WO2019187407A1 - Agent d'extraction pour métaux et procédé d'extraction l'utilisant - Google Patents

Agent d'extraction pour métaux et procédé d'extraction l'utilisant Download PDF

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Publication number
WO2019187407A1
WO2019187407A1 PCT/JP2018/046870 JP2018046870W WO2019187407A1 WO 2019187407 A1 WO2019187407 A1 WO 2019187407A1 JP 2018046870 W JP2018046870 W JP 2018046870W WO 2019187407 A1 WO2019187407 A1 WO 2019187407A1
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WO
WIPO (PCT)
Prior art keywords
complex
metal
fluorine
tantalum
chlorine
Prior art date
Application number
PCT/JP2018/046870
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English (en)
Japanese (ja)
Inventor
寛幸 田辺
加藤　義人
泰輔 下垣内
佐藤　亮平
博人 井上
真行 黒滝
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株式会社アサカ理研
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Publication date
Application filed by 株式会社アサカ理研 filed Critical 株式会社アサカ理研
Publication of WO2019187407A1 publication Critical patent/WO2019187407A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
    • C07C49/04—Saturated compounds containing keto groups bound to acyclic carbon atoms
    • 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
    • C22B11/00—Obtaining noble metals
    • 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
    • C22B61/00—Obtaining metals not elsewhere provided for in this subclass
    • 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 metal extractant and an extraction method using the same.
  • 5-methyl-2-hexanone (commonly known as isoamyl methyl ketone or methyl isoamyl ketone (MIAK)) has been known to be used as a solvent for inks, pastes, paints, resists and the like (for example, patent documents) 1).
  • MIAK methyl isoamyl ketone
  • 5-methyl-2-hexanone is classified as a second petroleum, and the designated quantity that can be stored is as large as 1000 liters compared to the 200 liters of the first petroleum. Development of applications is desired.
  • an object of the present invention is to provide a new use of 5-methyl-2-hexanone.
  • the present inventors have found that a metal complex capable of forming a chlorine complex or a fluorine complex or a chlorine complex of the metal from an aqueous solution of the fluorine complex or an aqueous solution of the fluorine complex.
  • the inventors have found that the present invention is useful as a metal extractant for extracting a fluorine complex and has reached the present invention.
  • the metal extractant of the present invention contains 5-methyl-2-hexanone, and can form a chlorine complex or a fluorine complex. It is used for extracting a complex.
  • a metal extractant containing 5-methyl-2-hexanone is added to the chlorine complex aqueous solution or the fluorine complex aqueous solution of a metal capable of forming a chlorine complex or a fluorine complex, thereby adding the aqueous solution. From the above, a chlorine complex or a fluorine complex of the metal can be extracted.
  • the extraction method of the present invention comprises a metal complex capable of forming a chlorine complex or a fluorine complex or an aqueous solution of the chlorine complex or fluorine complex of the metal, and the metal complex or fluorine complex containing 5-methyl-2-hexanone as an active ingredient.
  • the extraction is performed using an extraction solvent.
  • the metal that can form the chlorine complex is, for example, gold or rhenium
  • the metal that can form the fluorine complex is, for example, tantalum or niobium.
  • money or rhenium extraction process by the metal extracting agent of this invention The flowchart which shows the extraction process of tantalum or niobium by the metal extracting agent of this invention.
  • the metal extractant of the present embodiment is composed of 5-methyl-2-hexanone (hereinafter abbreviated as MIAK), and the metal extract from the chlorine complex aqueous solution or the fluorine complex aqueous solution of a metal capable of forming a chlorine complex or a fluorine complex. It is used to extract a chlorine complex or a fluorine complex.
  • MIAK 5-methyl-2-hexanone
  • the metal that can form the chlorine complex is, for example, gold or rhenium
  • the metal that can form the fluorine complex is, for example, tantalum or niobium.
  • a method of extracting the metal chlorine complex from the chlorine complex aqueous solution of a metal capable of forming a chlorine complex and recovering the metal particles is as follows. This will be described as an example.
  • an aqueous solution of chloroauric acid (HAuCl 4 ), which is a gold chlorine complex, is prepared.
  • An aqueous solution of chloroauric acid can be obtained, for example, by dissolving a raw material containing gold in aqua regia or 6-6.5N hydrochloric acid.
  • MIAK is added to the aqueous solution of chloroauric acid, and chloroauric acid is extracted into MIAK. At this time, metal complexes other than chloroauric acid are also extracted in MIAK.
  • MIAK substantially contains only chloroauric acid.
  • an alkaline aqueous solution is added to MIAK to generate gold hydroxide (Au (OH) 3 ), and the generated gold hydroxide is moved to the aqueous phase.
  • the aqueous solution containing gold hydroxide is separated from MIAK by oil-water separation.
  • the metal capable of forming a chlorine complex is a metal other than gold, such as rhenium
  • the metal chlorine complex is extracted by MIAK in the same manner as in the case of gold shown in FIG.
  • the metal particles can be recovered by the same procedure as in the case.
  • the metal is tantalum and niobium. A case will be described as an example.
  • the metal capable of forming the fluorine complex is tantalum (Ta) and niobium (Nb)
  • fluorinated tantalum acid H 2 TaF 7
  • niobium fluoride H 2 NbF 7
  • the aqueous solution is obtained by, for example, finely grinding an ore containing tantalum and niobium with a ball mill or the like, and using the obtained fine ore as a base. It can be obtained by dissolving in an acid and adjusting the fluoride ion concentration and sulfate ion concentration by adding sulfuric acid.
  • MIAK is added to the mixed aqueous solution of fluorinated tantalum acid and niobium fluoride to extract the tantalum fluoride and niobium fluoride into MIAK.
  • the tantalum MIAK solution obtained in STEP 15 is extracted into an aqueous solution by adding water in STEP 16. Next, oil-water separation is performed at STEP 17 to obtain MIAK (STEP 18) not containing tantalum and an aqueous solution of tantalum (STEP 19). The MIAK obtained in STEP 18 can be collected and reused.
  • tantalum hydroxide can be recovered as tantalum oxide (Ta 2 O 5 ) by filtering the precipitate of tantalum hydroxide in STEP 21 and calcining the obtained tantalum hydroxide in STEP 22 (STEP 23).
  • niobium hydroxide Nb (OH) 5
  • Nb (OH) 5 niobium hydroxide
  • STEP 26 the precipitation of niobium hydroxide is filtered at STEP 26, and the obtained niobium hydroxide is calcined at STEP 27, so that niobium can be recovered as niobium oxide (Nb 2 O 5 ) (STEP 28).
  • STEP 13 to 15 may be performed after STEP 12 without performing STEP 13 to 15. Further, when an aqueous solution containing only niobium fluoride is prepared in STEP 11, after STEP 12, the operations in STEP 25 to 28 may be performed without performing the operations in STEP 13 to 24.
  • the metal capable of forming the fluorine complex is a metal other than tantalum or niobium
  • the metal fluorine complex is extracted by MIAK in the same manner as in the case of tantalum or niobium shown in FIG.
  • the metal can be recovered as an oxide by the same procedure as in the case of niobium.
  • Example 1 In this example, first, a commercially available standard solution for atomic absorption analysis (manufactured by Wako Pure Chemical Industries, Ltd.) having a gold concentration of 1000 mg / liter was dispensed into a plurality of containers in a volume of 10 ml. Next, hydrochloric acid and water are added to each container, and the chlorine ion concentration in each container becomes a different concentration in the range of 0 to 10 mol / liter, and the total liquid volume is 50 milliliters (50 mg / liter in gold concentration). A plurality of sample solutions containing chloroauric acid as a gold chloride complex were prepared. Each sample solution was. The chlorine ion concentration of each sample solution was measured by an ion chromatograph.
  • each sample solution and MIAK were dispensed in the same volume and sealed in a sealed container.
  • the initial mass A of gold in each sample solution was calculated by the following equation (1).
  • Mass B after stirring gold in sample solution Gold concentration after stirring sample solution ⁇ Volume of sample solution (2) And the extraction rate of gold
  • FIG. 3 shows the extraction rate of gold with respect to the chloride ion concentration.
  • Example 2 the extraction rate of rhenium relative to the chlorine ion concentration was calculated in exactly the same manner as in Example 1 except that rhenium was used instead of gold.
  • the extraction rate of rhenium with respect to the chlorine ion concentration is shown in FIG.
  • Example 3 In this example, first, a commercially available standard solution for atomic absorption analysis (manufactured by Wako Pure Chemical Industries, Ltd.) having a tantalum concentration of 1000 mg / liter was dispensed into a plurality of containers 0.5 ml each. Next, hydrofluoric acid and sulfuric acid are added to each container, and the concentration of fluorine ions in each container is in the range of 0 to 5 mol / liter, and the concentration is different in the range of sulfate ion concentration in the range of 0 to 4 mol / liter.
  • a plurality of sample solutions containing fluorinated tantalum acid as a tantalum fluorine complex were prepared by adjusting the total liquid volume to 50 milliliters (10 mg / liter tantalum concentration).
  • the fluorine ion concentration and the sulfate ion concentration of each sample solution were measured by an ion chromatograph.
  • each sample solution and MIAK were dispensed in the same volume and sealed in a sealed container.
  • the initial mass A of tantalum in each sample solution was calculated by the following equation (4).
  • Mass after stirring of tantalum in sample solution B Concentration of tantalum after stirring of sample solution ⁇ Volume of sample solution (5) And the extraction rate of the tantalum with respect to a fluorine ion concentration and a sulfate ion concentration was computed by following Formula (6).
  • Extraction rate (%) ⁇ (AB) / A ⁇ ⁇ 100 (6)
  • the extraction rate of tantalum with respect to the fluorine ion concentration and the sulfate ion concentration is shown in FIG.
  • Example 4 the extraction rate of niobium with respect to the fluorine ion concentration and the sulfate ion concentration was calculated in exactly the same manner as in Example 3 except that niobium was used instead of tantalum.
  • FIG. 6 shows the extraction rate of niobium with respect to the fluorine ion concentration and the sulfate ion concentration.
  • the metal chlorine complex or fluorine complex is formed from the chlorine complex aqueous solution or the fluorine complex aqueous solution of a metal capable of forming a chlorine complex or fluorine complex. It is clear that it can be extracted.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne une nouvelle utilisation de la 5-méthyl-2-hexanone. Un agent d'extraction pour métaux contient de la 5-méthyl-2-hexanone en tant que principe actif, et peut être utilisé pour l'extraction d'un complexe de chlore ou d'un complexe de fluor d'un métal apte à former un complexe de chlore ou un complexe de fluor à partir d'une solution aqueuse du complexe de chlore du métal ou d'une solution aqueuse du complexe de fluor du métal.
PCT/JP2018/046870 2018-03-26 2018-12-19 Agent d'extraction pour métaux et procédé d'extraction l'utilisant WO2019187407A1 (fr)

Applications Claiming Priority (2)

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JP2018057834A JP6427698B1 (ja) 2018-03-26 2018-03-26 抽出方法
JP2018-057834 2018-03-26

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6996798B1 (ja) * 2021-05-31 2022-01-17 株式会社アサカ理研 酸化タンタルの製造方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63235435A (ja) * 1987-03-24 1988-09-30 Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk 金属タンタルの製造方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1417483A (en) * 1973-01-06 1975-12-10 Ciba Geigy Ag Hydrazide salts
JPS63199831A (ja) * 1987-02-16 1988-08-18 Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk 金属Ｔｉ、Ｚｒ、Ｈｆ、Ｎｂ及びＴａの製造方法
US5425855A (en) * 1994-04-08 1995-06-20 Lloyd Berg Separation of ethyl benzene from p-xylene by extractive distillation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63235435A (ja) * 1987-03-24 1988-09-30 Nishimura Watanabe Chiyuushiyutsu Kenkyusho:Kk 金属タンタルの製造方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
NETE. M. ET AL.: "Separation and isolation of tantalum and niobium from tantalite using solvent extraction and ion exchange", HYDROMETALLURGY, vol. 149, 22 July 2014 (2014-07-22), pages 31 - 40, XP055639189 *
PURCELL, W. ET AL.: "Possible methodology for niobium, tantalum and scandium separation in ferrocolumbite", MINERALS ENGINEERING, vol. 119, 4 February 2018 (2018-02-04), pages 57 - 66, XP055639193 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6996798B1 (ja) * 2021-05-31 2022-01-17 株式会社アサカ理研 酸化タンタルの製造方法

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JP2019167604A (ja) 2019-10-03

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