WO2012132107A1 - Procédé pour produire et procédé pour isoler/purifier du niobium - Google Patents

Procédé pour produire et procédé pour isoler/purifier du niobium Download PDF

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Publication number
WO2012132107A1
WO2012132107A1 PCT/JP2011/077009 JP2011077009W WO2012132107A1 WO 2012132107 A1 WO2012132107 A1 WO 2012132107A1 JP 2011077009 W JP2011077009 W JP 2011077009W WO 2012132107 A1 WO2012132107 A1 WO 2012132107A1
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niobium
organic solvent
raw material
sulfuric acid
solution
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PCT/JP2011/077009
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WO2012132107A9 (fr
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龍太郎 黒田
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三井金属鉱業株式会社
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    • 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
    • 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
    • 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 relates to a separation and purification method and a production method for obtaining niobium, and in particular, to a separation and purification technique of niobium that can reduce boron.
  • Niobium (hereinafter referred to as Nb in some cases) is frequently used as a steel additive because it has the effect of stabilizing carbon in steel and preventing intergranular corrosion.
  • Niobium oxide is also used for single crystals containing niobium such as optical, electronic ceramic, and lithium niobate (LN).
  • a niobium alloy is used as a conductive tube of a lamp light emitting part in a high-pressure sodium lamp, and is also used as an additive element such as a superconducting material or a superalloy.
  • niobium is usually obtained from raw materials such as ore and scrap.
  • raw materials such as ore and scrap.
  • a hydrofluoric acid dissolution-solvent extraction method is generally known (see Patent Documents 1 and 2).
  • MIBK methyl isobutyl ketone
  • MIBK containing niobium is washed with dilute sulfuric acid and further back-extracted with water to obtain a pure niobium aqueous solution.
  • Ammonia water is added to the niobium aqueous solution thus obtained to precipitate a hydroxide precipitate, the precipitate is filtered and dried, and finally calcined to obtain niobium oxide.
  • niobium is a rare product, has many uses, and the demand has increased significantly, and the supply of niobium cannot keep up with the demand. For this reason, niobium is reused by using waste such as glass scrap as a raw material.
  • JP-A-5-2614 Japanese Patent No. 3634747
  • the present invention provides a technology capable of separating and purifying high-purity niobium from which raw materials containing a large amount of boron, such as boron-based glass scrap, are reliably separated and removed, and other impurities are removed. Objective.
  • the present invention provides a phosphoryl-based extractant having the following general formula in a raw material aqueous solution containing niobium and containing hydrofluoric acid and sulfuric acid; (Wherein R is hydrogen, or an alkyl group or aryl group having 1 to 20 carbon atoms) is brought into contact with an organic solvent diluted with a petroleum hydrocarbon diluent to convert niobium A first step of extraction into an organic solvent; A second step of further reducing impurities remaining in the organic solvent by washing the organic solvent after the extraction with water or sulfuric acid, and back-extracting niobium contained in the organic solvent in which the impurities are reduced with an aqueous solvent A niobium separation and purification method comprising a third step of obtaining a niobium purification solution, wherein the concentration of free hydrofluoric acid in the raw material aqueous solution in the first step is 2 to 10 mol / L; The boron content of liquid impurities is 10 ppm
  • a raw material aqueous solution containing niobium and containing hydrofluoric acid and sulfuric acid is used.
  • the raw material aqueous solution is not particularly limited as long as it is an aqueous solution containing niobium.
  • raw material ore containing niobium eg, tantalite, columbite, pyrochlore, etc.
  • hydrofluoric acid or fluoride is hydrofluoric acid or fluoride. It can be obtained by dissolving with a mixed acid of hydrogen acid and sulfuric acid, filtering if necessary, and adjusting the concentration with hydrofluoric acid, sulfuric acid and / or water as appropriate. Therefore, such a raw material aqueous solution contains hydrofluoric acid and sulfuric acid.
  • raw materials that can be used include niobium compounds with low solubility in liquids, such as waste silos and scraps containing fluorosilicates, fluorotantalates, and fluoroniobates, niobium ferroalloys, niobium Examples thereof include metal scrap and LiNbO 3 (LN) scrap. More specifically, potassium fluoride tantalate, flux cleaning water when producing niobium powder from potassium fluoride niobate, and neutralization waste generated from surface treatment liquid, waste liquid discharged from target material manufacturers, etc. And waste such as low-grade niobium products that cannot be used for the production of niobium powder.
  • a method for removing impurities from the raw material in advance may be performed in accordance with a known method, and can be preferably performed by, for example, the following alkali decontamination treatment. That is, the raw material is stirred and mixed with a strong alkali solution (for example, sodium hydroxide solution) while being appropriately heated to obtain a sparse slurry, which is then filtered. Next, the residue obtained by filtration is washed with a mineral acid other than hydrofluoric acid (for example, sulfuric acid), and the mineral acid is filtered off.
  • a strong alkali solution for example, sodium hydroxide solution
  • the cake with reduced impurities obtained by this filtration separation is dissolved with hydrofluoric acid or the like in the same manner as the above-mentioned ordinary raw materials.
  • fluoroniobate K 2 NbF 7 and the like
  • oxyfluoroniobate K 3 Nb 2 F 11 O and the like
  • niobium oxide is not alkaline decontaminated below 100 ° C., it will not be necessary to perform alkaline decontamination on the raw material ore of the oxide.
  • ferroalloys it is effective to perform alkaline lysis because impurities mainly composed of iron are reduced.
  • the raw material prior to the above-mentioned dissection or hydrofluoric acid dissolution, can be appropriately pulverized with a ball mill or the like according to the form of the raw material. Thereby, resolving or hydrofluoric acid dissolution can be performed efficiently.
  • the raw material is not a powder but a lump, it is more preferable to coarsely pulverize with a jaw crusher or the like and further finely pulverize with a ball mill or the like.
  • the following pretreatment is preferably performed when the raw material aqueous solution used in the first step is used.
  • the free hydrofluoric acid concentration and sulfuric acid concentration of the raw material solution are adjusted as appropriate, and then the organic solvent (phosphoryl-based extractant and carbonization) used in the present invention is used.
  • the organic solvent (phosphoryl-based extractant and carbonization) used in the present invention is used.
  • 4-diethyl-2-pentanone methyl isobutyl ketone / MIBK
  • the concentration of free hydrofluoric acid in the raw material solution when removing Ta is preferably 0.1 mol / L or more and less than 2.0 mol / L, and more preferably 0.2 mol / L to 1.8 mol / L. .
  • the sulfuric acid concentration is preferably 0.2 mol / L to 3.0 mol / L, and more preferably 0.5 mol / L to 2.0 mol / L. If the free hydrofluoric acid concentration and the sulfuric acid concentration are too low, extraction of Ta into the organic solvent becomes insufficient, and if it is too high, Nb is easily extracted into the organic solvent together with Ta, resulting in loss of Nb.
  • the concentration of niobium in the raw material aqueous solution is not particularly limited, but the higher the concentration, the more advantageous the amount of drainage.
  • the concentration of the aqueous raw material solution varies depending on the composition of Nb in the ore (raw material) before separation, and is therefore in a wide range of 30 to 300 g / L.
  • Nb in the raw material aqueous solution is present in the aqueous solution in the form of a fluoride such as H 2 NbF 7 , NbF 5 ⁇ 2HF or H 2 NbOF 5 , and in addition to this, the surplus that exists free Hydrofluoric acid is present.
  • the surplus hydrofluoric acid present free is referred to as “free hydrofluoric acid”.
  • the raw material aqueous solution containing niobium and containing hydrofluoric acid and sulfuric acid is contacted with a solvent obtained by diluting a phosphoryl-based extractant with a petroleum-based hydrocarbon diluent. Perform one step.
  • This phosphoryl-based extractant is diluted with a diluent.
  • the phosphoryl-type extractant and petroleum-type hydrocarbon diluent used in the present invention may each be one kind or a mixture of two or more kinds, and are not particularly limited.
  • Examples of the phosphoryl-based extractant used in the present invention include the following general formula: (However, R is hydrogen, or an alkyl group or aryl group having 1 to 20 carbon atoms).
  • Preferred examples of such phosphoryl-based extractants include tri-n-butyl phosphate, triisobutyl phosphate, tri-n-octyl phosphate, tris (2-ethylhexyl) phosphate, tri-n-butylphosphine oxide, tri-n. -Ethylhexylphosphine oxide, tri-n-octylphosphine oxide, tri-n-decylphosphine oxide and the like.
  • Tri-n-octylphosphine oxide hereinafter also referred to as TOPO
  • TBP tri-n-butyl phosphate
  • the petroleum hydrocarbon diluent is not particularly limited, and various organic solvents can be used.
  • Examples of the petroleum hydrocarbon diluent include toluene, xylene, cyclohexane, benzene, kerosene, diethylbenzene, Shellzol A (manufactured by Shell Chemical Japan Co., Ltd.), and Ipsol (manufactured by Idemitsu Kosan Co., Ltd.). Benzene and toluene are not preferred because of environmental problems, but can be used.
  • the mixing ratio of the extractant is smaller than 5:95, the extraction ability of niobium tends to be lowered, and when the ratio of the extractant is larger than 95: 5, the adverse effect when the diluent is not used. Will be insufficient.
  • the concentration of free hydrofluoric acid in the aqueous raw material solution in the first step of the niobium separation and purification method of the present invention is 2 to 10 mol / L.
  • the free hydrofluoric acid concentration is more preferably 4 to 8 mol / L, and further preferably 5 to 7 mol / L.
  • concentration of free hydrofluoric acid in the raw material aqueous solution is less than 2 mol / L, the phosphoryl-based extractant becomes difficult to extract niobium in the first step, and a lot of niobium tends to remain in the extraction residual liquid. If it exceeds 10 mol / L, not only niobium but also boron will be extracted in the first step, and the boron content in the niobium refined solution will increase rapidly.
  • the organic solvent after extraction in the first step is washed with water or sulfuric acid to perform a second step of further reducing impurities remaining in the organic solvent.
  • the sulfuric acid concentration is preferably 0.5 mol / L or more, more preferably 0.7 mol / L or more, and 1.0 mol / L. The above is more preferable.
  • the O / A ratio in the second step is preferably 1 to 50, more preferably 1.5 to 40, and further preferably 2 to 30.
  • the value (O / A ratio ⁇ sulfuric acid concentration) obtained by multiplying the O / A ratio by the sulfuric acid concentration (g / L) is preferably 100 (g / L) or less, more preferably 80 or less, and even more preferably 60 or less. . If the value obtained by multiplying the O / A ratio by the sulfuric acid concentration exceeds 100, the reduction of impurities tends to be insufficient.
  • the third step of obtaining a niobium purified solution by back-extracting niobium contained in the organic solvent in which impurities are reduced in the second step with an aqueous solvent is performed.
  • niobium contained in the organic solvent with reduced impurities in the second step is back-extracted with an aqueous solvent.
  • the purified niobium solution obtained by this back extraction contains niobium with high purity.
  • the aqueous solvent used in the third step of the present invention is not particularly limited, but pure water or an aqueous solution containing ammonia and / or ammonium ions can be used, and these aqueous solvents can sufficiently extract back niobium. Is preferable. Among these, pure water, particularly highly pure water is most preferable because it does not contain impurities and niobium is not easily back-extracted. Examples of the aqueous solution containing ammonia and / or ammonium ions include dilute aqueous ammonia, aqueous ammonium fluoride solution, aqueous ammonium hydrogen fluoride solution, and the like.
  • the flow ratio (O / A ratio) of the organic solvent to the aqueous solvent is 0.5 to 16. It is preferable. If the O / A ratio is less than 0.5, the concentration of the resulting niobium liquid will be low, resulting in poor production efficiency and an increased amount of waste water. On the other hand, when the O / A ratio exceeds 16, the amount of niobium remaining in the organic solvent increases, and the amount to be newly extracted decreases with repeated use.
  • the niobium purification solution obtained by the niobium separation and purification method of the present invention has an impurity boron content of 10 ppm or less with respect to niobium oxide.
  • the sulfuric acid concentration in the raw material aqueous solution in the first step is 8 mol / L or less, and is 0.1 to 1.25 with respect to the hydrofluoric acid concentration in the raw material aqueous solution. It is preferable to be doubled.
  • the ratio of sulfuric acid concentration to hydrofluoric acid concentration in the raw material aqueous solution is less than 0.1 times, the amount of niobium that is not extracted into the organic solvent in the first step tends to increase.
  • the ratio of niobium to be extracted into an organic solvent increases, and the separation of niobium and boron tends to be insufficient.
  • the flow rate (volume) ratio of the organic solvent to the aqueous solvent (herein, the aqueous solvent includes the raw material aqueous solution and the solvent in sulfuric acid).
  • the (O / A ratio) is preferably 0.05 to 3. If the O / A ratio is less than 0.05, niobium extraction tends to be insufficient, the amount of organic solvent extracted per unit volume increases (high load concentration), and the phase separation from the aqueous phase is reduced. Deteriorate. On the other hand, when the O / A ratio exceeds 3, the possibility of causing an emulsion increases, which is not preferable.
  • the method for separating and purifying niobium according to the present invention includes a step of circulating part or all of the organic solvent after back extraction in the third step as part or all of the organic solvent in the first step. Is preferred. If it does in this way, it will become possible to reduce the usage-amount of an organic solvent.
  • niobium oxide by adding ammonia to the niobium purification solution obtained by the niobium separation and purification method of the present invention to precipitate niobium hydroxide, filtering the precipitate, and calcining it. Since the niobium purification solution obtained by the niobium separation and purification method of the present invention is reliably separated and removed of boron and other impurities are also removed, high-purity niobium oxide can be obtained.
  • Ammonia can be added in the form of a gas, but is preferably added in the form of an aqueous ammonia solution (NH 4 OH). The concentration of the aqueous ammonia solution and the amount added thereof can be appropriately determined according to the amount of niobium in the niobium purified solution.
  • the niobium recovery rate is preferably 50% or more, more preferably 60% or more, still more preferably 70% or more, and particularly preferably 80% or more.
  • the niobium recovery rate is the amount of niobium calculated by multiplying the niobium concentration of the purified niobium solution obtained in the third step by the volume of the purified niobium solution obtained in the third step. The ratio to the niobium amount calculated by multiplying the niobium concentration by the volume of the raw material aqueous solution used in the first step. If the recovery rate of niobium is low, industrial implementation becomes difficult. Therefore, a niobium recovery rate of 50% or more is preferable.
  • the niobium oxide obtained by the niobium production method of the present invention has a content of 10 ppm or less in boron, silicon, potassium, tin, antimony, copper, and zinc as impurities, and further, iron as impurities, Each content in titanium and phosphorus is 1 ppm or less.
  • Such high-purity niobium oxide can greatly improve these characteristics when applied to electronic materials and optical materials.
  • the raw material aqueous solution used in this embodiment will be described.
  • 2000 kg of Nb glass scrap was roughly pulverized with a jaw crusher and then finely pulverized with a wet ball mill (2000 L of industrial water) to obtain an Nb glass scrap slurry (1000 g / L).
  • This Nb glass scrap slurry was put into a reaction vessel, and 3100 kg of 48 mass% sodium hydroxide was added over 12 hours. After completion of the addition of sodium hydroxide, stirring was continued for 15 hours while maintaining the liquid temperature at 75 ° C. Thereafter, the entire amount was filtered and separated with a filter press, and washed with water with a filter press to obtain a lysed and washed cake.
  • the obtained lyophilized washed cake was slurried with 3000 L of industrial water, sulfuric acid was added, and the slurry pH was adjusted to pH 2.0. After the sulfuric acid treatment, the slurry was separated by filtration with a filter press to obtain a sulfuric acid-treated cake. And this sulfuric acid treatment cake was melt
  • a raw material aqueous solution used in the first step was prepared from the obtained raw material solution as follows. After adding predetermined amounts of 80 wt% hydrofluoric acid and 98 wt% sulfuric acid to 150 L of raw material solution, industrial water is added to bring the total volume to 450 L, so that the desired hydrofluoric acid concentration and sulfuric acid concentration A raw material aqueous solution was prepared. The sulfuric acid concentration was calculated from the 98 wt% sulfuric acid addition amount and the total liquid amount of 450 L, and for confirmation, the sulfur concentration was measured by ICP emission analysis and converted into the sulfuric acid concentration for comparison.
  • This aqueous raw material solution is Nb 2 O 5 100 g / L, and is the hydrofluoric acid concentration and sulfuric acid concentration of each of Examples and Comparative Examples described below.
  • the composition of the raw solution (each element / Nb 2 O 5) is selected from boron (B / Nb 2 O 5) 3000 mass ppm, silicon (Si / Nb 2 O 5 ) 10000 mass ppm, potassium (K / Nb 2 O 5 ) 300 mass ppm, tin (Sn / Nb 2 O 5 ) 10000 mass ppm, zinc (Zn / Nb 2 O 5 ) 20000 mass ppm, iron ( Fe / Nb 2 O 5 ) 4000 mass ppm, titanium (Ti / Nb 2 O 5 ) 50000 mass ppm, copper (Cu / Nb 2 O 5 ) 100 mass ppm, phosphorus (P / Nb 2 O 5 ) 800 mass
  • Sulfur is measured by ICP emission spectroscopy and converted to sulfuric acid concentration-Free hydrofluoric acid: ion exchange separation, fluorine ion electrode method (standard addition) -K, Na: Atomic absorption photometry-Others: ICP emission spectroscopy
  • Niobium was separated and extracted as follows using the prepared raw material aqueous solution and a countercurrent multistage mixer settler.
  • Table 1 shows operating conditions in each of the first to third steps, and FIG. 1 shows a specific apparatus configuration.
  • a countercurrent multi-stage system is adopted as a method for mixing and contacting the liquid in each process. Specifically, mixing contact is performed by supplying an organic solvent to the first stage and an aqueous solvent to the final stage. It was.
  • the free hydrofluoric acid concentration is fixed at 6 mol / L, and the sulfuric acid concentration has a coefficient (ratio of sulfuric acid concentration to free hydrofluoric acid concentration in the raw aqueous solution) of 0.05 to 1.5.
  • Table 2 Comparative Example 1, Examples 1 to 6, and Comparative Example 6.
  • 3 mol / L dilute sulfuric acid (aqueous phase) is added to the organic solvent obtained in the first step and mixed under the conditions shown in Table 1. Made contact. This transferred niobium and other impurities to dilute sulfuric acid, leaving pure niobium in the organic solvent.
  • a third step (FIG. 1, B: Nb purification stage)
  • niobium was extracted and mixed to obtain a purified niobium solution.
  • niobium oxide Nb 2 O 5 .
  • Table 2 shows the impurity concentration and the niobium recovery rate for the niobium oxide obtained under each condition.
  • Each impurity concentration (impurity weight concentration with respect to niobium oxide weight) and niobium recovery shown in Table 2 were measured as follows.
  • -Si ion exchange separation / molybdenum blue absorptiometry
  • -K ion exchange separation
  • atomic absorptiometry ion exchange separation
  • the conditions for separation and purification of niobium are basically the same as those described in Tables 1 and 2 and FIG. 1, with the coefficient fixed at 0.5 and the free hydrofluoric acid concentration of 1.5 to The amount was changed to 12 mol / L (Table 3, Comparative Example 3, Examples 7 to 11 and Comparative Example 4).
  • the niobium oxide production conditions, impurity concentrations, and niobium recovery rate were the same as described above.
  • Table 3 shows the results when the free hydrofluoric acid concentration was changed.
  • the extractant in the first step is changed.
  • the extractant include tri-n-butyl phosphate (TBP: manufactured by Daihachi Chemical Industry Co., Ltd .: Example 12) and tris (2-ethylhexyl) phosphate (TOP: manufactured by Daihachi Chemical Industry Co., Ltd .: Example 13).
  • TBP tri-n-butyl phosphate
  • TOP tris (2-ethylhexyl) phosphate
  • MIBK 4-methyl-2-pentanone
  • the niobium separation and purification conditions are basically the same as those in Example 1 described in Tables 1 and 2 and FIG.
  • the mixing ratio of the extractant to the diluent was determined in Examples 12 and 13 in a volume ratio of 35:65, and Comparative Example 5 was 100% extractant without using a diluent.
  • Niobium oxide production conditions, impurity concentrations, and niobium recovery were the same as above.
  • Table 4 shows the results when the extractant is changed. In Table 4, the results of Example 4 are also shown for reference.
  • TBP tri-n-butyl phosphate
  • TOP tri-n-octyl phosphate
  • TOPO tri-n-octyl phosphine oxide
  • MIBK 4-methyl-2-pentanone
  • high-purity niobium can be easily and efficiently obtained from glass scrap containing a large amount of boron, and niobium raw materials suitable for electronic materials and optical materials can be provided to the market.

Abstract

La présente invention concerne un procédé de traitement pour récupérer un matériau de départ de niobium très pur à partir de déchets de verre contenant du niobium et du bore. Le procédé pour isoler/purifier du niobium comprend : une première étape pour extraire du niobium dans un solvant organique par mise en contact du solvant organique, qui dilue un agent d'extraction à base de phosphoryle en utilisant un agent diluant d'hydrocarbure de pétrole, et d'une solution aqueuse de matériau de départ contenant du niobium, de l'acide fluorhydrique, et de l'acide sulfurique ; une deuxième étape pour diminuer plus avant les impuretés présentes dans le solvant organique par nettoyage du solvant organique post-extraction en utilisant de l'eau ou de l'acide sulfurique ; et une troisième étape pour obtenir un liquide de niobium purifié par utilisation d'une solution aqueuse pour contre-extraire le niobium contenu dans le solvant organique dans lequel les impuretés ont été diminuées. Le procédé pour isoler/purifier du niobium est caractérisé en ce que la concentration d'acide fluorhydrique libre dans la solution aqueuse de matériau de départ dans la première étape est de 2 à 10 moles/l, et la quantité de bore contenu, une impureté, dans le liquide de niobium purifié étant de pas plus de 10 ppm par rapport à l'oxyde de niobium obtenu à partir du liquide de niobium purifié.
PCT/JP2011/077009 2011-03-31 2011-11-24 Procédé pour produire et procédé pour isoler/purifier du niobium WO2012132107A1 (fr)

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CN108862384A (zh) * 2018-08-23 2018-11-23 广东致远新材料有限公司 一种低锑氧化铌的制备方法和一种低锑氧化钽的制备方法

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US11214495B2 (en) * 2016-08-26 2022-01-04 Central South University Preparation method of phosphotungstic acid
JP7430377B2 (ja) * 2019-06-19 2024-02-13 国立研究開発法人日本原子力研究開発機構 液液系での抽出分離による特定物質の製造装置
JP7297294B2 (ja) * 2019-06-19 2023-06-26 国立研究開発法人日本原子力研究開発機構 液液系での抽出分離による特定物質の製造方法

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JPS63162827A (ja) * 1986-12-25 1988-07-06 Naade Kenkyusho:Kk ニオブ含有合金の処理方法
JPS63243231A (ja) * 1987-03-31 1988-10-11 Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk 金属ニオブの製造方法
JPH01246144A (ja) * 1988-03-28 1989-10-02 Taki Chem Co Ltd 高純度酸化ニオブまたは酸化タンタルの製造方法
JP2004043229A (ja) * 2002-07-10 2004-02-12 Mitsui Mining & Smelting Co Ltd 溶媒抽出法によるタンタルおよび／またはニオブの分離精製のための結晶析出防止方法

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Publication number Priority date Publication date Assignee Title
JPS63162827A (ja) * 1986-12-25 1988-07-06 Naade Kenkyusho:Kk ニオブ含有合金の処理方法
JPS63243231A (ja) * 1987-03-31 1988-10-11 Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk 金属ニオブの製造方法
JPH01246144A (ja) * 1988-03-28 1989-10-02 Taki Chem Co Ltd 高純度酸化ニオブまたは酸化タンタルの製造方法
JP2004043229A (ja) * 2002-07-10 2004-02-12 Mitsui Mining & Smelting Co Ltd 溶媒抽出法によるタンタルおよび／またはニオブの分離精製のための結晶析出防止方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108862384A (zh) * 2018-08-23 2018-11-23 广东致远新材料有限公司 一种低锑氧化铌的制备方法和一种低锑氧化钽的制备方法

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