JPS6247817B2 - - Google Patents
Info
- Publication number
- JPS6247817B2 JPS6247817B2 JP6011882A JP6011882A JPS6247817B2 JP S6247817 B2 JPS6247817 B2 JP S6247817B2 JP 6011882 A JP6011882 A JP 6011882A JP 6011882 A JP6011882 A JP 6011882A JP S6247817 B2 JPS6247817 B2 JP S6247817B2
- Authority
- JP
- Japan
- Prior art keywords
- tantalum
- niobium
- hydrofluoric acid
- ammonium chloride
- resin column
- 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
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
本発明はニオブおよびタンタルを含む鉱石より
ニオブおよびタンタルを効率よく回収する方法に
関するものである。
ニオブおよびタンタルを含む鉱石としては、ニ
オカライト（Ca，Nb）4Si2（Ｏ，OH，Ｆ）９、
コロンバイト（Fe，Mn）（Nb，Ta）2O6、サマル
スカイト（Ｙ，Er）（Nb，Ta）2O6などがある。
ニオブおよびタンタルは機械工具、医療、歯科治
療用器具、白金代替品、電子材料等に利用される
工業的に重要な元素である。
従来ニオブおよびタンタルの回収方法としては
水酸化カリウム法、フツ化カリウム複塩法、タン
ニン酸法およびクペロン法などがあるが、完全分
離は難しい。
本発明はニオブおよびタンタルを含む鉱石より
ニオブおよびタンタルを純粋に回収する方法を開
発すべく鋭意研究を重ねた結果、イオン交換樹脂
により処理し、ニオブおよびタンタルのみを樹脂
に吸着させ、他元素との分離を完全にした後、フ
ツ化水素酸と塩化アンモニウム溶液によつてニオ
ブおよびタンタルを溶離させることを見出し本発
明を完成するに至つた。
すなわちニオブおよびタンタルを含む鉱石の微
粉末にフツ化水素酸および硫酸を加えて砂浴上で
加熱分解する。ニオカライトの様にSiおよびCa
を含むものはSiO2およびCaSO4などの沈殿を生
ずるので、これらの沈殿を分離した炉液を用い
る。この炉液中に存在するのはニオブ、タンタ
ル、鉄、マンガン、希土類元素などが含まれてい
る。この炉液を強塩基性陰イオン交換樹脂柱に通
すと、ニオブおよびタンタルが樹脂柱に吸着さ
れ、他の元素は樹脂柱を通過する。例えば樹脂柱
としてダウエツクス１−×８（商品名、ダウケミ
カル社製）を用いた場合、1M以上の濃度のフツ
化水素酸で樹脂柱を洗浄した後、フツ化水素とし
て1M以上の濃度の試料溶液を樹脂柱に流し、1M
濃度のフツ化水素酸で十分洗浄し、4M塩化アン
モニウムを含む1Mフツ化水素酸溶液で溶離する
とニオブおよびタンタルは１〜5CV（CVはカラ
ム容積）で溶出する。試料溶液中にジルコニウム
およびハフニウムを含む場合には、1Mフツ化水
素酸では溶出しないので、4N塩酸でジルコニウ
ムおよびハフニウムを溶離させる必要がある。
4N塩酸の後、1Mフツ化水素酸を流し次いで4M塩
化アンモニウムを含む1Mフツ化水素酸で溶離す
れば、ニオブおよびタンタルをジルコニウムおよ
びハフニウムから分離することができる。このニ
オブおよびタンタルの溶出液を蒸発乾固し、乾固
物を電気炉で焼成することによりニオブおよびタ
ンタルの混合酸化物として回収することができ
る。
本発明で用いられる陰イオン交換樹脂として
は、ダウエツクス１−×８（商品名、ダウケミカ
ル社製）、アンバーライトIRA―400（商品名、米
国、ローム・アンド・ハース社製）などが例とし
てあげられる。
本発明によればニオブおよびタンタルを含む鉱
石よりニオブおよびタンタルを高純度かつ高収率
で分離回収することができ、また経済的であり、
工業的回収方法として好適である。
なお本発明はニオブおよびタンタルを少量含む
鉱石、例えば中国産ニオブ含有鉄鉱石などにも応
用することができる。
次に本発明を実施例によりさらに詳細に説明す
る。
実施例 １
ニオカライト（Ca，Nb）4Si2（Ｏ，OH，Ｆ）
９の微粉末１ｇを白金蒸発皿に秤取し、フツ化水
素酸10mlと硫酸（１：１）１mlを加え砂浴上で加
熱分解を行う。
分解が終了した後に紙を用いて沈殿（SiO2
およびCaSO4）を過し、液をイオン交換分離
に使用する。イオン交換樹脂としてはポリエチレ
ンクロマトグラフ管にダウエツクス１−×８、10
mlを充填したものを用い、10Mフツ化水素酸でよ
く洗浄した後、試料溶液（1M以上のフツ化水素
含有）を樹脂柱に通し、1Mフツ化水素酸で洗浄
した後、4M塩化アンモニウムを含む1Mフツ化水
素酸溶液50mlを流してニオブおよびタンタルを溶
離させる。この溶出液を蒸発乾固した後残渣を電
気炉で焼成することによりニオブおよびタンタル
の混合酸化物を得ることができる。なお4M塩化
アンモニウムを含む1Mフツ化水素酸で樹脂柱か
らニオブおよびタンタルを溶離させる代りに、ニ
オブおよびタンタルを吸着した樹脂を電気炉で焼
成することによりニオブおよびタンタルの混合酸
化物を得ることもできる。得られたニオブおよび
タンタルの純度は99.8％、収率は99％であつた。
その他の実施例を表に示す。
The present invention relates to a method for efficiently recovering niobium and tantalum from ores containing niobium and tantalum. Ores containing niobium and tantalum include niocalite (Ca, Nb) 4 Si 2 (O, OH, F) 9 ,
Examples include columbite (Fe, Mn) (Nb, Ta) 2 O 6 and samarskite (Y, Er) (Nb, Ta) 2 O 6 .
Niobium and tantalum are industrially important elements used in mechanical tools, medical and dental instruments, platinum substitutes, electronic materials, etc. Conventional methods for recovering niobium and tantalum include the potassium hydroxide method, potassium fluoride double salt method, tannic acid method, and cuperone method, but complete separation is difficult. The present invention was developed as a result of intensive research to develop a method for purely recovering niobium and tantalum from ores containing niobium and tantalum.The result is a treatment using an ion exchange resin that allows only niobium and tantalum to be adsorbed onto the resin, allowing them to be removed from other elements. After complete separation of niobium and tantalum, the inventors discovered that niobium and tantalum could be eluted with a solution of hydrofluoric acid and ammonium chloride, leading to the completion of the present invention. That is, hydrofluoric acid and sulfuric acid are added to fine powder of ore containing niobium and tantalum, and the mixture is thermally decomposed on a sand bath. Si and Ca like niocalite
Since those containing SiO 2 and CaSO 4 will precipitate, the furnace liquid from which these precipitates have been separated is used. This furnace fluid contains niobium, tantalum, iron, manganese, and rare earth elements. When this furnace liquid is passed through a strongly basic anion exchange resin column, niobium and tantalum are adsorbed on the resin column, and other elements pass through the resin column. For example, when Dowex 1-x8 (trade name, manufactured by Dow Chemical Company) is used as a resin column, after cleaning the resin column with hydrofluoric acid with a concentration of 1M or more, a sample with a concentration of 1M or more as hydrogen fluoride is used. Pour the solution onto the resin column and add 1M
After thorough washing with concentrated hydrofluoric acid and elution with a 1M hydrofluoric acid solution containing 4M ammonium chloride, niobium and tantalum elute at 1 to 5 CV (CV is column volume). If the sample solution contains zirconium and hafnium, they will not be eluted with 1M hydrofluoric acid, so it is necessary to elute zirconium and hafnium with 4N hydrochloric acid.
Niobium and tantalum can be separated from zirconium and hafnium by eluting with 4N hydrochloric acid followed by 1M hydrofluoric acid and 4M ammonium chloride in 1M hydrofluoric acid. This eluate of niobium and tantalum is evaporated to dryness, and the dried product is fired in an electric furnace to recover a mixed oxide of niobium and tantalum. Examples of anion exchange resins used in the present invention include Dowex 1-x8 (trade name, manufactured by Dow Chemical Company) and Amberlite IRA-400 (trade name, manufactured by Rohm and Haas Company, USA). can give. According to the present invention, niobium and tantalum can be separated and recovered from ores containing niobium and tantalum with high purity and high yield, and it is also economical.
It is suitable as an industrial recovery method. The present invention can also be applied to ores containing small amounts of niobium and tantalum, such as niobium-containing iron ore produced in China. Next, the present invention will be explained in more detail with reference to Examples. Example 1 Niokalite (Ca, Nb) 4 Si 2 (O, OH, F)
Weigh out 1 g of fine powder of No. 9 in a platinum evaporation dish, add 10 ml of hydrofluoric acid and 1 ml of sulfuric acid (1:1), and heat decompose it on a sand bath. After the decomposition is complete, use paper to precipitate (SiO 2
and CaSO 4 ) and the liquid is used for ion exchange separation. As an ion exchange resin, use Dowex 1-x8, 10 in a polyethylene chromatography tube.
After thoroughly washing with 10M hydrofluoric acid, the sample solution (containing 1M or more hydrogen fluoride) was passed through the resin column, washed with 1M hydrofluoric acid, and 4M ammonium chloride was used. 50 ml of a 1M hydrofluoric acid solution containing niobium and tantalum are eluted. A mixed oxide of niobium and tantalum can be obtained by evaporating this eluate to dryness and then firing the residue in an electric furnace. Note that instead of eluting niobium and tantalum from the resin column with 1M hydrofluoric acid containing 4M ammonium chloride, a mixed oxide of niobium and tantalum can also be obtained by firing the resin that has adsorbed niobium and tantalum in an electric furnace. can. The purity of the obtained niobium and tantalum was 99.8%, and the yield was 99%. Other examples are shown in the table.
【表】
純度および収率はニオブとタンタルの合量
である。
[Table] Purity and yield are the total amount of niobium and tantalum.
Claims (1)
フツ化水素酸および硫酸にて分解し、その溶液を
強塩基性陰イオン交換樹脂で処理した後、フツ化
水素酸と塩化アンモニウム溶液でニオブとタンタ
ルを溶離させることを特徴とするニオブおよびタ
ンタルを含む鉱石よりニオブおよびタンタルを回
収する方法。1 Decompose fine powder of ore containing niobium and tantalum with hydrofluoric acid and sulfuric acid, treat the solution with a strong basic anion exchange resin, and then dissolve niobium and tantalum with hydrofluoric acid and ammonium chloride solution. A method for recovering niobium and tantalum from ores containing niobium and tantalum, the method comprising eluting niobium and tantalum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57060118A JPS58176128A (en) | 1982-04-09 | 1982-04-09 | Recovery of niobium and tantalum from ore containing niobium and tantalum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57060118A JPS58176128A (en) | 1982-04-09 | 1982-04-09 | Recovery of niobium and tantalum from ore containing niobium and tantalum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58176128A JPS58176128A (en) | 1983-10-15 |
| JPS6247817B2 true JPS6247817B2 (en) | 1987-10-09 |
Family
ID=13132880
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57060118A Granted JPS58176128A (en) | 1982-04-09 | 1982-04-09 | Recovery of niobium and tantalum from ore containing niobium and tantalum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58176128A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2772409B2 (en) * | 1993-06-08 | 1998-07-02 | 工業技術院長 | Method for separating niobium and tantalum |
| EP1484284A4 (en) | 2002-02-27 | 2008-03-05 | Stella Chemifa Kk | Purification method for producing high purity niobium compound and/or tantalum compound |
| WO2003072504A1 (en) | 2002-02-27 | 2003-09-04 | Stella Chemifa Kabushiki Kaisha | Purification method for producing high purity niobium compound and/or tantalum compound |
| KR100684356B1 (en) | 2005-05-20 | 2007-02-20 | 한국지질자원연구원 | Attrition mill type agitated chlorination reactor and smelting method of tantalum ore using the same |
| JP6910690B1 (en) | 2021-03-15 | 2021-07-28 | 学校法人福岡工業大学 | Niobium and tantalum liquefaction treatment methods |
-
1982
- 1982-04-09 JP JP57060118A patent/JPS58176128A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58176128A (en) | 1983-10-15 |
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