WO2003072504A1 - Procede de purification servant a produire un compose de niobium et/ou de tantale de grande purete - Google Patents
Procede de purification servant a produire un compose de niobium et/ou de tantale de grande purete Download PDFInfo
- Publication number
- WO2003072504A1 WO2003072504A1 PCT/JP2003/002225 JP0302225W WO03072504A1 WO 2003072504 A1 WO2003072504 A1 WO 2003072504A1 JP 0302225 W JP0302225 W JP 0302225W WO 03072504 A1 WO03072504 A1 WO 03072504A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- niobium
- compound
- tantalum
- solution
- extraction
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
- C01G33/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
- C01G35/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- 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
Definitions
- the present invention belongs to a method for obtaining a high-purity niobium compound and / or tantalum compound.
- Niobium is used as a steel additive because it stabilizes carbon in steel and prevents intergranular corrosion.
- niobium alloy has been put into practical use as a conductive tube attached to the lamp light emitting portion of a high-pressure sodium lamp, and is used as a superconducting material or an additive element of a superalloy.
- niobium oxide has been in great demand, and among them, it has been widely used in the fields of the electronics industry and the optics field. Particularly in these fields, high-purity niobium has become indispensable.
- niobium oxide for example, the fractional crystallization method, the solvent extraction method, and the ion exchange resin method.
- Methods such as the distillation method have been proposed.
- tantalum coexists with niobium in the ore for obtaining niobium, for example, Columpai Toniocolorite. Since niobium and evening are physically and chemically similar in nature, it was extremely difficult to separate them. For this reason, many means have been proposed to collect compounds containing these elements from ores together.
- an ore containing niobium and tantalum is pulverized and treated with hydrofluoric acid and a mineral acid, such as sulfuric acid and a mixed acid, to obtain a mixture of niobium and tantalum.
- tantalum are dissolved together with iron, manganese, calcium, rare earth elements and other metal impurities, and this solution is brought into contact with an organic solvent such as a lower fatty acid ketone, ester, or ether, particularly methyl isobutyl ketone, and then niobium and tantalum are dissolved. It describes a method of extracting and separating the organic solvent into an organic solvent phase.
- niobium N b F 7 2 - N b OF 5 2 By reducing the density, niobium N b F 7 2 - N b OF 5 2 from - to alter, the other tantalum by utilizing the fact that is present as a T a F 7 2 one, methyl iso
- a method of extracting tantalum with an organic solvent such as butyl ketone, or conversely, re-extracting niobium from the tantalum and niobium once extracted into the organic solvent to the acidic aqueous solution side is used. These methods are also described in JP-A-62-158018.
- a porous carrier such as activated carbon or polypropylene is provided with an oxygen-containing organic solvent such as trioctyl phosphine oxide or an alkyl group having 4 or more carbon atoms.
- an oxygen-containing organic solvent such as trioctyl phosphine oxide or an alkyl group having 4 or more carbon atoms.
- the present invention provides a method for purifying a high-purity niobium compound and / or tantalum compound, which can purify a high-purity niobium compound and / or tantalum compound more easily and at low cost.
- a method for purifying a high-purity niobium compound and / or tantalum compound which can purify a high-purity niobium compound and / or tantalum compound more easily and at low cost.
- the present invention is characterized in that a crystallization operation and an extraction operation are performed using a liquid in which a niobium compound is dissolved, thereby achieving high purification.
- niobium oxide is dissolved in a hydrofluoric acid solution, but not limited to crystallization from a hydrofluoric acid solution, but also includes crystallization from an aqueous solution or an organic solvent. Furthermore, it can be applied to various salts, and the desired high-purity niobium compound Needless to say, can be manufactured.
- niobate fluoride H 2 N b F 7
- O carboxymethyl full O Roni niobate H 2 N b OF 5
- metal impurities such as Fe, Ni, and Ti.
- impurities remain on the solution side, and pure niobic acid or oxyfluoroniobate is obtained as crystals.
- a solution system containing hydrofluoric acid to which sulfuric acid, nitric acid, hydrochloric acid, etc. are added in the dissolution / crystallization step may be used.
- the HF concentration may be adjusted by diluting with water.
- the crystallization method is not limited to the cooling method, but includes crystallization by concentration.
- the niobium source is not limited to the aqueous niobium compound solution, but the melt of the crystal obtained in claim 2 is used.
- the extraction solvent ketones such as MIBK (methyl isobutyl ketone), esters, ethers, organic phosphorus compounds, Extract and purify by adding amines.
- MIBK methyl isobutyl ketone
- esters esters
- ethers organic phosphorus compounds
- Extract and purify by adding amines by using the above-mentioned niobium compound, there is no need for reverse extraction or the like, and it is possible to remove tantalum which is the same family at least once.
- an extraction condition generally, a phase ratio with an organic phase / aqueous phase is 1 or more, but in the present invention, it was found that extraction was possible even under a condition of less than 1.
- the extraction step it is also possible to perform extraction using a niobium compound aqueous solution dissolved only in water or a crystal melt obtained in claim 2 without adding sulfuric acid or the like for adjusting the acidity.
- a target high-purity niobium compound By treating the obtained niobium compound, a target high-purity niobium compound can be obtained.
- an insoluble niobium hydroxide is obtained by subjecting a niobium compound solution extracted after crystallization to alkali treatment, and high-purity niobium oxide can be produced by roasting this niobium hydroxide.
- potassium fluoride or lime carbonate potassium fluoroniobate (K 2 NbF 7 ) can be produced.
- high-purity niobium metal can be produced by melting a high-purity niobium compound with alkali.
- niobium-containing mineral or a commercially available industrial niobium compound can be used, and preferably, about 99% of a niobium compound is used. Since it can be easily purified to the level of 9.9% (4N) or more, it can be industrially manufactured at low cost.
- the present invention is characterized in that it is a method that can be highly purified by performing an extraction operation in addition to a crystallization operation using a solution in which a niobium compound is dissolved.
- the obtained aqueous niobium solution is niobium fluoride or oxyniobium fluoride, and solid-liquid separation is performed by crystallizing this solution. Do. This crystallization step removes most of the homologous tantalum and other metal impurities such as Fe, Ni and Ti. At this time, impurities move to the liquid phase side, the crystal side is purified, and high purity can be easily achieved.
- ketones generally give good results.
- a ketone extraction solvent which is a well-known technique, is mainly used, but it goes without saying that purification can be performed using esters, ethers, organic phosphorus compounds, amines, and the like.
- phase ratio (organic phase / aqueous phase) is reduced to less than 1.
- the amount of the organic solvent can be reduced, leading to a reduction in cost.
- sulfuric acid is generally used to adjust the acidity, but in the present invention, it can be carried out without adding sulfuric acid. The amount can be reduced.
- tantalum is extracted into the organic layer, and a purified aqueous niobium compound solution is obtained in the aqueous phase. Needless to say, In order to obtain a high-purity niobium compound, it is possible to repeat this extraction step.In the present invention, however, tantalum, which is a homologous impurity of niobium, can be extracted in a single extraction operation to a concentration of 0.5 ppm or less. Can be reduced to
- niobium fluoride or oxyfluorinated niobate which is a water-soluble crystal obtained by crystallization, is used as an intermediate raw material and is made of high-purity lithium niobate.
- niobium compound such as salts containing other niobium.
- tantalum can be purified by the same operation as niobium.
- a high purity tantalum oxide (T a 2 0 5), ⁇ oxidation degree Tan lithium Tal acid (L i T a0 3), potassium high purity fluoride tantalate (K 2 T a F 7) and high High-purity tantalum compounds such as pure metal tantalum (Ta) and other salts containing tantalum can be produced.
- niobium hydrofluoric acid solution 500 g of 75% -HF was placed in a 1 L transparent PFA container equipped with a stirrer, and 150 g of niobium oxide containing metal impurities was supplied with stirring for about 3 hours. Stirring was performed. Thereafter, insoluble components were removed by filtration to prepare a niobium hydrofluoric acid solution of about 300 g / L in terms of niobium element.
- Example 1 In the extraction operation of Example 1, the crystal after crystallization obtained above was used.
- the impurity concentrations of the crystals used for this extraction are as shown in Table 1.
- the extraction operation was performed using a 1 L batch extractor with niobium crystals obtained by the above crystallization. 40 g were added, and then 360 g of distilled water or a 1N aqueous sulfuric acid solution was added. Then the organic solvent was added.
- the organic solvent methyl isobutyl ketone (hereinafter abbreviated as MIBK) or cyclohexanone was used.
- MIBK methyl isobutyl ketone
- trioctylphosphine oxide crystal After adding 40 g of the niobium crystal after the above crystallization and 360 g of a 1 N aqueous solution of sulfuric acid, adding 80 g of trioctylphosphine oxide crystal, and then heating to 65 ° C, the trioctylphosphine was heated. After dissolving the oxide crystals, the trioctylphosphine oxide layer was separated to obtain 398 g of extracted water.
- niobium hydroxide 65 g of 28% -ammonia water was added to the extracted water or the extracted melt to precipitate niobium as niobium hydroxide, and then ammonium fluoride was removed by filtration to obtain niobium hydroxide.
- the obtained niobium hydroxide was calcined at 1,000 ° C. in an electric furnace to obtain 13.9 g of niobium oxide.
- ICP-AES inductively coupled plasma atomic emission spectrometer
- Table 1 shows that the results of the impurity amounts were the same when distilled water was used instead of the sulfuric acid for adjusting the acidity and the sulfuric acid.
- the feature of the present invention is that impurities are reduced to the same degree under the condition that the oZw phase ratio is less than 1. It is also a feature of the present invention that there is no need to particularly add sulfuric acid for adjusting the acidity. This reduces the amount of alkali added during alkali neutralization. Can lead to lower costs.
- the impurity removal efficiency was analyzed by the extraction operation, and compared with the crystallization operation. An experiment was also performed on the number of extractions.
- niobium hydrofluoric acid solution 500 g of 50% -HF is placed in a 1-liter transparent PFA container equipped with a stirrer, and 150 g of niobium oxide is supplied with stirring for about 3 hours. Stirred. A small amount of insoluble matter was removed by filtration to prepare a niobium hydrofluoric acid solution of 300 g / L in terms of niobium element. The concentration of impurities in the solution used for this extraction is as shown in Table 2.
- the obtained niobium hydroxide was fired at 1000 ° C. in an electric furnace to obtain 25.7 g of niobium oxide.
- ICF-AES inductively coupled plasma atomic emission spectrometer
- tantalum hydrofluoric acid solution 500 g of 50% -HF was placed in a 1-liter transparent PFA container equipped with a stirrer, and 130 g of tantalum oxide containing metal impurities was supplied with stirring, followed by heating to 70 ° C and reflux. Stirring was performed for about 5 hours below. Thereafter, insoluble components were removed by filtration to prepare a tantalum hydrofluoric acid solution of about 300 g / L in terms of tantalum element.
- Example 2 In the extraction operation of Example 2, the crystals after crystallization obtained above were used.
- the impurity concentration of the crystals used for this extraction is as shown in Table 3.
- the obtained tantalum hydroxide was calcined at 1,000 ° C. in an electric furnace to obtain 12.1 g of tantalum oxide.
- ICP-AES inductively coupled plasma atomic emission spectrometer
- Table 3 shows that, in the case of tantalum, as in the case of niobium, it was possible to easily purify up to 99.99% or more in the dissolution step ⁇ only one crystallization step ⁇ only one extraction step.
- niobium-containing mineral or a commercially available industrial niobium compound can be used, and preferably, about 99% of a niobium compound is used. Since it can be easily purified to the level of 9.9% (4N) or more, it can be produced industrially at low cost.
- the use of the niobium compound crystal or niobium compound obtained after the crystallization step obtained in the present invention can be used as an intermediate raw material for various high-purity niobium compounds.
- the high-purity niobium compound obtained by these methods it becomes possible to manufacture as high-performance materials in various fields such as high-quality electronic materials and optical materials.
- This purification method is characterized by the following three major steps: (1) dissolving step, (2) crystallization step, and (3) extraction step (at least once).
- the impurity removal process By adopting a crystallization process as the primary treatment, it is characterized by a purification technology that can be easily performed industrially. Also, in the extraction step, the amount of organic solvent is reduced and the amount of alkali neutralization is reduced by eliminating the addition of sulfuric acid for adjusting the acidity, thereby reducing the labor required for the solvent extraction method and reducing the load in the next step.
- tantalum can be obtained by the same operation.
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR10-2004-7012779A KR20040093062A (ko) | 2002-02-27 | 2003-02-27 | 고순도 니오브 화합물 및/또는 탄탈 화합물의 정제 방법 |
EP03743049A EP1484283A4 (en) | 2002-02-27 | 2003-02-27 | CLEANING METHOD FOR THE PRODUCTION OF A HIGH-PURITY NIOB CONNECTION AND / OR TANTALI COMPOUND |
BR0307879-5A BR0307879A (pt) | 2002-02-27 | 2003-02-27 | Método para purificar um composto de nióbio e/ou um composto de tântalo altamente puro |
JP2003571215A JP4326345B2 (ja) | 2002-02-27 | 2003-02-27 | 高純度ニオブ化合物及び/又はタンタル化合物の精製方法 |
US10/505,803 US7214362B2 (en) | 2002-02-27 | 2003-02-27 | Purification method for producing high purity niobium compound and/or tantalum compound |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002/52412 | 2002-02-27 | ||
JP2002052412 | 2002-02-27 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2003072504A1 true WO2003072504A1 (fr) | 2003-09-04 |
Family
ID=27764338
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2003/002225 WO2003072504A1 (fr) | 2002-02-27 | 2003-02-27 | Procede de purification servant a produire un compose de niobium et/ou de tantale de grande purete |
Country Status (8)
Country | Link |
---|---|
US (1) | US7214362B2 (ja) |
EP (1) | EP1484283A4 (ja) |
JP (1) | JP4326345B2 (ja) |
KR (1) | KR20040093062A (ja) |
CN (1) | CN1639069A (ja) |
BR (1) | BR0307879A (ja) |
TW (1) | TWI274042B (ja) |
WO (1) | WO2003072504A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010155909A (ja) * | 2008-12-26 | 2010-07-15 | Pilot Corporation | 中空樹脂粒子の製造方法および中空樹脂粒子 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2214853A4 (en) * | 2007-10-15 | 2013-05-22 | Hi Temp Specialty Metals Inc | PROCESS FOR PREPARING TANTALUM POWDER USING RECYCLED AGENTS AS AN EXISTING MATERIAL |
CN102399990A (zh) * | 2011-11-28 | 2012-04-04 | 镇江中孚复合材料有限公司 | 一种从废旧含铌高温合金提取氧化铌的方法 |
CN113186399B (zh) * | 2021-03-12 | 2022-11-18 | 北京工业大学 | 一种提取钽和铌的方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4932897A (ja) * | 1972-07-27 | 1974-03-26 | ||
JPH0421524A (ja) * | 1990-05-15 | 1992-01-24 | Nikko Kyodo Co Ltd | 弗化タンタルカリウムの精製方法 |
JP2000327330A (ja) * | 1999-05-18 | 2000-11-28 | Tokuyama Corp | 酸化ニオブの精製方法 |
JP2001146424A (ja) * | 1999-11-17 | 2001-05-29 | Tokuyama Corp | 酸化ニオブ及び/又は酸化タンタルの製造方法 |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
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US2962327A (en) * | 1957-10-09 | 1960-11-29 | Electrolux Ab | Self-lubricating bearing |
US3072459A (en) * | 1959-12-30 | 1963-01-08 | Union Carbide Corp | Process for producing fluoride-free columbium or tantalum pentoxide |
US4164417A (en) * | 1978-04-28 | 1979-08-14 | Kawecki Berylco Industries, Inc. | Process for recovery of niobium values for use in preparing niobium alloy products |
JPS58176128A (ja) | 1982-04-09 | 1983-10-15 | Agency Of Ind Science & Technol | 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 |
JPS62158118A (ja) | 1985-12-28 | 1987-07-14 | Chiyuugai Tekunosu Kk | 酸化ニオブの製法 |
JPS6431937U (ja) | 1987-08-21 | 1989-02-28 | ||
DE4021207A1 (de) * | 1990-07-03 | 1992-01-16 | Starck Hermann C Fa | Verfahren zur gewinnung und trennung von tantal und niob |
DE4030707A1 (de) * | 1990-09-28 | 1992-04-02 | Starck Hermann C Fa | Verfahren zur herstellung von fluoridarmen tantal-/niob-oxidhydraten bzw. oxiden |
US5385713A (en) * | 1992-05-29 | 1995-01-31 | Ecotek, Inc. | Metal and fluorine values recovery from mineral ore treatment |
US5620936A (en) * | 1993-12-14 | 1997-04-15 | E. I. Dupont De Nemours And Company | Recovery of spent catalyst |
WO1995016635A1 (en) * | 1993-12-14 | 1995-06-22 | E.I. Du Pont De Nemours And Company | Recovery of spent catalyst |
SE512978C2 (sv) * | 1998-10-26 | 2000-06-12 | G S G As | Bearbetning av niob-och tantalinnehållande material |
US6764669B2 (en) * | 1999-12-28 | 2004-07-20 | Mitsui Mining & Smelting Co., Ltd. | Method for producing fluorinated potassium tantalate crystal |
US6800268B2 (en) * | 2000-11-29 | 2004-10-05 | Mitsui Mining & Smelting Co., Ltd. | Method for producing potassium fluoroniobate crystals and potassium fluoroniobate crystals |
DE502004011120D1 (de) * | 2003-07-15 | 2010-06-17 | Starck H C Gmbh | Niobsuboxidpulver |
-
2003
- 2003-02-27 WO PCT/JP2003/002225 patent/WO2003072504A1/ja not_active Application Discontinuation
- 2003-02-27 BR BR0307879-5A patent/BR0307879A/pt not_active Application Discontinuation
- 2003-02-27 TW TW092104179A patent/TWI274042B/zh not_active IP Right Cessation
- 2003-02-27 EP EP03743049A patent/EP1484283A4/en not_active Withdrawn
- 2003-02-27 JP JP2003571215A patent/JP4326345B2/ja not_active Expired - Fee Related
- 2003-02-27 US US10/505,803 patent/US7214362B2/en not_active Expired - Fee Related
- 2003-02-27 KR KR10-2004-7012779A patent/KR20040093062A/ko not_active Application Discontinuation
- 2003-02-27 CN CNA03804725XA patent/CN1639069A/zh active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4932897A (ja) * | 1972-07-27 | 1974-03-26 | ||
JPH0421524A (ja) * | 1990-05-15 | 1992-01-24 | Nikko Kyodo Co Ltd | 弗化タンタルカリウムの精製方法 |
JP2000327330A (ja) * | 1999-05-18 | 2000-11-28 | Tokuyama Corp | 酸化ニオブの精製方法 |
JP2001146424A (ja) * | 1999-11-17 | 2001-05-29 | Tokuyama Corp | 酸化ニオブ及び/又は酸化タンタルの製造方法 |
Non-Patent Citations (1)
Title |
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See also references of EP1484283A4 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010155909A (ja) * | 2008-12-26 | 2010-07-15 | Pilot Corporation | 中空樹脂粒子の製造方法および中空樹脂粒子 |
Also Published As
Publication number | Publication date |
---|---|
TW200303293A (en) | 2003-09-01 |
CN1639069A (zh) | 2005-07-13 |
EP1484283A4 (en) | 2008-03-05 |
KR20040093062A (ko) | 2004-11-04 |
JP4326345B2 (ja) | 2009-09-02 |
US20050115364A1 (en) | 2005-06-02 |
BR0307879A (pt) | 2004-12-28 |
US7214362B2 (en) | 2007-05-08 |
TWI274042B (en) | 2007-02-21 |
EP1484283A1 (en) | 2004-12-08 |
JPWO2003072504A1 (ja) | 2005-08-11 |
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