrap with an acid and recovering a rare earth compound in the form of rare earth fluoride, rare earth oxalate or the like from the solution.
  • a mineral acid such as sulfuric acid, hydrochloric acid, or nitric acid at a high concentration and in an amount equivalent to the scrap.
  • the scrap is a solid solid such as a truncated portion during magnet molding or a defective magnet body, or a sludge mixed with such a solid solid
  • acid mist, hydrogen gas, and NOx gas are generated, so there is also a problem in working environment safety.
  • a scrap is once burned and oxidized to an oxide, and a rare earth element is mainly eluted using a strong acid, and the form of rare earth oxalate, rare earth carbonate or the like is extracted from the solid oxide.
  • This is a method for recovering rare earth compounds.
  • the scrap is ignitable sludge such as abrasive waste
  • the oxidation can proceed if it is once ignited by a heating / combustion device after drying.
  • the drying and firing of the sludge is costly in terms of equipment and energy, and the work efficiency is low, such as the need to grind oxides after firing.
  • it is not easy to oxidize the core of the scrap containing the solid solid it is necessary to separately perform preliminary pulverization, which further lengthens the working process.
  • the (3) pH-controlled monoacid leaching method is a method in which sludge is introduced into hydrochloric acid or the like, and the pH is maintained at 3 to 5 to elute rare earth elements (Japanese Patent Publication No. 7-72312), or the pH is 5 or more.
  • This is a method of eluting a rare earth element with dilute nitric acid while maintaining the temperature (JP-A-9-217132).
  • Pre-grinding process is indispensable if lumpy solids are mixed.
  • the conventional chemical separation / recovery method requires a large amount of high-concentration acid, regardless of which method is used.
  • sludge containing solid matter cannot be handled as it is, and pre-sorting and preliminary powder framing are required, making it difficult to implement large-scale treatment in terms of cost. Disclosure of the invention
  • a rare earth transition alloy scrap is immersed in a mineral acid ammonium H solution (hereinafter referred to as MAS 7) (A), and the MAS water in step (A) is immersed.
  • a step of passing a gas containing oxygen and oxidizing the scrap to obtain a precipitate containing a powder containing at least one of oxides and hydroxides and a step (B).
  • Recovery of useful elements from rare earth-transition metal alloy scrap including a step (C) of separating the precipitate from the MAS ⁇ solution and a step (D) of recovering the rare earth element from the precipitate separated in step (C)
  • a method is provided.
  • FIG. 1 is a graph showing the relationship between the solids remaining rate and the immersion time depending on the type of the MAS 7 solution in the oxidation treatments performed in Test Examples 1 to 5.
  • FIG. 2 is a graph showing the relationship between the immersion temperature and the time until the residual ratio of solids becomes 10% or less in the oxidation treatment performed in Test Example 6.
  • FIG. 3 is a graph showing the results of X-ray diffraction measurement of the oxide powder prepared in Test Example 6.
  • FIG. 4 is a graph showing the relationship between the concentration of ammonium sulfate and the immersion time until the residual ratio of solids becomes 10% or less in the oxidation treatments performed in Test Examples 7 and 8.
  • the rare earth-transition metal alloy to be recovered includes a rare earth-cobalt permanent magnet alloy, a rare earth-iron-boron permanent magnet alloy, and a rare earth-iron-boron permanent magnet alloy.
  • Typical magnetic materials include permanent magnet alloys in which boron has been replaced with carbon, nitrogen, etc., rare earth-iron-cobalt alloys for forming magneto-optical recording thin films, and sputtering target materials, and are usually contained in these alloys.
  • the rare earth element may be any of light rare earth elements such as Nd, Pr and Sm, heavy rare earth elements such as Gd, Tb and Dy, or a mixture thereof.
  • the form of the scrap to be subjected to the recovery process is as follows: a solid compact such as a compact, a sintered body, or a waste magnet body that is cut off in the process of being processed into a magnetic material such as a magnet from the above alloy; Sludge, which is a suspended waste of alloy powder such as, and polishing liquid, water, oil, etc .; sludge mixed with lumpy solids is mainly used.
  • solid substances such as dissolved slag derived in the raw metal production process are also included in the scope of the present invention.
  • the present inventors have proposed a method for recovering active elements at a high rate without using a large amount of acid, A simple collection method that eliminates the pre-selection and pre-grinding of the massive solids, which has been a major obstacle to the conventional collection process, and can be dealt with only by a chemical process that requires little human and equipment load.
  • scraps such as sludge, massive solids, or sludge mixed with both are reacted with MAS water under specific conditions to reduce oxides and / or hydroxides as a whole.
  • these powders are collectively abbreviated as oxide powder), and useful elements such as rare earth elements can be easily recovered from the oxide powder. And completed the present invention.
  • ammonium salt of a mineral acid in the MAS film examples include ammonium chloride (NH 4 C1), ammonium sulfate ((NH 4 ) 2 SO 4 ), ammonium nitrate (NH 4 NO 3 ), and ammonium hydrogen fluoride (NH 4 NO 3 ). NH 4 HF2), etc. Of these, ammonium sulfate is the most effective in promoting the oxidation and disintegration of scrap.
  • the concentration of MAS 7W ⁇ 3 ⁇ 4 can be appropriately determined depending on the form of the scrap, the ease of oxidative degradation, and the allowable reaction time. Usually, it is 0.1 to 2.0 molZl, preferably 0.2 to 1.5 molZl. If the concentration is less than 0.1 molZl, the reaction rate is too slow to be practical, and if it exceeds 2.0 mol / l, no further improvement in the reaction rate is observed, which is not preferable. If the scrap is sludge, the MAS water concentration is the concentration after dilution with the water in the sludge.
  • the scrap can be immersed in the MAS 7 solution by, for example, containing the MAS ⁇ solution having the above concentration and an appropriate amount of scrap in a reaction vessel. At this time, if the scrap is sludge, it can be stored after removing the water and oil from the supernatant if necessary.
  • a material which is hardly contaminated such as FRP is suitably used.
  • the amount of scrap contained in the container and the amount of MAS 7j solution, the amount of scrap relative to the total amount, that is, the concentration of scrap is not particularly limited, and the scrap is immersed in the aqueous solution and agitated simultaneously with aeration or aeration described later. If the gas containing oxygen and MAS 7_ ⁇ ⁇ can be sufficiently corroded with the scrap when performing the The concentration of the tip is acceptable. Although the mechanism is not fully understood, the ammonium salt of the mineral acid in MAS 7 used in the present invention probably acts as a reaction promoter or catalyst when the scrap is oxidized by air, and the conventional scrap is directly converted into a metal.
  • the step (B) of passing a gas containing oxygen through the MAS 7) in the step (A) to oxidize the scrap to obtain a precipitate containing an oxide powder is performed.
  • the gas containing oxygen air can be usually used, but it is not particularly limited as long as it is a gas containing an amount of oxygen enough to obtain a desired oxide powder.
  • the method of flowing such a gas through the MAS aqueous solution is not particularly limited.
  • the method can be performed by a method of publishing the gas.
  • gas containing oxygen and MAS water may be mixed using known stirring means and mixing means. The scythe may be in sufficient contact with the scrap.
  • the temperature of the MAS water at the time of oxidizing the scrap to obtain the oxide powder that is, the temperature at the time of the oxidation reaction of the scrap may be room temperature or more, but the reaction is further accelerated. From the viewpoint, 40 to 90 ° C is preferable. Therefore, in the step (B), it is desirable to maintain the temperature of the MAS water in the above-mentioned preferable temperature range at least when oxidizing the scrap. At this time, if the temperature of the MAS 7 solution is lower than 40 ° C., the effect of promoting the reaction is small. On the other hand, if the temperature exceeds 90 ° C., no particular effect of promoting the reaction can be expected. As such a temperature maintaining means, for example, a throwing heater or direct blowing of steam is preferred because it is simple.
  • the time required for the oxidation reaction varies depending on the form of the scrap, the easiness of the oxidation / disintegration reaction, the concentration of MAS water and the temperature, etc., but is usually about 12 to 96 hours, and the size of the solid matter in the scrap It can be further or extended depending on the situation.
  • the reaction is preferably terminated at a stage where almost all the solid in the scrap collapses and the particle size of the powder contained in the precipitate becomes 1 mm or less.
  • Such a step can be easily determined, for example, by visual inspection or by searching the bottom of the container with a rod or the like.
  • the particle size of the oxide powder at the stage when the solids in the scrap have almost completely collapsed is usually several tens of meters or less, but the particle size of the powder contained in the obtained precipitate is not limited to this. .
  • the separation and recovery efficiency of useful elements is sufficient in the step (D) described below, it is not necessary to completely make the scrap into a low-level powder with a small particle size, and a solid having a particle size of about several mm or less remains. May be.
  • the oxidation Depending on the reaction time or the like, there is a possibility that a solid having such a particle size is included.
  • the step (C) of separating the precipitate containing the oxide powder obtained in the step (B) from the MAS water is performed.
  • the separation can be performed by separating a precipitate phase and an aqueous phase.
  • the separation method can be carried out by a known method such as a gradient method or a filter press method.
  • the ammonium salt of a mineral acid adsorbed on the separated precipitate can be washed with water. The precipitate after washing does not need to be particularly dried.
  • the ammonium salt of the mineral acid in the MAS 7 solution acts as a catalyst as described above, and hardly changes after the reaction in the step (B), so that the water after the separation remains unchanged or If necessary, specific gravity measurement etc. will be performed to adjust the concentration of the ammonium salt of mineral acid, and the next patch will be used for recycling.
  • the oxide powder is a powder mainly composed of an oxide and azo or hydroxide.
  • all of the iron in the scrap is iron oxyhydroxide ( FeO (OH)) and ferric hydroxide or ferric hydroxide (Fe (OH) 3 ), with more than 90% of the rare earth elements possibly contained in the powder as R (OH) 3 . Therefore, by analyzing the precipitate separated in the step (C), it can be confirmed that the precipitate obtained in the step (B) contains the desired oxide powder in the present invention.
  • the step (D) of recovering the rare earth element from the precipitate separated in the step (C) is performed.
  • the method of recovering the rare earth element from the precipitate containing the oxide powder separated in the step (C) is not particularly limited, and can be performed by referring to a known acid leaching method or the like. .
  • Leaching may be employed particularly advantageously in the present invention, but is not limited thereto.
  • the reason that such an acid leaching method is preferable is that the iron in the alloy has already been converted into iron oxyhydroxide, ferric hydroxide or the like by the step (B) in the present invention as described above. This is because when the oxide powder is subsequently reacted with an acid, elution of iron is almost completely suppressed, and the rare earth element can be selectively eluted with a small amount of acid.
  • the rare earth element is dissolved from the precipitate containing the oxide powder by the acid leaching method.
  • the rare earth compound can be recovered from the solution in which the rare earth element has been eluted by a known precipitation forming method or the like.
  • a soluble precipitation agent such as fluoride, oxalate, and carbonate is added to the scythe to form an insoluble precipitate of rare earth salts such as rare earth fluoride, rare earth oxalate, and rare earth carbonate. It can be recovered by a method of separating and drying, or a method of further baking to form a rare earth oxide.
  • the conditions of the acid leaching method and the precipitation forming method that can be employed in the step (D) are not particularly limited, and can be appropriately determined in consideration of known conditions and the like for achieving the object.
  • a precipitate containing the oxide powder obtained in the step (C) is dispersed in water, and a mineral acid such as sulfuric acid, hydrochloric acid, or nitric acid having a desired concentration is added dropwise while aeration is performed. be able to.
  • the temperature of the solution containing the precipitate at the time of the dropwise addition is at least room temperature, preferably about 40 to 60 ° C.
  • the amount and time of addition of the mineral acid can be selected as appropriate, and the end of the reaction can be determined by measuring the pH of the solution.
  • the alloy of the rare earth-transition metal alloy scrap contains other useful metals, for example, copult.
  • copult When the oxidation by MAS water in step (B) is performed, 90% by weight or more of the copult is an oxide. Since it remains in the powder, cobalt can be recovered together with the rare earth element according to the aforementioned acid leaching method that can be employed in the step (D), particularly the method described in JP-A-9-217132.
  • the step (B) of passing a gas containing oxygen through the MAS aqueous solution and oxidizing the scrap to obtain a precipitate containing a specific oxide powder is performed, so that the rare earth transition ⁇
  • Useful elements such as elements can be economically, safely, and efficiently recovered without consuming a large amount of acid and without the need for pre-sorting and pre-milling of scrap forms. .
  • Test Example 1 was repeated except that a 0.5 mol Zl aqueous solution of ammonium sulfate was used as the MAS water, and the temperature of the water was changed to 25 ° C, 40 ° C, 60 ° C, 80 ° C, and 100 ° C.
  • the scrap material which is a massive solid, was oxidized.
  • the time required for the residual ratio of the solid to become 10% or less was measured. The result is shown in figure 2.
  • the precipitate was collected by filtration from a sample that had completely collapsed by treatment at 60 ° C for 72 hours, and the powder dried at 100 ° C was examined by X-ray diffraction. The results are shown in Figure 3.
  • the generated powder has strong diffraction peaks such as Fe (OH) 3 and FeO (OH).
  • the peak of the rare earth compound is not always clear, probably due to its presence as a low crystalline hydroxide.
  • the powdered ground sludge (dry weight: 119.7 g) containing six cut-out parts (about 17 g / piece) derived from the manufacturing process of the rare earth-iron-boron based sintered magnet with the composition shown in Table 1 It was immersed in 500 ml of a 0.8 mol / l ammonium sulfate aqueous solution. Subsequently, the resultant was subjected to an oxidation treatment at 70 ° C. for 30 hours with stirring and aeration, whereby a precipitate of oxide powder was formed from the sludge. The powder of this acidified product was separated by filtration and dried to obtain 192.5 g. A part was sampled and analyzed for composition. Table 1 shows the results.
  • Table 1 shows that the obtained powder contains 98% or more of the rare earth elements in the sludge and 93% or more of Co.
  • R in Tables 1 and 2 indicates a mixture of (1, Pr and Dy, and “Others” in Table 1 indicates gas components such as oxygen, hydrogen, carbon, and sulfur.
  • a rare earth element and coparte can be selectively recovered by a precipitation generation method or a solvent extraction method performed by adding an aqueous solution of fluoride, oxalate, z-oxide, carbonate, or the like to the filtrate.
  • Example 2 350 g (dry weight: 175 g) of sludge containing grinding chips derived from the production process of the rare-earth iron-boron sintered magnet having the same composition as in Example 1 was immersed in 500 ml of a 0.2 mol / l ammonium sulfate aqueous solution. Subsequently, an oxidizing treatment was performed at 70 ° C. for 12 hours with stirring and aeration, and the generated oxide powder was filtered and separated. Next, the whole amount of the obtained oxide powder was dispersed in 200 ml of water, and a 5N aqueous nitric acid solution was added dropwise with stirring and aeration. The temperature was kept at 40-50 ° C.
  • the pH gradually decreased from around 7, and the dropping was completed when the pH reached 3.
  • the total amount dropped was 140 ml and the required time was 8 hours.
  • the precipitate was filtered, and the obtained precipitate was washed with water.
  • the filtrate and the water from which the precipitate was washed were mixed to make a nitric acid leached filtrate 1000 ml, and the filtrate was analyzed.
  • the content of the rare earth element in the sludge was 31.5 g
  • the content of the rare earth element in the filtrate for nitric acid leaching was 30.9 g
  • the recovery rate of the rare earth element was 98.0%.
  • Example 2 350 g (dry weight: 175 g) of the same sludge as used in Example 2 was not subjected to oxidation treatment with an aqueous solution of ammonium sulfate, and a 5N aqueous nitric acid solution was added dropwise while stirring and aeration. The temperature was maintained at 40-50 ° C. As the reaction progressed, the pH gradually decreased from around 11, and the dropping was completed when the pH reached 3. The total dripping amount was 300 ml and the required time was 30 hours. Next, the precipitate was filtered, and the obtained precipitate was washed with water.
  • the filtrate and the water from which the precipitate was washed were mixed together to make a nitric acid leached filtrate 1000 ml, and the filtrate was analyzed.
  • the content of the rare earth element in the sludge was 31.5 g
  • the content of the rare earth element in the nitric acid leaching filtrate was 25.2 g
  • the recovery rate of the rare earth element was 80.0%.

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Abstract

La présente invention concerne un procédé permettant de récupérer dans des rebuts de terres rares alliées à des métaux de transition un élément utile. Ce procédé enchaîne plusieurs opérations. (A) On commence par plonger dans une solution aqueuse de sel d'ammonium d'un acide minéral les chutes de l'alliage de terres rares et de métaux de transition. (B) On fait passer dans la solution un gaz oxygéné pour oxyder l'alliage et obtenir un précipité de poudre composée essentiellement d'oxydes, d'hydroxydes et analogue. (C) On filtre ensuite le précipité. Il ne reste plus qu'à (D) récupérer dans le précipité filtré les terres rares. Ce procédé permet de récupérer de façon économique et en toute sécurité des éléments utiles, et notamment des terres rares, sans consommer de grandes quantités d'acide, et ce, sans qu'il n'y ait besoin, ni d'une régulation en fonction de la forme des chutes, ni de broyage préalable.
PCT/JP2003/003238 2002-03-19 2003-03-18 Procede pour recuperer un element utile dans les rebuts de terres rares alliees a des metaux de transition WO2003078671A1 (fr)

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JP2003576661A JP4287749B2 (ja) 2002-03-19 2003-03-18 希土類−遷移金属合金スクラップからの有用元素の回収方法
AU2003221047A AU2003221047A1 (en) 2002-03-19 2003-03-18 Method for recovering useful element from rare earth - transition metal alloy scrap

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JP2002-76054 2002-03-19
JP2002076054 2002-03-19

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RU2469116C1 (ru) * 2011-03-14 2012-12-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Национальный исследовательский ядерный университет "МИФИ" Способ переработки шлифотходов от производства постоянных магнитов
RU2574543C1 (ru) * 2014-11-17 2016-02-10 Открытое акционерное общество "Ведущий научно-исследовательский институт химической технологии" Способ переработки шлифотходов от производства постоянных магнитов
JP2017115175A (ja) * 2015-12-21 2017-06-29 トヨタ自動車株式会社 希土類磁石から希土類元素を回収する方法
KR101867739B1 (ko) * 2016-12-23 2018-06-15 주식회사 포스코 Ni 농축액을 제조하는 방법
JP2020125521A (ja) * 2019-02-05 2020-08-20 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
US11155898B2 (en) * 2016-06-03 2021-10-26 Brgm Method for extracting rare earth elements contained in permanent magnets
JP2022060262A (ja) * 2019-02-05 2022-04-14 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
US11764416B2 (en) 2019-08-02 2023-09-19 Iowa State Univerity Research Foundation, Inc. Chemical dismantling of permanent magnet material and battery material

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US8940256B2 (en) * 2011-12-07 2015-01-27 Xylon Technical Ceramics, Inc. Method for recycling of rare earth and zirconium oxide materials
CN104169471A (zh) 2012-07-19 2014-11-26 吉坤日矿日石金属株式会社 从含稀土元素合金回收稀土元素的方法
CN104232905B (zh) * 2014-06-16 2015-08-12 赣州力赛科新技术有限公司 一种含有高价值元素氢氧化铁基原料及其用途
CN115261610B (zh) * 2022-08-03 2023-08-22 中国科学院赣江创新研究院 一种分离废旧镍氢电池中稀土元素与过渡金属元素的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62187112A (ja) * 1986-02-13 1987-08-15 Santoku Kinzoku Kogyo Kk 希土類元素・鉄系磁石材料から希土類元素を回収する方法
JPS634028A (ja) * 1986-06-23 1988-01-09 Sumitomo Metal Mining Co Ltd 希土類と鉄を含有するスクラツプの処理方法
JPH0514777B2 (fr) * 1985-10-08 1993-02-25 Santoku Metal Ind
JPH0790394A (ja) * 1993-09-22 1995-04-04 Sumitomo Metal Ind Ltd フェロスクラップの脱亜鉛方法とその装置
EP0790321A1 (fr) * 1996-02-13 1997-08-20 Santoku Metal Industry Co., Ltd. Procédé de récupération des espèces réutilisables à partir de déchets d'alliages de terres rares et de fer

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86101311A (zh) * 1986-06-06 1988-02-17 李久成 从酸碱性岩浆岩风化壳或离子吸附型稀土矿中提炼铷铯工艺方案
JPH0772312B2 (ja) * 1991-05-17 1995-08-02 住友金属鉱山株式会社 希土類元素の回収方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0514777B2 (fr) * 1985-10-08 1993-02-25 Santoku Metal Ind
JPS62187112A (ja) * 1986-02-13 1987-08-15 Santoku Kinzoku Kogyo Kk 希土類元素・鉄系磁石材料から希土類元素を回収する方法
JPS634028A (ja) * 1986-06-23 1988-01-09 Sumitomo Metal Mining Co Ltd 希土類と鉄を含有するスクラツプの処理方法
JPH0790394A (ja) * 1993-09-22 1995-04-04 Sumitomo Metal Ind Ltd フェロスクラップの脱亜鉛方法とその装置
EP0790321A1 (fr) * 1996-02-13 1997-08-20 Santoku Metal Industry Co., Ltd. Procédé de récupération des espèces réutilisables à partir de déchets d'alliages de terres rares et de fer

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RU2469116C1 (ru) * 2011-03-14 2012-12-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Национальный исследовательский ядерный университет "МИФИ" Способ переработки шлифотходов от производства постоянных магнитов
RU2574543C1 (ru) * 2014-11-17 2016-02-10 Открытое акционерное общество "Ведущий научно-исследовательский институт химической технологии" Способ переработки шлифотходов от производства постоянных магнитов
JP2017115175A (ja) * 2015-12-21 2017-06-29 トヨタ自動車株式会社 希土類磁石から希土類元素を回収する方法
US11155898B2 (en) * 2016-06-03 2021-10-26 Brgm Method for extracting rare earth elements contained in permanent magnets
KR101867739B1 (ko) * 2016-12-23 2018-06-15 주식회사 포스코 Ni 농축액을 제조하는 방법
JP2020125521A (ja) * 2019-02-05 2020-08-20 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
JP7044082B2 (ja) 2019-02-05 2022-03-30 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
JP2022060262A (ja) * 2019-02-05 2022-04-14 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
JP7151916B2 (ja) 2019-02-05 2022-10-12 信越化学工業株式会社 酸性スラリーの製造方法及び希土類元素の回収方法
US11764416B2 (en) 2019-08-02 2023-09-19 Iowa State Univerity Research Foundation, Inc. Chemical dismantling of permanent magnet material and battery material

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CN1656239A (zh) 2005-08-17

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