JP3363646B2 - Rare earth metal separation method - Google Patents
Rare earth metal separation methodInfo
- Publication number
- JP3363646B2 JP3363646B2 JP05122495A JP5122495A JP3363646B2 JP 3363646 B2 JP3363646 B2 JP 3363646B2 JP 05122495 A JP05122495 A JP 05122495A JP 5122495 A JP5122495 A JP 5122495A JP 3363646 B2 JP3363646 B2 JP 3363646B2
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth metal
- optical glass
- lanthanum
- elute
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】Detailed Description of the Invention
【０００１】[0001]
【産業上の利用分野】本発明は、レアアースメタルの分
離方法に関し、詳しくは光学硝子の研磨・洗浄工程及び
付帯する排水処理より発生する光学硝子汚泥（以下、単
に光学硝子汚泥という）からのレアアースメタルの分離
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for separating rare earth metals, and more specifically, rare earth from optical glass sludge (hereinafter, simply referred to as optical glass sludge) generated by polishing and cleaning steps of optical glass and accompanying wastewater treatment. Regarding separation method of metal.
【０００２】[0002]
【従来の技術】レアアースメタル（原子番号５７番のラ
ンタンから７１番のルテシウムまでのランタノイドの１
５元素に原子番号２１番のスカンジウムと３９番のイッ
トリウムを加えた１７元素）は光学材料、電子材料、金
属材料、触媒等に利用され、なかでも酸化ランタンを多
量に含有した光学硝子は、通過する光を高屈折かつ低分
散させる性質を有していることから、光学硝子工業に多
量に使用されている。2. Description of the Related Art Rare earth metals (1 of lanthanoids from atomic number 57 lanthanum to atomic number 71 lutetium)
17 elements (5 elements plus scandium with atomic number 21 and yttrium with atomic number 39) are used for optical materials, electronic materials, metallic materials, catalysts, etc. Among them, optical glass containing a large amount of lanthanum oxide passes through. It is used in a large amount in the optical glass industry because it has the property of highly refracting and reducing the dispersion of light.
【０００３】従来、レアアースメタルは鉱石（モナザイ
ト、バストネサイト、ゼノタイム等）から、湿式法（浸
出、固液分離、金属及び化合物採取、電解等）または乾
式法（焼結、還元、揮発、精製等）により、鉱石→［選
鉱、製錬、加工］→粗金属→［高純度化、機能化］→新
素材→製品化の諸工程を経て製品化されている。Conventionally, rare earth metals are produced from ores (monazite, bastnasite, xenotime, etc.) by a wet method (leaching, solid-liquid separation, metal and compound extraction, electrolysis, etc.) or a dry method (sintering, reduction, volatilization, purification). Etc.), it is commercialized through the steps of ore → [beneficiation, smelting, processing] → crude metal → [high purification, functionalization] → new material → commercialization.
【０００４】一方、一般に光学硝子汚泥は有機物及び有
害金属を多量に含有しており、廃棄物として扱われ、溶
融・固化等を経て埋立処分されているのが現状である。On the other hand, in general, optical glass sludge contains a large amount of organic substances and harmful metals, is treated as waste, and is currently landfilled after being melted and solidified.
【０００５】そこで、二次公害防止や資源の有効利用の
観点から、レアアースメタル資源をリサイクルする技術
が望まれている。Therefore, a technique for recycling rare earth metal resources is desired from the viewpoint of prevention of secondary pollution and effective use of resources.
【０００６】従って、本発明の目的は、有機物及び有害
金属を多く含有する光学硝子汚泥からレアアースメタル
を分離回収する方法を提供することにある。Therefore, it is an object of the present invention to provide a method for separating and recovering rare earth metals from optical glass sludge containing a large amount of organic substances and harmful metals.
【０００７】[0007]
【課題を解決するための手段】すなわち、第１の本発明
は、光学硝子汚泥をアルカリ溶融してレアアースメタル
を溶出させた後、残存する不溶物を酸煮沸して更にレア
アースメタルを溶出させることを特徴とするレアアース
メタルの分離方法である。アルカリ溶融法と酸煮沸法と
の組み合わせによりレアアースメタルを溶出させてい
る。[Means for Solving the Problems] That is, according to the first aspect of the present invention, after melting optical glass sludge with an alkali to elute the rare earth metal, the remaining insoluble matter is boiled with an acid to further elute the rare earth metal. Is a method for separating rare earth metals. Rare earth metals are eluted by a combination of the alkali melting method and the acid boiling method.
【０００８】第２の本発明は、第１の本発明において、
アルカリ溶融を、光学硝子汚泥１重量部に対し１．５〜
１０重量部の炭酸塩を添加して行う場合である。The second aspect of the present invention is the same as the first aspect of the present invention.
Alkali melting from 1.5 to 1 part by weight of optical glass sludge
This is the case where 10 parts by weight of carbonate is added.
【０００９】第３の本発明は、光学硝子汚泥をアルカリ
溶融してレアアースメタルを溶出させた後、残存する不
溶物を酸煮沸して更にレアアースメタルを溶出させ、次
いで溶出したレアアースメタルをシュウ酸塩にした後、
焼成して酸化物として回収することを特徴とするレアア
ースメタルの分離方法である。第１の本発明の工程に続
いて、シュウ酸塩にした後焼成して酸化物のかたちで分
離回収している。In the third aspect of the present invention, the optical glass sludge is alkali-melted to elute the rare earth metal, the remaining insoluble matter is boiled with acid to further elute the rare earth metal, and then the eluted rare earth metal is converted to oxalic acid. After salting
It is a method for separating a rare earth metal, which is characterized by firing and recovering it as an oxide. Subsequent to the first step of the present invention, the oxalate is converted into oxalate, which is then calcined and separated and recovered in the form of an oxide.
【００１０】これら第１、第２、第３の本発明の方法
は、これまで廃棄物として処分されていた光学硝子汚泥
を有価物に変えるという、レアアースメタル資源のリサ
イクルに貢献する技術である。The methods of the first, second and third aspects of the present invention are technologies for contributing to the recycling of rare earth metal resources, that is, converting optical glass sludge, which has been disposed of as waste, to valuables.
【００１１】[0011]
【実施例】以下、本発明を実施例により説明する。
（実施例１ アルカリ溶融＋酸煮沸）光学硝子汚泥とし
て、レアアースメタル含有量がランタン１０〜４０重量
％、ネオジム５〜１０重量％のものを使用した。EXAMPLES The present invention will be described below with reference to examples. (Example 1 Alkali melting + acid boiling) As the optical glass sludge, those having a rare earth metal content of 10 to 40% by weight of lanthanum and 5 to 10% by weight of neodymium were used.
【００１２】るつぼに光学硝子汚泥を１０ｇ、炭酸塩
（Ｎａ2 ＣＯ3 ）を１５〜１００ｇとり、このるつぼを
電気炉に入れて９００℃で１時間、アルカリ溶融により
光学硝子汚泥を分解した。この分解汚泥を水洗した後、
ランタン、ネオジムが検出されなくなるまで混酸で濾過
を繰り返して、ランタン、ネオジムを溶出させた。10 g of optical glass sludge and 15 to 100 g of carbonate (Na 2 CO 3 ) were placed in a crucible, and the optical glass sludge was decomposed by alkaline melting in an electric furnace at 900 ° C. for 1 hour. After washing this decomposed sludge with water,
The filtration with a mixed acid was repeated until lanthanum and neodymium were not detected, and lanthanum and neodymium were eluted.
【００１３】次に、ビーカーに５〜６０体積％硝酸溶液
を５０ｍｌ、上記濾過の不溶物をとり、ビーカーをヒー
ターで加熱して１０分間酸煮沸を行い、ランタン、ネオ
ジムを溶出させた。Next, 50 ml of a 5-60 volume% nitric acid solution was placed in a beaker, the insoluble matter of the above filtration was taken, the beaker was heated by a heater and acid-boiled for 10 minutes to elute lanthanum and neodymium.
【００１４】ランタン、ネオジムの溶出率を測定したと
ころ、９０〜９８重量％と高い値を示した。When the dissolution rate of lanthanum and neodymium was measured, it showed a high value of 90 to 98% by weight.
【００１５】次に、上記溶出液に、シュウ酸をｐＨ１〜
３になるように添加して、ランタン、ネオジムのシュウ
酸塩を生成させた。この溶液に対し、ランタン、ネオジ
ムが検出されなくなるまで混酸で濾過を繰り返して不溶
物を得た。この不溶物を乾燥後、電気炉に入れて９００
℃で１時間焼成して、ランタン、ネオジムの酸化物を生
成させ、酸化物として分離回収した。Next, oxalic acid is added to the above eluate at pH 1 to
The oxalates of lanthanum and neodymium were generated by adding 3 to each other. The solution was repeatedly filtered with mixed acid until lanthanum and neodymium were not detected, and an insoluble matter was obtained. After drying this insoluble matter, put it in an electric furnace to 900
Firing at 1 ° C. for 1 hour produced oxides of lanthanum and neodymium, which were separated and collected as oxides.
【００１６】また、炭酸塩添加量を表のように変えて、
Ｌａ溶出率との関係を調べた。The amount of carbonate added is changed as shown in the table,
The relationship with the La elution rate was investigated.
【００１７】 [0017]
【００１８】表より、光学硝子汚泥量１部に対して、炭
酸塩を１．５〜１０部添加した場合に効果が顕著である
ことが分る。From the table, it can be seen that the effect is remarkable when 1.5 to 10 parts of carbonate is added to 1 part of optical glass sludge.
【００１９】（比較例１ 酸浸漬）ビーカーに５〜６０
体積％硝酸溶液を５０ｍｌ、光学硝子汚泥１０ｇをと
り、２４時間浸漬を行った。ランタン、ネオジムの溶出
率は１重量％であった。(Comparative Example 1 acid immersion) 5-60 in a beaker
50 ml of a volume% nitric acid solution and 10 g of optical glass sludge were taken and immersed for 24 hours. The dissolution rate of lanthanum and neodymium was 1% by weight.
【００２０】（比較例２ 酸煮沸）ビーカーに５〜６０
体積％硝酸溶液を５０ｍｌ、光学硝子汚泥１０ｇを加
え、１０分間煮沸を行った。ランタン、ネオジムの溶出
率は３０〜４５重量％であった。Comparative Example 2 Acid boiling 5-60 in a beaker
50 ml of a volume% nitric acid solution and 10 g of optical glass sludge were added and boiled for 10 minutes. The dissolution rate of lanthanum and neodymium was 30 to 45% by weight.
【００２１】（比較例３ アルカリ溶融）るつぼに光学
硝子汚泥を１０ｇ、炭酸塩（Ｎａ2 ＣＯ3 ）を１５〜１
００ｇとり、このるつぼを電気炉に入れて９００℃で１
時間、アルカリ溶融により光学硝子汚泥を分解した。こ
の分解汚泥を水洗した後、ランタン、ネオジムが検出さ
れなくなるまで混酸で濾過を繰り返して、ランタン、ネ
オジムを溶出させた。ランタン、ネオジムの溶出率は６
５〜８０重量％であった。Comparative Example 3 Alkali Melt 10 g of optical glass sludge and 15 to 1 carbonate (Na 2 CO 3 ) were placed in a crucible.
Take 00g and put this crucible in an electric furnace at 900 ° C for 1
The optical glass sludge was decomposed by alkali melting for a time. After washing the decomposed sludge with water, filtration with a mixed acid was repeated until lanthanum and neodymium were not detected, and lanthanum and neodymium were eluted. The dissolution rate of lanthanum and neodymium is 6
It was 5 to 80% by weight.
【００２２】[0022]
【発明の効果】以上説明したように、本発明によれば、
光学硝子汚泥から高効率でレアアースメタルの分離が可
能となり、光学硝子汚泥の有価物として資源再利用が可
能になった。As described above, according to the present invention,
It has become possible to separate rare earth metals from optical glass sludge with high efficiency, and resources can be reused as valuable materials for optical glass sludge.
【図１】本発明のレアアースメタルの分離回収方法を説
明する図である。FIG. 1 is a diagram illustrating a method for separating and collecting rare earth metal according to the present invention.
【図２】本発明のレアアースメタルの分離回収方法のフ
ローチャートである。FIG. 2 is a flowchart of a method for separating and recovering rare earth metal according to the present invention.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C01F 17/00 C22B 59/00 ─────────────────────────────────────────────────── ─── Continuation of front page (58) Fields surveyed (Int.Cl. 7 , DB name) C01F 17/00 C22B 59/00
Claims (3)
ースメタルを溶出させた後、残存する不溶物を酸煮沸し
て更にレアアースメタルを溶出させることを特徴とする
レアアースメタルの分離方法。1. A method for separating a rare earth metal, which comprises melting an optical glass sludge with an alkali to elute the rare earth metal and then boiling the remaining insoluble matter with an acid to further elute the rare earth metal.
に対し１．５〜１０重量部の炭酸塩を添加して行う請求
項１記載のレアアースメタルの分離方法。2. The method for separating rare earth metals according to claim 1, wherein the alkali melting is performed by adding 1.5 to 10 parts by weight of carbonate to 1 part by weight of optical glass sludge.
ースメタルを溶出させた後、残存する不溶物を酸煮沸し
て更にレアアースメタルを溶出させ、次いで溶出したレ
アアースメタルをシュウ酸塩にした後、焼成して酸化物
として回収することを特徴とするレアアースメタルの分
離方法。3. After melting the optical glass sludge with an alkali to elute the rare earth metal, the remaining insoluble matter is boiled with an acid to further elute the rare earth metal, and then the eluted rare earth metal is converted into an oxalate salt, A method for separating rare earth metals, which comprises firing and recovering the oxides.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05122495A JP3363646B2 (en) | 1995-03-10 | 1995-03-10 | Rare earth metal separation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05122495A JP3363646B2 (en) | 1995-03-10 | 1995-03-10 | Rare earth metal separation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08245218A JPH08245218A (en) | 1996-09-24 |
| JP3363646B2 true JP3363646B2 (en) | 2003-01-08 |
Family
ID=12880981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05122495A Expired - Fee Related JP3363646B2 (en) | 1995-03-10 | 1995-03-10 | Rare earth metal separation method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3363646B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5398369B2 (en) * | 2009-06-15 | 2014-01-29 | 株式会社東芝 | Rare metal production method and system |
| FR2970709A1 (en) * | 2011-01-25 | 2012-07-27 | Rhodia Operations | PROCESS FOR RECOVERING RARE EARTHS FROM SOLID MIXTURE CONTAINING HALOPHOSPHATE AND RARE EARTH COMPOUND AND SOLID MIXTURE ADAPTED THEREFOR |
| WO2014169322A1 (en) * | 2013-04-18 | 2014-10-23 | Valdrew Nominees Pty Ltd | Recovery of rare earth elements |
-
1995
- 1995-03-10 JP JP05122495A patent/JP3363646B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08245218A (en) | 1996-09-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gupta et al. | Extractive metallurgy of rare earths | |
| Binnemans et al. | Recovery of rare earths from industrial waste residues: a concise review | |
| CN102011020B (en) | Method for recovering rare earth elements from neodymium-iron-boron wastes | |
| EP3180290B1 (en) | Method for extraction and separation of rare earth elements | |
| US20160068929A1 (en) | EXTRACTION OF RARE EARTH METALS FROM NdFeB USING SELECTIVE SULFATION ROASTING | |
| CN1064109A (en) | The treatment process of ores containing rare earths | |
| JP5825074B2 (en) | Rare earth metal recovery method | |
| JPH1150168A (en) | Recovery of rare earth metal component from optical glass sludge | |
| RU2180927C2 (en) | Processes of recovery of valuable metals from tantalumniobium ore carrying insoluble fluorides | |
| JP3363646B2 (en) | Rare earth metal separation method | |
| KR20220032524A (en) | How to recover PGM | |
| KR101031985B1 (en) | Method for manufacturing high purity metal compounds using the hydrometallurgical process from the tantalum ore | |
| AU2021301442B9 (en) | Recovery of rare earth metals from ferromagnetic alloys | |
| EP0244910B1 (en) | Separation of non-ferrous metals from iron-containing powdery material | |
| EP0467180A2 (en) | Rare earth/transition metal alloy scrap treatment method | |
| WO1995013985A1 (en) | Metal and fluorine values recovery from mineral ore treatment | |
| US4964996A (en) | Liquid/liquid extraction of rare earth/cobalt values | |
| WO2022003694A1 (en) | Recovery of rare earth metals from ferromagnetic alloys | |
| CA2192084C (en) | Hydrometallurgical treatment for the purification of waelz oxides through lixiviation with sodium carbonate | |
| KR100787205B1 (en) | Method for recovering precious metal using seawater from mining waste | |
| TW201012940A (en) | Recycling of lead-free silver containing tin solder dross | |
| JP5962404B2 (en) | Iron separation method | |
| US5385713A (en) | Metal and fluorine values recovery from mineral ore treatment | |
| JP2000144276A (en) | Recovering method for rare earth element and cobalt | |
| Narajanan et al. | Processing of monazite at the rare earths Division, Udyogamandal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20071025 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081025 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091025 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091025 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101025 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101025 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111025 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111025 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121025 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131025 Year of fee payment: 11 |
|
| LAPS | Cancellation because of no payment of annual fees |