JPS58193331A - Treatment of alloy power of rare earth element-cobalt - Google Patents

Abstract

PURPOSE:To make it possible to separate and recover a high grade rare earth element and Co, by a method wherein an acid or an aqueous solution thereof is added to the mechanically processed powder of a rare earth element-cobalt alloy and chemical reaction is generated to separate the reaction mixture into a rare earth element-rich precipitate and a Co ion-rich solution. CONSTITUTION:A mechanically processed powder such as a shaved powder or a cut powder generated during the processing a parmanent magnet comprising a rare earth element - Co alloy RCo (wherein R is one kind or more rare earth element including Y) and conventionally thought impossible in the utilization thereof is treated as mentioned below. That is, an acid such as hydrochloric acid or oxalic acid or an aqueous solution thereof is added to the above mentioned processed powder and chemical reaction is generated to separate the reaction mixture into a R element rich precipitate and a Co element ion solution.

Description

【発明の詳細な説明】 本発明はＲＣｏ希土類コバルト合金の機械加工によシ出
る粉からＲ元素お↓ひＣｏ７ｃｌＫを回収するための処
理方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a processing method for recovering the R element ↓Co7clK from the powder produced during machining of an RCo rare earth cobalt alloy.

ＲＣｏ希土類コバルト合金（ＲはＹ’Ｊ−富む１種類以
上の希土類金属元Ｘ）は、従来のアルニコ研石、フェラ
イト磁石をしのぐ高い磁気特性ｔＭすることから第５の
永久磁石として注目され、その生産高は年々増加しつつ
ある。その代表的なものはＲＣｏ、。RCo rare earth cobalt alloy (R is Y'J - rich in one or more rare earth metal elements Production volume is increasing year by year. A typical example is RCo.

Ｒ宜Ｃｏｔｙ合金（あるいは金属間化合物）である。It is a Coty alloy (or intermetallic compound).

現在種々の改良の結果、ＲＣｏ希土類コバルト合金永久
磁石の磁気％性は、最大エネルギー棟が３０ＭＧ・０６
以上に達するもの、あるいは、保磁力が５０ＫＯｅ以上
に達するものが報告され、またその一部が量産されてい
る。この意味で現在のＲＣｏ希土類コバルト合金永久出
石磁石磁気特性的には需要各分野からの要求ｔはぼ満足
するレベルに達していると１りても過言ではない。Currently, as a result of various improvements, the magnetic % of RCo rare earth cobalt alloy permanent magnet has a maximum energy of 30MG・06
It has been reported that magnets with a coercive force of 50 KOe or more have been reported, and some of them are being mass-produced. In this sense, it is no exaggeration to say that the magnetic properties of current RCo rare earth cobalt alloy permanent magnets have reached a level that almost satisfies the demands t from various fields of demand.

一万このＲＣｏ希土類コバルト合金永久磁石磁石上の主
成分がきわめて高価なＲ元素、Ｃｏ元素であることから
必然的にその製造原価および製品価格が！　米のアルニ
コ磁石、フェライト磁石に比べ高価となり、このことが
改善されれはそのｉ％ｉ［ｉａ気特性と相まってＲＣｏ
希土類コバルト合金永久磁石の需要が飛躍的に増大する
ものである。10,000 Since the main components of this RCo rare earth cobalt alloy permanent magnet are the extremely expensive R and Co elements, the manufacturing cost and product price are inevitably high! They are more expensive than American alnico magnets and ferrite magnets, and if this is improved, combined with their i%i
Demand for rare earth cobalt alloy permanent magnets will increase dramatically.

従来ＲＣｏ希土類コバルト合金永久磁七のｌ１１！造原
価を低減するため、Ｒ２Ｏ素の種類、Ｒ２Ｏ素とＣｏ元
素の比率、他の絵肌物元索のａｉ加等の組成的な面での
検討ならひに成形、焼結、熱処理、加工等の製造プロセ
ス的な面での検討が種々なされて睡た。Conventional RCo rare earth cobalt alloy permanent magnetic 7 l11! In order to reduce manufacturing costs, we consider compositional aspects such as the type of R2O element, the ratio of R2O element and Co element, and the addition of AI to other Ehadamono elements, including molding, sintering, heat treatment, and processing. Various studies have been conducted on manufacturing process aspects such as:

し〃１し必要磁気特性上の制約からこれらの検討にはお
のづから限界があり、画期的な製造原価の低減となって
いないのが実状である。However, due to constraints on the required magnetic properties, these studies have their own limits, and the reality is that they have not resulted in an epoch-making reduction in manufacturing costs.

本発明名らはＢＣＯ希土類コバルト合金永久磁石の裂ｍ
原価低減のため、従来利用不可耗と考えられてい７ｊＲ
Ｃｏ希土類コバルト合金永久磁６の加工時に発生する研
削粉、切削粉、切断粉等の機械加工粉に注目し、種々の
実験の結果これを酸、アルカリ等で化学処理することに
よジＲ元素およびＣｏ元素を分離、回収することが司耗
であることｔ見いだした。The name of the present invention is BCO rare earth cobalt alloy permanent magnet crack m
In order to reduce costs, 7jR, which was previously considered to be unusable,
We focused on machining powder such as grinding powder, cutting powder, and cutting powder generated during processing of Co rare earth cobalt alloy permanent magnet 6, and as a result of various experiments, di-R elements were produced by chemically treating it with acid, alkali, etc. It has been found that separating and recovering the Co element and Co element is a waste.

８Ｃｏ希土類コバルト合金永久磁石會最＃１！製品寸法
に仕上けるにｆｌ　＠　Ｑｌｊ　、切１ｉＪｌｊ、９］
断等の機械加工は不可避であり、その工程において研削
粉、切削粉、切断粉等の機械加工粉が発生する。そして
これら機械加工粉の主成分はＲ２Ｏ素とＣｏｙｒ：累で
ある。8Co Rare Earth Cobalt Alloy Permanent Magnet Society #1! To finish to product dimensions, fl @ Qlj, cut 1iJlj, 9]
Machining such as cutting is unavoidable, and machining powder such as grinding powder, cutting powder, and cutting powder is generated in the process. The main components of these machining powders are R2O and Coyr.

発生機械加工粉の量は製品形状、加工方法等の条件によ
って異なるが一般的には総原料投入量の２０〜ＡＯＭＭ
％であると考えられる。The amount of mechanical processing powder generated varies depending on conditions such as product shape and processing method, but generally it is 20 to AOMM of the total raw material input.
%.

従ってこれら機械加工粉〃為らＲ元素、Ｃｏ元素か分離
、回部可能であり、またこれらが再利用可能であるなら
ば、省資源に寄与すると共に原料費の低減となシその結
果大幅な製造原価の低減が期待されることは盲うまでも
ない。Therefore, if the R element and Co element can be separated and recycled from these mechanically processed powders, and if they can be reused, it will contribute to resource conservation and reduce raw material costs. It goes without saying that a reduction in manufacturing costs is expected.

しかしながら、これらの機械加工粉には主成分であるＲ
２Ｈ索、Ｃｏ元素以外に加工時に混入する機　１ｊ械油
、肩愼浴媒、接層剤、砥石粉などの不純物が多量に介在
する。また＠械刀ロエ粉の主成分であるＲ２Ｏ素、Ｃ０
７Ｃ累は〃ロエ時に受ける加工摩擦熱あるいは加工時に
使用する冷却水によシその大部分が酸化されている。こ
のような理由から従来これらの機械加工粉を再処理し、
工業的に使用し得る品位のＲ元素、Ｃ０７Ｃ索を分陥回
枢することは不司乾かあるいは経済的オリ点が無いと考
えられ、これら機械加工粉り放置されているのが実状で
ある。However, these mechanically processed powders contain R, which is the main component.
In addition to the 2H wire and the Co element, there are a large amount of impurities that are mixed in during processing, such as machine oil, bath medium, coating agent, and grindstone powder. In addition, R2O element, which is the main component of Machito Loe powder, C0
Most of 7C is oxidized by the processing friction heat received during rolling or the cooling water used during processing. For this reason, conventionally these machined powders are reprocessed,
It is thought that it is unwise or economically unwise to convert industrially usable grade R element and C07C cables, and the reality is that they are left unprocessed.

本発明に、ＲＣｏ希土類コバルト合金の研削粉、切削粉
および切断粉等の機械加工により出る粉から、工業的に
使用し得る品位のＲ２Ｈ索とＣｏ元素會分際、回収する
処理方法上提供することを目的とするものである。The present invention provides a processing method for recovering industrially usable grade R2H cable and Co element from powder generated by machining such as grinding powder, cutting powder, and cutting powder of RCo rare earth cobalt alloy. The purpose is to

本発明は、ＲＣｏ希土類コバルト合金の研削粉、切削粉
および切ｌ１ｉｌ′ｒ８等の機械力ロエ粉を塩酸、蓚酸
等の酸又はその水浴液で処理して冨Ｒ７Ｃ索沈ｌＲｗＩ
Ｊと冨Ｃｏ元票イオン溶液に分離し、さらに分離された
冨Ｒ７Ｃ累沈ｌ！ｉ物、■ＣｏＣｏ元素イオン溶液々に
水酸化ナト１」ラム水溶液、炭酸ナトリウム水浴液等の
アルカリ水溶液あるい仁蓚酸等の酸又ねその水溶ｇ盆硝
加して、Ｒ７ｃ累、　Ｃｏ元素のアルカリま友は酸との
化合物を生成せしめ、この生成化合物を焼成してＲ７Ｃ
累酸化物、Ｃｏ元素酸化物を得ることを［ｋとするもの
である。In the present invention, grinding powder of RCo rare earth cobalt alloy, cutting powder and mechanical powder such as cutting l1il'r8 are treated with an acid such as hydrochloric acid or oxalic acid or a water bath solution thereof to produce a rich R7C cable precipitate lRwI.
J and Tomi Co are separated into ion solution, and further separated Tomi R7C sedimentation l! ■ To the CoCo element ion solution, add a sodium hydroxide solution, an alkaline aqueous solution such as a sodium carbonate water bath solution, an acid such as oxalic acid, or an aqueous solution of oxalic acid, and add R7c, Co element. Alkali mayo generates a compound with acid and burns this generated compound to form R7C.
Obtaining a cumulative oxide and a Co element oxide is defined as [k].

ＲＣｏ希土類コバルト合金のｆｉｔ削粉、切削粉および
切断粉等の機械加工により出る粉からのＲ２Ｈ索とＣｏ
元素の分囁、回収においてまず第一に問題になるのは慎
械刀ロエ粉中に混入している砥石粉などの不純物とＲ元
素、Ｃｏ元素の分離である。この点本発明名らはこのＲ
元素、Ｃａｘ素と砥石粉などの不純物との分離方法につ
いて種々の研死を１ねた結果、機械加工粉をｒｊＲ％し
くにその水溶液から回収処理する方法がこの分離の目的
に非常に有効であることを見いだした。すなわち、例え
は塩酸を機械加工粉に冷加して機械加工粉を塩酸で溶解
すると、Ｒ７Ｈ累とＣｏ元素の大部分はＲ元素イオン、
Ｃｏ元素イオンとして溶液中に存在し、砥石粉などの不
純物の大部分ね不溶層物残滓として残存する。R2H cables and Co
The first problem in the separation and recovery of elements is the separation of R and Co elements from impurities such as grinding stone powder mixed in Shinkaito Roe powder. In this respect, the name of the present invention is this R
As a result of various experiments on methods for separating impurities such as elements, Cax elements, and grinding wheel powder, we found that a method of recovering and processing machined powder from its aqueous solution in a rjR% manner is very effective for this separation purpose. I discovered something. That is, for example, when hydrochloric acid is cooled to machining powder and the machining powder is dissolved in hydrochloric acid, most of the R7H and Co elements become R element ions,
It exists in the solution as Co element ions, and most of the impurities such as grindstone powder remain as insoluble layer residue.

この溶層処理においては投入塩酸の童、溶解溶液のＰＨ
のｇ埋等が重要であるのは言うまでもない。また上記溶
解のために使用する酸に塩酸以外にも種々のものが使用
可能でやることは言ｔｌ−待たない。In this solution layer treatment, the pH of the dissolved solution is
It goes without saying that g filling etc. are important. Moreover, various acids other than hydrochloric acid can be used as the acid used for the above-mentioned dissolution.

しかして、＠記不溶解物残滓をろ過し除去することで、
Ｒ７Ｃ素イオンとＣｏ元素イオンに冨んだ溶液を得るこ
とができる。However, by filtering and removing the undissolved residue,
A solution rich in R7C elemental ions and Co elemental ions can be obtained.

次に問題なのｔｚＲ７Ｃ票イオンとＣｏ元素イオンの分
際である。この様な２１１＠以上のイオンを含む溶液か
ら各元素イオンを分離する方法として位、従来溶媒抽出
法という手法が一般的に採用されている。これは２種類
以上のイオンを含む浴液を油に会合接触させ、油に抽出
逼れやすい元素を溶液から分離する方法である。し力為
しこの溶媒抽出法は溶液を何回も繰り返し油に会合接触
させる必要があるため、分際に多大の時間と費用を要す
るという欠点がある。The next problem is the separation between the tzR7C ion and the Co element ion. As a method for separating each element ion from a solution containing such ions of 211@ or more, a conventional technique called solvent extraction method is generally employed. This is a method in which a bath solution containing two or more types of ions is brought into contact with oil, and elements that are easily extracted and trapped in oil are separated from the solution. However, this solvent extraction method has the drawback of requiring a large amount of time and expense, since it is necessary to bring the solution into contact with the oil many times.

この点本発ａＡ名らはこの溶液中ＯＲ元素イオンとＣ０
７Ｃ素イオンの分離方法についても種々の検討を刃口え
た結果、散を添加することによりこの問題を％決するこ
とができた。On this point, the present authors aA et al.
As a result of various studies regarding the method of separating 7C elementary ions, we were able to solve this problem by adding powder.

Ｒ元素イオンとＣ０７Ｃ累イオンに冨む溶液に例えは蓚
酸水溶液をｆｊ＆加することによりＲ２Ｏ索は蓚酸塩と
して沈殿する。この沈＊Ｗはろ過によって（９）収可能
であシ、残った溶液はＣ０７Ｃ累イオンに冨んだもので
ある。For example, by adding an aqueous solution of oxalic acid to a solution rich in R element ions and C07C ions, R2O molecules precipitate as oxalate. This precipitate (9) can be collected by filtration, and the remaining solution is enriched with C07C ions.

以上のような化学処理によ、ＱＲＣｏ希土類コバルト合
金の機械加工粉を冨Ｒｙｃ＄沈殿物と冨Ｃｏ７Ｃ素イオ
ン溶液に分離することが可能となる。The chemical treatment described above makes it possible to separate the machined powder of the QRCo rare earth cobalt alloy into a rich Ryc$ precipitate and a rich Co7C elementary ion solution.

Ｂ元素の回収については安定な酸化物の形態が保管上、
取り扱い上の点からも好ましい。そして８元素酸化物の
生成は、前記Ｒ元素沈殿物を乾燥後焼成することで可能
である。Regarding recovery of B element, stable oxide form is required for storage.
It is also preferable from the point of view of handling. The eight element oxides can be produced by drying and then firing the R element precipitate.

しかし回収Ｒ元素酸化物の品位の点からは、Ｒ元素沈殿
物をさらに水酸化ナトリウム水浴液、蓚酸などのアルカ
リ、酸で順次処理し、得られた化合物を焼成してＲ７Ｃ
索酸化物を得ることがより好ましい。However, from the standpoint of the quality of the recovered R element oxide, the R element precipitate is further treated with a sodium hydroxide water bath solution, an alkali such as oxalic acid, and an acid, and the resulting compound is calcined to produce R7C.
It is more preferable to obtain oxidized carbonate.

この理由ね、ＲＣｏ希土類コバルト合金中にＦｓ。The reason for this is that Fs is present in the RCo rare earth cobalt alloy.

Ｃｕ、Ｈｆ等他の元素が不純物あるいは冷加物とし　　
１て存在する場合、それらの大部分は塩酸等での浴牌時
にＰＨ刺Ｗ！によシ砥石等の不純物と共に不溶牌物残滓
中に残留させ除去可能であるが、その一部分が溶′％溶
液中に浴出しＲ元素沈殿時に共沈するからである。従っ
て共沈したこれらの元素を除去するために、Ｒ元素沈殿
物を酸、アルカリで繰り返し処理しｎ製するのがよシ好
ましいのである。Other elements such as Cu and Hf may act as impurities or coolants.
1, most of them are PH stings when bathing with hydrochloric acid etc. Although it is possible to remove the insoluble tile residue by leaving it together with impurities such as the grindstone, a part of it is taken out into the solution and co-precipitated when the R element is precipitated. Therefore, in order to remove these co-precipitated elements, it is highly preferable to repeatedly treat the R element precipitate with acid and alkali to produce n.

以上のようにＲ元素沈殿物を例えは水酸化ナトリウム水
浴液、次いで蓚酸で処理しまたこれらの工程間に数回の
水洗、ろ過を行えば、得られ九Ｒ元素修ｒＲ堪を乾燥・
焼成した場合、きわめて高品位のＲ元素酸化物が得られ
る。As described above, if the R element precipitate is treated with, for example, a sodium hydroxide water bath solution and then with oxalic acid, and washed and filtered several times between these steps, the nine R element precipitates obtained can be dried and dried.
When fired, an extremely high-grade R element oxide is obtained.

しかしてＲ元素そのものは、Ｒ元素酸化物を還元するこ
とで容易に得られる。シカし、この還元技術は既に工業
的に広く一般ＫＭ立されているものであシ、ここではそ
の詳細について述べることね省略する。However, the R element itself can be easily obtained by reducing the R element oxide. However, since this reduction technology has already been widely used in general KM industrially, we will not discuss its details here.

Ｃ０７Ｃ索の回収についてもＲ元素の場合と同様の理由
で酸化物の形態が好ましい。すなわち、Ｒ元素沈殿物を
゛除去した冨Ｃｏ光・素イオン溶液にアルカリ水浴液１
に添加することにより、容易にＣｏ元素化合物を沈殿さ
せることが可能である。例えＵ水酸化す）　ＩＪウム水
溶液の重加でＣｏ元素の水酸化物が沈殿し、炭酸ナトリ
ウム水溶液の冷加でにＣｏ元素の炭酸塩が沈殿する。そ
してこれらＣ０７ＣＸ化合物は水洗が容易でありこれら
を水洗・ろ過し、乾燥後焼成することで高品位のＣｏ元
素酸化物が得られる。Regarding the recovery of C07C cords, the oxide form is preferable for the same reason as in the case of the R element. That is, 1 part of the alkaline water bath solution is added to the Co light/element ion solution from which the R element precipitate has been removed.
It is possible to easily precipitate a Co element compound by adding Co to . For example, when an aqueous sodium carbonate solution is added, the hydroxide of the Co element precipitates, and when the aqueous sodium carbonate solution is cooled, a carbonate of the Co element precipitates. These C07CX compounds are easy to wash with water, and high-grade Co element oxides can be obtained by washing, filtering, drying, and firing.

以上のように本発明によｐＲｃｏ希土類コバルト合金の
機械加工粉からきわめて容易にＲ元素とＣ。As described above, according to the present invention, R element and C can be obtained very easily from the machined powder of pRco rare earth cobalt alloy.

元素が高品位の酸化物の形態で分離・回収可能である。Elements can be separated and recovered in the form of high-grade oxides.

そしてこれらの酸化物は一般に既知の従来技術によって
容易にＲ２Ｏ索とＣｏ元素に処理可能であるから、本発
明によって分離・回収したＲ元素とＣｏ元素を再ひＲＣ
ｏ希土類コバルト合金の＃！造に使用できる。従って本
発明によるとＲＣｏ希土類コバルト合金の製ｆ１原価低
減の効果が著しいものである。Since these oxides can generally be easily processed into R2O elements and Co elements by known conventional techniques, the R elements and Co elements separated and recovered by the present invention can be reprocessed by RC.
o Rare earth cobalt alloy #! Can be used for construction. Therefore, according to the present invention, the effect of reducing the manufacturing cost of RCo rare earth cobalt alloy f1 is remarkable.

以下実施例にて本発明をさらに詳しく説明する。The present invention will be explained in more detail in the following examples.

実施例ｔ ＳｍＣｏ＠希土類コバルト合金の含水機械加工粉を組成
分析した。この含水機械加工粉の含水率は４４ｙｔ％で
あった。また水分以外の粉体の組Ｉｉ！、は８ｍ２７．
！ｉｗｔ％、Ｃｏｊａ６ｖｔ％、砥石粉などの不純物Ｕ
ｗｔ％であった。粉体の組成分析値の合計が１００ｗｔ
うとならないことから、ＳｍとＣｏのかなりの部分が酸
化されているものと考えられる。Example t A hydrous machining powder of SmCo@rare earth cobalt alloy was analyzed for its composition. The moisture content of this hydrous mechanical powder was 44 yt%. Also, group Ii of powder other than water! , is 8m27.
! iwt%, Coja6vt%, impurities such as whetstone powder U
It was wt%. The total composition analysis value of powder is 100wt
It is considered that a considerable portion of Sm and Co is oxidized.

この含水機械加工粉ｚｏｏｏＫｆに水を加え、合計１．
５７０Ｊのスラリー状溶液とし、このスラリー状溶液に
２９０ノの３５％塩酸水溶液を徐々に添加し１切削粉を
溶解した。この化学処理によってｇｏ。Water was added to this water-containing mechanical powder zooooKf, and a total of 1.
A slurry solution of 570 J was prepared, and 290 J of a 35% aqueous hydrochloric acid solution was gradually added to the slurry solution to dissolve one cutting powder. This chemical treatment allows go.

ｌの機械加工粉溶解の溶液が得られた。化学処理用のタ
ンク底にね、砥石粉等の不純物を中心成分とした不溶解
物残滓が石干残舊したが、これらはろ過で除云した。上
記溶液を分析した結果Ｓｍ９α７１１／Ｉ、Ｃｏ　１５
９ｉ　Ｉ／ｌ　テア”：）’Ｉｔ：、、。A solution of 1 of machining powder was obtained. At the bottom of the tank used for chemical treatment, there were insoluble residues mainly composed of impurities such as whetstone powder, but these were removed by filtration. As a result of analyzing the above solution, Sm9α711/I, Co 15
9i I/l Thea":)'It:,,.

次にこの機械加工粉溶解溶液に５００１の蓚酸水溶液を
徐々に添加して８ｍ元票を蓚酸塩として沈殿させた。こ
の沈殿物をろ過、した後、得られたＳｍ元素硫化物に若
干の水と５００１の水酸化す）　ＩＪウム水浴液を徐々
に添加し、Ｓｍ元素を水酸化−とした。この水酸化物を
ろ過、水洗した後、これに若干の水と５００ノの蓚酸水
溶液を徐々に加え、Ｓｍ元素を修Ｗｌ塩として沈殿させ
た。沈殿したＳｍ元素の蓚ａＩ塩を水洗、ろ過した。Next, an aqueous solution of 5001 oxalic acid was gradually added to this machining powder solution to precipitate 8m oxalate as oxalate. After filtering this precipitate, some water and a 5001 hydroxide water bath solution were gradually added to the obtained Sm element sulfide to hydroxylate the Sm element. After this hydroxide was filtered and washed with water, some water and a 500 ml oxalic acid aqueous solution were gradually added thereto to precipitate the Sm element as a Wl salt. The precipitated Sm element Al al salt was washed with water and filtered.

以上の処理によって得られた含水スラリー状のａｍ　７
Ｃ素の修ｆＩｔ塩は４４０〜であった。Am7 in the form of water-containing slurry obtained by the above treatment
The modified fIt salt of C element was 440~.

このスラリー状のＳｍ元素の蓚酸塩を脱水・乾燥し、焼
成炉にてＦＩＬ１００℃の温度で２時間焼成して酸化物
とした。得られたＳｍ元素の酸化物の１童は１５０Ｋｆ
であつ次。そしてこの８ｍ元票の酸化物を分析した結果
、工業的に従来一般に使用されているＳｍ元素酸化物と
同品位のものであった。This slurry-like oxalate of Sm element was dehydrated and dried, and fired in a firing furnace at a FIL temperature of 100° C. for 2 hours to form an oxide. One child of the obtained oxide of Sm element is 150 Kf
And next. As a result of analysis of this 8m oxide, it was found to be of the same quality as the Sm element oxide commonly used industrially.

−万、Ｓｍ元素を除去した後のＣｏ元素イオンに富む浴
Ｗ＃溶液にｔｏｏｏｌの水酸化す）　Ｉ）ラム水溶液を
徐々に加え、Ｃｏ元素を水酸化物として沈散さぜた。沈
殿物を水洗・ろ過し、含水Ｃｏ元素の水酸化物ａａＱｌ
１４ｆ得た。この含水Ｃ０７Ｃ素酸化物を脱水・乾燥し
、焼成炉にてｆＪｌ、　１００℃の温度で２時間焼成し
て酸化物とした。得られｆｃＣｏ元素の酸化　１１゜智
の１重は５１０Ｋｆであった。このＣｏ元素の酸化物を
分析した結果、工業的に従来一般に使用されているＣｏ
元嵩酸化豐と同品位のものであった。-10,000, After removing the Sm element, the Co element ion-rich bath W# solution was subjected to hydroxylation of toool) I) Rum aqueous solution was gradually added, and the Co element was precipitated as a hydroxide. The precipitate was washed with water and filtered, and hydrated Co element hydroxide aaQl was obtained.
I got 14f. This hydrous C07C elementary oxide was dehydrated and dried, and fired in a firing furnace at fJl and 100° C. for 2 hours to obtain an oxide. One layer of oxidation of the obtained fcCo element at 11° was 510 Kf. As a result of analyzing this oxide of Co element, we found that Co
It was of the same quality as the former bulk oxidized bamboo shoots.

実施例２ ａｍ　（Ｃｏｂｉｌ　Ｆｅｏ、ｔ　Ｃｕｏ、＋　Ｈｆｏ
、ｗｔ鵞）ａ、ｓ　　希土類コバルト合金の含水機械加
工粉を組成分析した。この含水機械加工粉の含水率は４
４ｖｔ９１であった。また、水分以外の粉体の組成は８
ｍ２ｒＬＳ　ｗｔ　ＩＧ、Ｃｏ　４重１ｗｔ％、Ｆ曖１
ｔ、０ｗｔ％、Ｃｕ　４０　ｖｔ　％、Ｈｆ　１０　ｖ
ｒｔ　％、砥石粉などの不純物２．４　ｗｔ　％でめっ
た。粉体の組成分析値の合計が１００Ｗ′ｔＩｓになら
ないことから、各元素のかなｐの部分が酸化されている
ものと考えられる。Example 2 am (Cobil Feo, t Cuo, + Hfo
, wt) a, s We analyzed the composition of hydrated machining powder of rare earth cobalt alloy. The moisture content of this hydrous mechanical powder is 4
It was 4vt91. In addition, the composition of the powder other than water is 8
m2rLS wt IG, Co 4x 1wt%, F vague 1
t, 0 wt%, Cu 40 vt%, Hf 10 v
rt %, and impurities such as grindstone powder were 2.4 wt %. Since the total compositional analysis value of the powder does not reach 100 W'tIs, it is considered that the kana p portion of each element is oxidized.

この含水機械加工粉ｚｏｏｏＫｆに水を加え合計１，４
００ｔのスラリー状溶液とし、このスラリー状浴液に＄
２００１の３５チ塩酸水溶液を徐々に添加して切削粉を
溶解した。この化学処理によってλ４０Ｑｔの機械加工
＠溶解溶液が得られた。また化学処理用夕／りの底には
砥石粉などの不純物とＣｕ、’Ｆ・、■元素などを中心
成分とし九不溶解物鴻滓が残留したがこれらはろ過で除
去し丸。上記溶ｔを分析した結果Ｓｍ４　ＡＤ　ｐ／Ｌ
ＳＣｏａ４１　Ｎ、Ｆｓ　＆　Ｑ　ｐ　／　Ｌ、　Ｃｕ
（１００墨＃／１．出αｏｏ　１ｐ／Ｌで参つ九。Add water to this water-containing mechanical powder zooooKf for a total of 1.4
00t slurry solution, and add $ to this slurry bath liquid.
A 35% hydrochloric acid aqueous solution of 2001 was gradually added to dissolve the cutting powder. This chemical treatment resulted in the machining of λ40Qt@dissolution solution. In addition, impurities such as grinding stone powder and slag, which is an insoluble substance mainly composed of elements such as Cu, F, and ■, remained at the bottom of the chemical treatment tank, but these were removed by filtration. As a result of analyzing the above melt t, Sm4 AD p/L
SCoa41 N, Fs & Q p/L, Cu
(100 ink #/1.9 out of αoo 1p/L.

次にこの機械加工粉溶解溶液に５００１の蓚酸水溶液を
徐々にａ７Ｊｌ］シてＳｍ元素を蓚酸塩として沈殿させ
た。この沈殿物をろ過した後、得られたＳｍ元素修蓚酸
塩若干の水と５００ノの水酸化す）　ＩＪウム水溶液を
徐々に肉刃口し、Ｓｍ７Ｃ索全水酸化物とした。この水
酸化＠をろ過、水洗した恢、これに若干の水と５００１
の蓚酸水浴液を加え、Ｓｍ７［：索を蓚１１ｔＪｉとし
て沈殿させた。沈殿したＳｍ７ｃ素の蓚酸塩を水洗・ろ
過した。Next, an aqueous solution of 5001 oxalic acid was gradually poured into this solution of machining powder to precipitate the Sm element as oxalate. After filtering this precipitate, the obtained Sm elemental oxalate was gradually mixed with some water and 500% IJ hydroxide aqueous solution to obtain Sm7C total hydroxide. After filtering and washing this hydroxide, add some water and 5001
An oxalic acid water bath solution was added to precipitate Sm7[:Sm7] as Sm11tJi. The precipitated oxalate of Sm7c was washed with water and filtered.

以上の処理によって得られ次官水スラリー状のＳｍ元素
の蓚酸＃ＡはｓｓａＫｇであった。The Sm element oxalic acid #A in the form of a water slurry obtained by the above treatment was ssaKg.

このスラリー状のＳｍ元素の蓚酸塩を脱水・乾燥し、焼
成炉にて約１１００℃の温度で２５８間焼成して酸化物
とした。得られたＳｍ元素の酸化物の１童は１１０Ｖ４
であった。そしてこのＳｍ元素の酸化物を分析した結果
、工業的に従来一般に使用されているＳｒｎ元索酸化物
と同品位のものであった。This slurry of oxalate of Sm element was dehydrated and dried, and fired in a firing furnace at a temperature of about 1100° C. for 258 hours to form an oxide. One child of the obtained Sm element oxide is 110V4
Met. As a result of analysis of this oxide of the Sm element, it was found to be of the same quality as the Srn element oxide commonly used industrially.

一方、８ｍ元票を除云した後のＣｏ元素イオンに富む溶
Ｗ＃溶液に２，０ＯＯＡ！の炭酸す）　ＩＪウム水溶液
を徐々に加え、Ｃｏｙｃ累を炭酸塩として沈殿させた。On the other hand, after removing 8m yuan, the molten W# solution rich in Co element ions contains 2,0OOA! An aqueous solution of COYC was gradually added to precipitate the COYC as carbonate.

沈殿物を水洗・ろ過し、含水Ｃｏ元素の炭識塩７００〜
を得た。この含水Ｃｏ元元素酸塩を脱水・乾燥し、焼成
炉にてｉｆ）　１．１００℃の温度で２時間焼成して酸
化物とした。得られ友Ｃｏ元素の酸化物の１量ね２５０
Ｋｐであった。このＣｏ元素の酸化物を分析した粕来、
工業的に従来一般に使用されているＣｏ元素の酸化物と
同品位のものであった。The precipitate is washed with water and filtered, and the carbon salt of hydrated Co element is 700 ~
I got it. This hydrated Co elemental salt was dehydrated and dried, and fired in a firing furnace at a temperature of 1.100°C for 2 hours to form an oxide. The amount of oxide of Co element obtained is 250
It was Kp. Kasuki, who analyzed this oxide of Co element,
It was of the same quality as the Co element oxide commonly used industrially.

以上得られた結果を表に示すと以下の通シとなる。The results obtained above are shown in the table below.

第１表は回収Ｓｍ元素酸化物の各分析値を示す。Table 1 shows each analysis value of the recovered Sm element oxide.

表中ＡＵ従従来業的に使用されている８ｍ元Ｘ酸化物、
Ｂは本楯明の実施例１に＋るＳｍＣｏ５の酸化物、Ｃは
本発明の実施例２によるＳｍ　（Ｃｏ　ｂａ　ｌ　Ｆ＠
ｏ、＊　Ｃｕｏ、ｉＨｆ　Ｏ，００１！　）ｓ、ｓの酸
化物についてのものである。In the table, AU conventionally used 8m elemental X oxide,
B is an oxide of SmCo5 according to Example 1 of the present invention, and C is Sm (Cobal F@) according to Example 2 of the present invention.
o, * Cuo, iHf O,001! )s, s oxide.

第２表は回収Ｃｏ元素酸化物の各分析値を示す。Table 2 shows each analytical value of the recovered Co element oxide.

表中りは従来工業的に使用されているＣｏ元素酸化物、
Ｅは本発明の実施例１によるＳｍＣｏｇの酸化物、Ｆは
本発明の実施例２によるＳｍ　（Ｃｏｂａｌ　Ｆｅｅ、
ｓ　Ｃｕｅ、１Ｈｆｏ、ｏｕ　）ｓ、ｓの酸化物につい
てのものである。In the table, Co element oxides conventionally used industrially,
E is an oxide of SmCog according to Example 1 of the present invention, F is Sm (Cobal Fee,
s Cue, 1Hfo, ou ) Regarding the oxides of s and s.

以上説明し友とおシ、本発明にょシＲＣｏ希土類コバル
ト合金を機械加工することにょシ出る粉から、Ｒ元素と
Ｃｏ元素とが工業的に使用可能な品位の酸化物として各
々分離・回収が可能とな９、省資源等の工業的効果は大
なるものがある。さらに本発明はＲＣｏ希土類コバルト
合金の製造面例えば製造原価の大幅な低減にも寄与する
等の効果ｔＶするものである。Having explained the above, my friend and I would like to express our understanding that in accordance with the present invention, R element and Co element can be separated and recovered as oxides of industrially usable grade from the powder produced when machining RCo rare earth cobalt alloy. 9. It has great industrial effects such as resource saving. Furthermore, the present invention has advantages in terms of manufacturing RCo rare earth cobalt alloys, such as contributing to a significant reduction in manufacturing costs.

代理人弁理士　本　間　　　崇Representative Patent Attorney Takashi Honma

Claims (1)

【特許請求の範囲】 ｔ　　ＲＣｏ希土類コバルト合金（ＲはＹ？含むＩＩＩ
類以上の希土類金属元素）の研削粉、切削粉おめ、上記
機械力ロエ粉會冨Ｒ元素沈殿物と冨Ｃｏ元素イオン溶液
とに分離することに％徴とする希土類コバルト合金粉の
処理方法。 ２、　　ＲＣｏ希土希土類ルト合金（ＲはＹを含む１種
類以上の希土類金属元素）の研削粉、切削粉および切断
粉等の機械加工粉に、塩酸、蓚酸等のイ゛。 酸又はその水溶液七飽加して化学反応を生七しめ、上記
機械加工粉を冨Ｒ７Ｃ素沈殿物と冨Ｃｏ元素イオン浴液
とに分離し、この冨Ｒ元素沈殿物、冨Ｃｏ元素イオン溶
液の各々に水酸化ナトリウム水浴液、炭酸ナトリウム水
溶液等のアルカリ水浴液あるいは蓚酸等の酸又はその水
溶液’ｔｆｊＳｍして、Ｒ元素、Ｃｏ元素のアルカリま
たは酸との化合物を生成せしめ、この生成化合物を焼成
してＲ７Ｃ素酸化智、Ｃｏ元素酸化物を得ることを特徴
とする希土類コバルト合金粉の処理方法。[Claims] t RCo rare earth cobalt alloy (R is Y?
A method for processing rare earth cobalt alloy powder, which involves separating grinding powder, cutting powder, and the above-mentioned mechanical force into a rich Co element precipitate and a rich Co element ion solution. . 2. Add hydrochloric acid, oxalic acid, etc. to machining powder such as grinding powder, cutting powder, and cutting powder of RCo rare earth metal alloy (R is one or more rare earth metal elements including Y). Acid or its aqueous solution is saturated to induce a chemical reaction, and the mechanically processed powder is separated into a rich R7C elementary precipitate and a rich Co element ion bath solution, and this rich R element precipitate and a rich Co element ion solution are separated. A sodium hydroxide water bath solution, an alkaline water bath solution such as a sodium carbonate aqueous solution, or an acid such as oxalic acid or its aqueous solution 'tfjSm is added to each of the above to form a compound of R element and Co element with an alkali or acid. A method for processing rare earth cobalt alloy powder, which comprises firing to obtain R7C element oxide and Co element oxide.