JP6187768B2 - Recovery method of rare earth elements - Google Patents
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Description
本発明は、希土類磁石のように希土類元素と鉄を含む原料から鉄を効率よく分離して希土類元素を回収する方法に関する。 The present invention relates to a method for recovering rare earth elements by efficiently separating iron from a raw material containing rare earth elements and iron such as rare earth magnets.
希土類磁石は希土類元素を多く含むので、その廃棄物から希土類元素が回収されている。希土類磁石のうち、ネオジム磁石はＮｄ2Ｆｅ14Ｂを主成分としており、ネオジムと共に鉄を含んでいる。また、サマリウム鉄窒素磁石にも鉄が含まれている。このような希土類元素と鉄の合金から希土類元素を選択的に回収するには、共存する鉄を効率よく分離する必要がある。 Since rare earth magnets contain a large amount of rare earth elements, rare earth elements are recovered from the waste. Among rare earth magnets, neodymium magnets are mainly composed of Nd 2 Fe 14 B and contain iron together with neodymium. Samarium iron nitrogen magnets also contain iron. In order to selectively recover a rare earth element from such a rare earth element and iron alloy, it is necessary to efficiently separate the coexisting iron.
例えば、ネオジム鉄ホウ素合金（ネオジム磁石）から鉄を分離して希土類元素のネオジムを選択的に回収する方法として酸化ホウ素を用いる処理方法が知られている（特許文献１）。この方法は、希土類合金を酸化ホウ素と混合して溶融すると、溶融した希土類元素が酸化ホウ素と反応して希土類元素だけが酸化物になってガラススラグに移動し、鉄およびホウ素は合金中に残るので、希土類元素をガラススラグと共に回収する方法である。しかし、この方法は、ガラススラグを回収した後に該ガラススラグから希土類元素を取り出す手間がかかる。 For example, as a method for selectively recovering rare earth neodymium by separating iron from a neodymium iron boron alloy (neodymium magnet), a treatment method using boron oxide is known (Patent Document 1). In this method, when a rare earth alloy is mixed with boron oxide and melted, the molten rare earth element reacts with boron oxide, and only the rare earth element becomes an oxide and moves to glass slag, and iron and boron remain in the alloy. Therefore, it is a method of collecting rare earth elements together with glass slag. However, this method requires time and effort to extract rare earth elements from the glass slag after the glass slag is recovered.
また、希土類元素を含む原料を酸化焙焼する処理方法が知られている（特許文献２）。この方法は、希土類磁石合金を含む原料を空気中で焙焼して合金成分を酸化物にし、これに水を加えてスラリーにし、塩酸を加えて希土類元素を選択的に溶解し、多くの酸化鉄を未溶解のまま残して希土類元素の浸出液を回収し、この溶液にアルカリを加えて溶解した鉄を水酸化物にして沈殿させて分離する方法である。
しかし、この方法は焙焼温度を８００℃程度にする必要があり、さらに、水酸化鉄を生成させるためアルカリの添加が必要であり、処理コストがかかる。
Moreover, the processing method of oxidizing and baking the raw material containing rare earth elements is known (patent document 2). In this method, a raw material containing a rare earth magnet alloy is roasted in the air to convert the alloy components into oxides, to which water is added to form a slurry, hydrochloric acid is added to selectively dissolve the rare earth elements, and a large amount of oxidation. In this method, the leachate of rare earth elements is recovered while leaving the iron undissolved, and the dissolved iron is added to the solution to form a hydroxide, which is then precipitated and separated.
However, this method requires a roasting temperature of about 800 ° C., and further requires addition of an alkali to generate iron hydroxide, which increases the processing cost.
この他に、希土類磁石屑を硫酸浸出する処理方法が知られている（特許文献３，４，５、６）。特許文献３の方法は、希土類磁石屑を硫酸に溶解し、不溶分を除去した溶解液にアンモニア水を加えて希土類硫酸アンモニウム塩を析出させ、これを１３８０℃以上で焼成して希土類元素酸化物にして回収する方法である。
特許文献４、６の方法は、希土類磁石屑を硫酸に溶解した液に還元剤を加えｐＨ５以下にして鉄の析出を抑制しつつ希土類元素硫酸塩を析出させ、固液分離して液分に含まれる鉄を分離し、希土類元素硫酸塩を回収する方法である。
特許文献５の方法は、希土類磁石屑を硫酸に溶解し、液に酸化物を加えて酸化還元電位を調整して希土類元素沈殿を形成し、これを回収して再溶解した液にシュウ酸を加えて希土類元素シュウ酸塩を回収する方法である。
これらの方法は何れも、希土類磁石屑の硫酸溶解液から希土類元素を固形分にして鉄を含む液分を分離する方法であり、液分に含まれる鉄を廃棄するため固形分にする手間がかかる。また希土類を含有する固形分から希土類を取り出す手間がかかる。
In addition, a processing method for leaching rare earth magnet scraps with sulfuric acid is known (
In the methods of Patent Documents 4 and 6, a reducing agent is added to a solution obtained by dissolving rare earth magnet scraps in sulfuric acid, and the pH is adjusted to 5 or less to precipitate the rare earth element sulfate while suppressing the precipitation of iron. In this method, the iron contained is separated and the rare earth element sulfate is recovered.
In the method of Patent Document 5, rare earth magnet scraps are dissolved in sulfuric acid, an oxide is added to the liquid to adjust the redox potential to form a rare earth element precipitate, and this is recovered and re-dissolved with oxalic acid in the liquid. In addition, it is a method for recovering rare earth element oxalate.
Each of these methods is a method of separating a liquid component containing iron from a rare earth magnet scrap sulfuric acid solution by solidifying the rare earth element into a solid content. Take it. Moreover, it takes time and effort to extract the rare earth from the solid content containing the rare earth.
本発明は、従来技術の上記問題を解決した処理方法であり、希土類元素と鉄を含む原料から鉄を固形分として分離し、希土類元素を含む浸出液を回収する処理方法を提供する。本発明によれば鉄の分離と後処理が容易であり、希土類元素を効率よく回収することができる。 The present invention is a treatment method that solves the above-mentioned problems of the prior art, and provides a treatment method for separating iron as a solid content from a raw material containing rare earth elements and iron and recovering a leachate containing rare earth elements. According to the present invention, iron can be easily separated and post-treated, and rare earth elements can be efficiently recovered.
〔１〕希土類元素と鉄を含む原料を粉砕し、硫酸を加えてスラリーにして希土類元素と鉄を硫酸塩にし、次いで該スラリーを乾燥した後に、希土類元素の硫酸塩を残して鉄の硫酸塩が分解し酸化鉄になる温度に加熱し、さらに該焙焼物を水に混合して希土類元素を浸出させる一方、固形分の酸化鉄を残渣として分離して希土類元素の浸出液を回収することを特徴とする希土類元素の回収方法。
〔２〕希土類元素と鉄を含む原料としてネオジム磁石屑を用い、該ネオジム磁石屑を１.５mm以下に粉砕し、この粉砕物に、希土類元素および鉄分に対して０.８５〜１.３当量の硫酸を加えてスラリーにし、希土類元素と鉄の硫酸塩を生成させる上記[１]に記載する希土類元素の回収方法。
〔３〕原料の粉砕物に硫酸と共に水を加えて希土類元素および鉄の硫酸塩を生成させる上記[１]または上記[２]に記載する希土類元素の回収方法。
〔４〕上記スラリーを乾燥した後に、空気下で６５０℃〜７５０℃の温度に加熱し、希土類元素の硫酸塩を残し、硫酸鉄を分解して酸化鉄にする上記[１]〜上記[３]の何れかに記載する希土類元素の回収方法。
〔５〕上記焙焼物を水に混合し、室温で撹拌溶解した後、固液分離して希土類元素含有の硫酸溶液を回収する上記[１]〜上記[４]何れかに記載する希土類元素の回収方法。
[1] A raw material containing rare earth elements and iron is pulverized, and sulfuric acid is added to make a slurry to make rare earth elements and iron sulfate. Then, the slurry is dried, and then the sulfate of iron is left leaving the rare earth element sulfate. Is heated to a temperature at which it decomposes into iron oxide, and the roasted product is further mixed with water to leach rare earth elements, while solid iron oxide is separated as a residue to collect the rare earth element leachate. A method for recovering rare earth elements.
[2] Using neodymium magnet scrap as a raw material containing rare earth element and iron, pulverizing the neodymium magnet scrap to 1.5 mm or less, and adding 0.85 to 1.3 equivalents to the pulverized product with respect to the rare earth element and iron content. The method for recovering a rare earth element according to the above [1], wherein the sulfuric acid is added to form a slurry to produce a sulfate of the rare earth element and iron.
[3] The method for recovering a rare earth element according to the above [1] or [2], wherein water is added to the pulverized raw material together with sulfuric acid to generate a rare earth element and iron sulfate.
[4] After the slurry is dried, the slurry is heated to a temperature of 650 ° C. to 750 ° C. under air to leave a sulfate of rare earth elements and decompose iron sulfate into iron oxide. The method for recovering rare earth elements according to any one of the above.
[5] The roasted product is mixed with water, stirred and dissolved at room temperature, and then solid-liquid separated to recover a rare earth element-containing sulfuric acid solution. The rare earth element according to any one of the above [1] to [4] Collection method.
〔具体的な説明〕
本発明の希土類元素回収方法は、希土類元素と鉄を含む原料を粉砕し、硫酸を加えてスラリーにして希土類元素と鉄を硫酸塩にし、次いで該スラリーを乾燥した後に、希土類元素の硫酸塩を残して鉄の硫酸塩が分解し酸化鉄になる温度に加熱し、さらに該焙焼物を水に混合して希土類元素を浸出させる一方、不溶性の酸化鉄を残渣として分離して希土類元素の浸出液を回収することを特徴とする希土類元素の回収方法である。
本発明の希土類元素回収方法の処理工程を図１に示す。
[Specific description]
In the rare earth element recovery method of the present invention, a raw material containing a rare earth element and iron is pulverized, and sulfuric acid is added to form a slurry to form a rare earth element and iron sulfate, and then the slurry is dried. The iron sulfate is left to decompose and heated to iron oxide, and the roasted product is mixed with water to leach rare earth elements, while insoluble iron oxide is separated as a residue to separate the rare earth element leachate. A method for recovering rare earth elements characterized by recovering.
The processing steps of the rare earth element recovery method of the present invention are shown in FIG.
本発明の回収方法において、希土類元素と鉄を含む原料として、例えば、ネオジム磁石屑（Ｎｄ2Ｆｅ14Ｂ）などを用いることができる。該原料を粗粉砕してスクリーンに通し、磁石表面のニッケル箔などを除去する。原料を粗粉砕した後にさらに０.５ｍｍ以下に粉砕して硫酸との反応性を高めると良い。 In the recovery method of the present invention, for example, neodymium magnet scrap (Nd 2 Fe 14 B) can be used as a raw material containing rare earth elements and iron. The raw material is coarsely pulverized and passed through a screen to remove nickel foil and the like on the magnet surface. After roughly pulverizing the raw material, it may be further pulverized to 0.5 mm or less to increase the reactivity with sulfuric acid.
〔硫酸塩工程〕
粉砕した原料を硫酸に加え混錬してスラリーにする。この硫酸スラリーにおいて、原料中の鉄分および希土類元素は硫酸と反応して硫酸塩〔ＦｅＳＯ4，Ｆｅ2(ＳＯ4)3、Ｎｄ2(ＳＯ4)3等〕になる。
[Sulfate process]
The pulverized raw material is added to sulfuric acid and kneaded to make a slurry. In this sulfuric acid slurry, iron and rare earth elements in the raw material react with sulfuric acid to become sulfates [FeSO 4 , Fe 2 (SO 4 ) 3 , Nd 2 (SO 4 ) 3, etc.].
硫酸の添加量は原料中の希土類元素および鉄分に対して０.８５〜１.３当量が好ましい。硫酸の添加量が０.８５当量より少ないと鉄および希土類元素の硫酸塩の生成が不十分になる。一方、硫酸の添加量が１.３当量を超えても希土類元素の浸出率は増加しない。 The amount of sulfuric acid added is preferably 0.85 to 1.3 equivalents relative to the rare earth element and iron content in the raw material. When the addition amount of sulfuric acid is less than 0.85 equivalent, the formation of sulfates of iron and rare earth elements becomes insufficient. On the other hand, even if the addition amount of sulfuric acid exceeds 1.3 equivalents, the leaching rate of rare earth elements does not increase.
原料の粉砕物に硫酸と共に水を加えると硫酸塩の生成反応が激しく進行し、短時間で硫酸塩が生成する。水の添加量は原料の２倍程度の重量が好ましい。 When water is added to the pulverized raw material together with sulfuric acid, the sulfate formation reaction proceeds vigorously, and sulfate is formed in a short time. The amount of water added is preferably about twice the weight of the raw material.
〔酸化焙焼工程〕
原料と硫酸の混合スラリーを乾燥して水分と硫酸を揮発させ、この乾燥物を空気下で加熱して酸化焙焼する。焙焼温度は希土類元素の硫酸塩が残り、鉄の硫酸塩が分解して酸化鉄になる温度である。具体的には、空気下で６５０℃〜７５０℃の温度で１〜２時間加熱すると良い。
[Oxidation roasting process]
The mixed slurry of raw material and sulfuric acid is dried to volatilize moisture and sulfuric acid, and this dried product is heated in the air and oxidized and roasted. The roasting temperature is the temperature at which the rare earth element sulfate remains and the iron sulfate decomposes to iron oxide. Specifically, it may be heated at a temperature of 650 ° C. to 750 ° C. for 1 to 2 hours under air.
上記温度下の焙焼において、希土類元素の硫酸塩の大部分は分解せずに残り、硫酸鉄は分解して酸化鉄になる。発生したＳＯ3ガスは系外に導かれる。 In the baking at the above temperature, most of the rare earth element sulfate remains without being decomposed, and the iron sulfate is decomposed into iron oxide. The generated SO 3 gas is led out of the system.
このように、原料に含まれる鉄分を硫酸塩にしてから６５０℃〜７５０℃の加熱温度で焙焼することによって、希土類元素の硫酸塩を残し、鉄分を十分に酸化することができる。最初から原料を酸化焙焼する従来の処理方法（特許文献２）では、金属鉄が残留しないように８００℃以上の高温に加熱しているが、本発明の回収方法では従来の加熱温度よりも大幅に低い温度で焙焼することによって鉄分を全て酸化鉄にすることができる。 As described above, the iron contained in the raw material is sulfated and then roasted at a heating temperature of 650 ° C. to 750 ° C., thereby leaving the rare earth element sulfate and sufficiently oxidizing the iron. In the conventional processing method (Patent Document 2) in which the raw material is oxidized and roasted from the beginning, it is heated to a high temperature of 800 ° C. or higher so that metallic iron does not remain. By roasting at a significantly lower temperature, all iron can be converted to iron oxide.
〔水浸出工程〕
上記焙焼物を水に混合してスラリーする。焙焼物に含まれる希土類元素の硫酸塩は水溶性であるので室温で、使用した原料の２倍量の水に溶解する。一方、酸化鉄は不溶性であるので固形分として残る。このスラリーを固液分離して希土類元素浸出液を回収し、酸化鉄を残渣として除去する。
[Water leaching process]
The roasted product is mixed with water and slurried. Since the rare earth element sulfate contained in the baked product is water-soluble, it dissolves in water twice as much as the raw material used at room temperature. On the other hand, iron oxide remains insoluble because it is insoluble. This slurry is subjected to solid-liquid separation to recover a rare earth element leachate, and iron oxide is removed as a residue.
本発明の回収方法は、原料に含まれる希土類元素と鉄分を硫酸塩にした後に酸化焙焼するので、従来の処理方法よりも格段に低い温度で鉄分を酸化鉄に分解することができる。
本発明の回収方法では原料に含まれる鉄分を固形分（酸化鉄）にして分離することができるので、鉄分の後処理が容易であり、また、希土類元素は浸出液として回収することができるので、希土類金属の回収工程が容易になる。
In the recovery method of the present invention, since the rare earth elements and iron contained in the raw material are sulfated and then oxidized and roasted, the iron can be decomposed into iron oxide at a temperature much lower than that of the conventional treatment method.
In the recovery method of the present invention, the iron content contained in the raw material can be separated into a solid content (iron oxide), so that the post-treatment of the iron content is easy, and the rare earth element can be recovered as a leachate. The recovery process of rare earth metal is facilitated.
本発明の実施例を以下に示す。液中の希土類元素と鉄の濃度はＩＣＰによって測定した。硫酸の当量はＮｄ2(ＳＯ4)3,Ｄｙ2(ＳＯ4)3,Ｆｅ2(ＳＯ4)3に基づいて算出した。 Examples of the present invention are shown below. The concentrations of rare earth elements and iron in the liquid were measured by ICP. Equivalent of sulfuric acid was calculated based on the Nd 2 (SO 4) 3, Dy 2 (SO 4) 3, Fe 2 (SO 4) 3.
〔実施例１〕
希土類磁石屑４ｇ（Ｎｄ:２０wt％、Ｄｙ:１０wt％、Ｆｅ：６８wt％）を粗粉砕して磁石表面のニッケル箔を除去した後に１.５mm以下に粉砕し、この粉砕物に、０.２０〜１.２８当量の硫酸（硫酸濃度９８wt％）を加え、一部の試料には硫酸と共に水を加えて撹拌し、硫酸スラリーにした。この硫酸スラリーを１５０℃に加熱して乾燥し、水分を除去した後に、空気下で６８０℃に１.５時間加熱して焙焼した。この焙焼物を５０ｇの水に混合し撹拌して水スラリーにした。この水スラリーを１０分後に固液分離して浸出液を回収した。浸出液に含まれる希土類元素と鉄の浸出率を表１に示す。浸出率は原料中の含有量に対する浸出液中の含有量より求めた。
[Example 1]
4 g of rare earth magnet scraps (Nd: 20 wt%, Dy: 10 wt%, Fe: 68 wt%) were coarsely pulverized to remove the nickel foil on the magnet surface, and then pulverized to 1.5 mm or less. ˜1.28 equivalent of sulfuric acid (sulfuric acid concentration 98 wt%) was added, and water was added to some samples together with sulfuric acid and stirred to form a sulfuric acid slurry. The sulfuric acid slurry was heated to 150 ° C. and dried to remove moisture, and then heated to 680 ° C. for 1.5 hours under air to be baked. This roasted product was mixed with 50 g of water and stirred to form a water slurry. This water slurry was subjected to solid-liquid separation after 10 minutes to recover the leachate. Table 1 shows the leaching rates of rare earth elements and iron contained in the leachate. The leaching rate was determined from the content in the leachate relative to the content in the raw material.
表１に示すように、原料の希土類磁石屑に含まれる希土類元素の殆どが水に浸出される。一方、浸出液の鉄濃度は極めて低く、鉄分は残渣に分離されている。また、硫酸の添加量の増加とともに浸出率も増加しており、硫酸の添加量は１.３当量程度が好ましい。 As shown in Table 1, most of the rare earth elements contained in the raw rare earth magnet scraps are leached into water. On the other hand, the iron concentration of the leachate is extremely low, and the iron content is separated into residues. In addition, the leaching rate increases as the amount of sulfuric acid added increases, and the amount of sulfuric acid added is preferably about 1.3 equivalents.
〔実施例２〕
実施例１の試料No.３と同様の硫酸スラリーについて、乾燥後、空気下で６００℃、６５０℃、７５０℃に１.５時間加熱した。この焙焼物を５０ｇの水に混合し撹拌して水スラリーにした。この水スラリーを１０分後に固液分離して浸出液を回収した。浸出液に含まれる希土類元素と鉄の浸出率を表２に示す。
[Example 2]
About the sulfuric acid slurry similar to sample No. 3 of Example 1, after drying, it heated at 600 degreeC, 650 degreeC, and 750 degreeC under air for 1.5 hours. This roasted product was mixed with 50 g of water and stirred to form a water slurry. This water slurry was subjected to solid-liquid separation after 10 minutes to recover the leachate. Table 2 shows the leaching rates of rare earth elements and iron contained in the leachate.
表２に示すように、６５０℃〜７５０℃に加熱することによって硫酸鉄の殆どが酸化鉄になるため浸出し難く、浸出液の鉄濃度が低いことが確認された。一方、焙焼温度が６００℃では硫酸鉄の分解が不十分になり、浸出液の鉄濃度が高くなる。 As shown in Table 2, it was confirmed that by heating to 650 ° C. to 750 ° C., most of the iron sulfate becomes iron oxide, so that it is difficult to be leached and the iron concentration of the leaching solution is low. On the other hand, when the roasting temperature is 600 ° C., the decomposition of iron sulfate becomes insufficient, and the iron concentration of the leachate becomes high.
〔比較例１〕
実施例１と同様の希土類磁石屑４ｇを粉砕した後に、空気下で６５０℃に１.５時間加熱して酸化焙焼した。この焙焼物に硫酸１L/kg（０.８５当量）と水５０ｍｌを加えてスラリーにし、室温で撹拌した。３時間経過後に固液分離して浸出液を回収した。浸出液の希土類元素、鉄の浸出率を測定したところ、Ｎｄ：５８wt％、Ｄｙ：５５wt％、Ｆｅ：６６wt％であった。
[Comparative Example 1]
After crushing 4 g of the rare earth magnet scrap similar to that in Example 1, it was heated to 650 ° C. under air for 1.5 hours for oxidation roasting. 1 L / kg (0.85 equivalent) of sulfuric acid and 50 ml of water were added to the baked product to make a slurry, and the mixture was stirred at room temperature. After 3 hours, the liquid was separated and the leachate was collected. When the leaching rate of rare earth elements and iron in the leachate was measured, they were Nd: 58 wt%, Dy: 55 wt%, and Fe: 66 wt%.
Claims (5)
The raw material containing rare earth elements and iron is pulverized, and sulfuric acid is added to make a slurry to make the rare earth elements and iron sulfate, and then the slurry is dried, and then the iron sulfate is decomposed leaving the rare earth element sulfate. Heating to a temperature at which it becomes iron oxide, and further mixing the roasted material with water to leach rare earth elements, while separating solid iron oxide as a residue and recovering a rare earth element leachate Element recovery method.
Neodymium magnet scrap is used as a raw material containing rare earth element and iron, the neodymium magnet scrap is pulverized to 1.5 mm or less, and 0.85-1.3 equivalent of sulfuric acid is added to the pulverized product with respect to the rare earth element and iron content. The method for recovering a rare earth element according to claim 1, further comprising forming a slurry of the rare earth element and iron by forming a slurry.
The method for recovering a rare earth element according to claim 1 or 2, wherein water is added to the pulverized raw material together with sulfuric acid to produce a rare earth element and iron sulfate.
The slurry is dried and then heated under air to a temperature of 650 ° C to 750 ° C. By this roasting, rare earth element sulfate is left and iron sulfate is decomposed into iron oxide. 4. The method for recovering rare earth elements according to any one of 3).
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| CN114737049A (en) * | 2021-12-27 | 2022-07-12 | 包头华美稀土高科有限公司 | Method for removing phosphorus in rare earth leaching solution |
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| JP2765740B2 (en) * | 1990-01-10 | 1998-06-18 | 日立粉末冶金株式会社 | Separation and recovery of rare earth elements from raw materials containing rare earth elements and iron |
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