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WO2025205842A1 - Procédé de production d'un composé de scandium - Google Patents

Procédé de production d'un composé de scandium

Info

Publication number
WO2025205842A1
WO2025205842A1 PCT/JP2025/011857 JP2025011857W WO2025205842A1 WO 2025205842 A1 WO2025205842 A1 WO 2025205842A1 JP 2025011857 W JP2025011857 W JP 2025011857W WO 2025205842 A1 WO2025205842 A1 WO 2025205842A1
Authority
WO
WIPO (PCT)
Prior art keywords
scandium
acidic solution
chelating resin
amount
chromium
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.)
Pending
Application number
PCT/JP2025/011857
Other languages
English (en)
Japanese (ja)
Inventor
寛人 渡邉
達也 檜垣
雅子 末包
広人 加地
啓司 大塚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Mining Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Publication of WO2025205842A1 publication Critical patent/WO2025205842A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • 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
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • C22B59/00—Obtaining rare earth metals
    • 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 method for producing scandium compounds by subjecting an acidic solution containing scandium and chromium-containing impurities to an ion exchange treatment using a chelating resin.
  • Scandium is extremely useful as an additive to high-strength aluminum alloys and as an electrode material for fuel cells, but its use has been limited due to its low production volume and high cost.
  • Nickel oxide ores such as laterite and limonite, are known to contain trace amounts of scandium. However, because nickel oxide ores have a low nickel content, recovering the nickel is costly. For this reason, they have only been used for purposes other than dry smelting, in which they are melted at high temperatures in a furnace to obtain ferronickel, an alloy of iron and nickel, which is used as a raw material for stainless steel.
  • a neutralizing agent is added to the leachate obtained from the leaching process to separate impurities, and then a sulfiding agent is added to recover nickel as nickel sulfide.
  • the recovered nickel sulfide can then be processed in an existing nickel refining process to obtain nickel salt compounds such as electrolytic nickel and nickel sulfate.
  • the scandium contained in the nickel oxide ore becomes contained in the leachate along with the nickel.
  • a neutralizing agent is then added to the resulting leachate to separate impurities, and a sulfurizing agent is then added to perform a sulfurization treatment.
  • Nickel is recovered as nickel sulfide, while scandium remains in the acidic solution after the sulfurizing agent has been added. Therefore, using the HPAL process makes it possible to effectively separate nickel and scandium.
  • the scandium separated by the HPAL process is dilute and contains a wide variety of impurities. Therefore, further purification is required to concentrate and recover the scandium by separating it from the impurities.
  • This purification process is the method using a chelating resin, as disclosed in Patent Document 2.
  • Patent Document 2 involves first selectively leaching nickel and scandium from nickel oxide ore in an acidic solution under high temperature and pressure in an oxidizing atmosphere to obtain a leachate, then adjusting the pH of the leachate to 2-4 and using a sulfiding agent to selectively precipitate and recover nickel as a sulfide. Next, the resulting post-sulfidation liquid after nickel recovery is brought into contact with a chelating resin to adsorb scandium, and the chelating resin is washed with dilute acid. After washing, the chelating resin is then brought into contact with a strong acid to elute the scandium.
  • the impurities contained in nickel oxide ore are known to include elements such as iron, aluminum, chromium, manganese, and magnesium, although the type and amount vary depending on the region where it is produced.
  • Patent Document 3 discloses a method for eluting chromium from a chelating resin using a sulfuric acid solution with a higher concentration than the sulfuric acid solution used to elute scandium.
  • the ion exchange process includes an adsorption process in which the post-sulfurization solution is brought into contact with a chelating resin to adsorb scandium onto the chelating resin; a scandium elution process in which a sulfuric acid solution of 0.3N or more but less than 3N is brought into contact with the chelating resin to obtain a scandium eluate; and a chromium removal process in which a sulfuric acid solution of 3N or more is brought into contact with the chelating resin that has undergone the scandium elution process to remove the chromium adsorbed onto the chelating resin.
  • the method disclosed in Patent Document 3 involves adsorbing the impurity chromium along with scandium onto a chelating resin, and then utilizing differences in the concentrations of the sulfuric acid solutions used for elution to elute only scandium from the chelating resin while the chromium remains adsorbed to the chelating resin, thereby separating it from the chromium.
  • this method is based on the premise that the impurity chromium is also adsorbed onto the chelating resin, and as a result, the amount of adsorbed impurities, including chromium, can increase, which can increase the processing load in the elution process.
  • Patent Document 4 proposes a method of increasing the amount of scandium recovered by contacting an acidic solution containing scandium and chromium with a chelating resin at a predetermined temperature to reduce the amount of chromium adsorbed. This method is useful because it reduces the amount of impurities, including chromium, adsorbed to the chelating resin, thereby preventing an increase in the processing load in the elution process.
  • the present invention therefore aims to provide a method for more effectively adsorbing scandium by reducing the amount of chromium adsorbed onto a chelating resin during ion exchange treatment of an acidic solution containing at least scandium and chromium using a chelating resin.
  • the value of the flow rate BV of the acidic solution at which max,Sc is obtained is set as an upper limit, and the flow rate BV of the acidic solution is set to a range from the lower limit to the upper limit.
  • a third aspect of the present invention is a method for producing a scandium compound according to the first or second aspect of the present invention, wherein the concentration of scandium contained in the acidic solution is 10 mg/L or more.
  • a fourth aspect of the present invention is a method for producing a scandium compound, wherein the compound production step involves producing a precipitate containing scandium from the scandium eluate and roasting the precipitate to produce scandium oxide.
  • the amount of chromium-containing impurities adsorbed onto the chelating resin can be reduced, allowing scandium to be more effectively adsorbed.
  • 1 is a graph showing the relationship between the metal ion concentration in the eluate recovered from the column after passing an acidic solution through a chelating resin, and the amount of metal ions adsorbed onto the chelating resin, based on the test results of an ion exchange treatment.
  • 1 is a graph showing breakthrough curves based on the measurement results of scandium leakage rate under treatment conditions of a liquid flow rate BV of 35 and a liquid flow rate BV of 50 in an ion exchange treatment test.
  • the method for producing a scandium compound according to this embodiment is a method for producing a scandium compound from an acidic solution containing at least scandium and chromium.
  • the acidic solution may be a solution obtained by subjecting nickel oxide ore to leaching with a sulfuric acid solution, and then adding a sulfurizing agent to the resulting leachate to separate nickel sulfide.
  • the ion exchange treatment process is characterized by adjusting the temperature of the acidic solution to a range of 15°C to 45°C and passing it through a column packed with a chelating resin, and by setting the range of the amount of acidic solution passed through the chelating resin (BV) as follows, causing scandium to be adsorbed onto the chelating resin.
  • BV chelating resin
  • the temperature of the acidic solution passed through the chelating resin is adjusted to a temperature range of 15°C or higher and 45°C or lower, and the flow rate BV of the acidic solution is set to a range from a specific lower limit to an upper limit based on its relationship with the amount of scandium adsorbed.
  • the acidic solution to be treated is a solution containing scandium that is recovered by adsorption onto a chelating resin in the ion exchange treatment step.
  • the acidic solution also contains at least chromium as an impurity.
  • the acidic solution to be treated is not particularly limited, but preferably has a scandium concentration of 10 mg/L or more.
  • An acidic solution with a scandium concentration of 10 mg/L or more can be suitably treated using the ion exchange treatment process described below.
  • the concentration of chromium, an impurity, in the acidic solution is not particularly limited, but is preferably 0.1 mg/L or more and 500 mg/L or less.
  • the hydrometallurgical process for nickel oxide ore can be carried out using known methods, but will be briefly described below.
  • the hydrometallurgical process comprises a leaching step in which nickel oxide ore is leached with a sulfuric acid solution under high temperature and pressure to obtain a leachate; a neutralization step in which a neutralizing agent is added to the leachate to obtain a neutralized precipitate containing impurities and a neutralized solution; and a sulfurization step in which a sulfurizing agent is added to the neutralized solution to obtain nickel sulfide and a sulfurized solution.
  • the sulfurized solution recovered from the sulfurization step is a sulfuric acid solution containing impurities including scandium and chromium.
  • the leaching process is a process in which a sulfuric acid solution is added to a slurry of nickel oxide ore using, for example, a high-temperature pressurized vessel (autoclave), and the mixture is stirred under high temperature and high pressure to produce a leached slurry consisting of a leachate and a leach residue.
  • the resulting leach slurry consisting of the leachate and the leach residue is washed and subjected to solid-liquid separation into a leachate containing nickel, cobalt, scandium, etc. and a leach residue mainly containing hematite.
  • Nickel oxide ores mainly include so-called laterite ores such as limonite and saprolite. These nickel oxide ores contain scandium.
  • the neutralization step is a step in which a neutralizing agent is added to the obtained leachate to adjust the pH, thereby obtaining a neutralized precipitate containing impurities and a neutralized solution.
  • a neutralizing agent a conventionally known agent can be used, and examples thereof include calcium carbonate, slaked lime, and sodium hydroxide.
  • a sulfurizing agent such as hydrogen sulfide gas, sodium sulfide, or sodium hydrosulfide is added to the resulting neutralized liquid to produce sulfides containing nickel and cobalt with few impurities, and a post-sulfurization liquid containing scandium with a stabilized nickel concentration at a low level.
  • the slurry containing nickel sulfide is subjected to a sedimentation separation process using a thickener or the like to separate and recover the nickel sulfide, while the post-sulfurization liquid containing scandium is allowed to overflow and be recovered.
  • the manufacturing method according to the present embodiment includes an ion exchange treatment step in which an acidic solution containing scandium and impurities including chromium is passed through a column packed with an iminodiacetic acid type chelating resin, thereby causing the scandium contained in the acidic solution to be adsorbed onto the chelating resin.
  • the adsorption step is a step in which the acidic solution is passed through a column packed with a chelating resin to bring it into contact with the chelating resin, thereby adsorbing scandium in the acidic solution onto the chelating resin.
  • iminodiacetic acid-type chelating resins also have a relatively high selectivity for chromium, particularly in the form of trivalent chromium ions (Cr 3+ ), among other impurities. Therefore, chromium may be adsorbed onto the adsorption sites before scandium, resulting in a decrease in the amount of scandium adsorbed. Furthermore, scandium adsorbed onto the chelating resin may begin to be replaced by chromium during treatment.
  • the acidic solution passed through the chelating resin is adjusted to a temperature range of 15°C or higher and 45°C or lower, and lower and upper limits for the amount of liquid passed through BV are set, so that the amount of liquid passed through BV of the acidic solution passed through the chelating resin falls within the range from the lower limit to the upper limit.
  • the upper limit of the flow rate BV through the chelating resin is the flow rate of the acidic solution at which q max,Sc is the maximum amount of scandium adsorbed onto the chelating resin.
  • the iminodiacetic acid type chelating resin used was Diaion CR11, a product name of Mitsubishi Chemical Corporation, and 15 mL of this chelating resin was packed into a column.
  • the temperature of the acidic solution when passing through the chelating resin was set to two conditions: 23°C and 60°C, and tests were conducted under each condition.
  • SV is a unit that represents the amount of acidic solution passed per hour as a multiple of the volume of the chelating resin in the column.
  • Figure 1 is a graph showing the relationship between the metal ion concentration in the eluate recovered from the column after passing an acidic solution through a chelating resin at a flow rate BV of 50 and the amount of metal ion adsorbed onto the chelating resin, based on the results of an ion exchange treatment test.
  • the eluate is the solution that emerges from the column after passing an acidic solution through the chelating resin, and is also referred to as the post-passage solution.
  • the metal ions located on the upper left side have larger apparent distribution coefficients Dapp ,i , which means that they have higher selectivity to the chelating resin.
  • the test results shown in the graph of Figure 1 show that scandium (Sc) has the highest selectivity to the chelating resin at a temperature of 23°C, and chromium (Cr) has the highest selectivity to the chelating resin at a temperature of 60°C.
  • the amount of scandium adsorbed onto the chelating resin can be calculated from the breakthrough curve, which shows the relationship between the leakage rate at that time and the amount of acidic solution passed through BV during the ion exchange process.
  • 2A is a graph obtained from the above-mentioned ion exchange treatment test, and is a graph of a breakthrough curve based on the measurement results of the scandium leakage rate under treatment conditions where the liquid flow rate BV is 35 and the measurement results of the scandium leakage rate under treatment conditions where the liquid flow rate BV is 50.
  • the leakage rate is 100%, and the shaded area in the graph represents the maximum amount of scandium adsorbed to the chelating resin.
  • the maximum adsorption amount is represented as "q max,Sc .”
  • the amount of scandium adsorbed onto the chelating resin depends on the flow rate BV of the acidic solution. From this, it is possible to determine the adsorption efficiency of scandium onto the chelating resin under treatment conditions of a given flow rate BV. That is, the adsorption efficiency of scandium onto the chelating resin can be determined from the relationship between the ratio of the amount of scandium adsorbed (q Sc ) at a given flow rate BV to the maximum amount of scandium adsorbed (q max,Sc ). Specifically, the adsorption efficiency of scandium onto the chelating resin is expressed by the ratio "q Sc /q max,Sc , " and the larger this ratio, the higher the adsorption efficiency of scandium.
  • the flow rate BV it is preferable to set the flow rate BV so that the ratio of the amount of scandium adsorbed (q Sc ) at a given flow rate BV to the maximum amount of scandium adsorbed ( q max,Sc ) is 0.5 or more.
  • the temperature condition during flow that results in a low scandium leakage rate and a high amount of adsorption to the chelating resin is in the range of 15°C to 45°C.
  • a range of 20°C to 40°C is also preferred, and a range of 23°C to 40°C is even more preferred.
  • the scandium eluate obtained from the elution step may be used, and the scandium eluate may be brought into contact with the chelating resin to elute the scandium. This makes it possible to increase the concentration of scandium contained in the scandium eluate.
  • the compound production step is a step of producing a scandium compound from the scandium eluate obtained through the ion exchange treatment step.
  • the scandium contained in the scandium eluate can be converted into the form of scandium oxide.
  • scandium compounds can be produced by known methods using a scandium eluent.
  • a scandium hydroxide precipitate can be produced by adding an alkali to the scandium eluent and performing a neutralization treatment.
  • a scandium oxalate precipitate can be produced by performing an oxalation treatment on the scandium eluent.
  • methods using oxalation treatment can more effectively separate impurities and produce scandium compounds containing high-purity scandium.
  • the scandium hydroxide or scandium oxalate obtained as described above is subjected to a roasting process.
  • the roasting process involves washing the scandium oxalate precipitate obtained, for example, by oxalation treatment, with water, drying, and then roasting.
  • This roasting process can convert scandium into extremely pure scandium oxide.
  • the roasting conditions are not particularly limited, but for example, the material can be placed in a tubular furnace and heated to approximately 900°C for approximately two hours.
  • the scandium eluate obtained through the ion exchange process may be subjected to purification processes such as solvent extraction and neutralization.
  • purification processes such as solvent extraction and neutralization.
  • impurities contained in the scandium eluate can be selectively extracted into an organic solvent containing an extractant, thereby purifying the scandium eluate and obtaining a solution with concentrated scandium.
  • ⁇ Ion exchange treatment> In order to produce a scandium compound from an acidic solution containing scandium (Sc) and impurities including chromium (Cr), the acidic solution was subjected to an ion exchange treatment using a chelating resin. Specifically, a solution containing scandium and impurities including chromium, having the composition shown in Table 2 below, was prepared, and the acidic solution was passed through an iminodiacetic acid type chelating resin to perform an ion exchange treatment.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne une technologie qui supprime la quantité de chrome adsorbée sur une résine chélatée pendant un traitement d'échange d'ions effectué sur une solution acide contenant du scandium et du chrome à l'aide de la résine chélatée, ce qui permet d'obtenir une adsorption plus efficace du scandium.　La présente invention comprend une étape de traitement par échange d'ions dans laquelle une solution acide qui contient du scandium et des impuretés comprenant du chrome est amenée à passer à travers une colonne remplie d'une résine chélatée de type acide iminodiacétique de façon à amener le scandium à être adsorbé sur la résine chélatée. Dans l'étape de traitement par échange d'ions, la solution acide est amenée à une température dans la plage de 15 °C à 45 °C. Lorsque la quantité d'adsorption du scandium sur la résine chélatée est qSc et que la quantité maximale d'adsorption du scandium sur la résine chélatée est qmax, Sc, la quantité BV de solution acide qui passe à laquelle qSc/qmax, Sc = 0,5 est définie comme valeur limite inférieure, et la quantité BV de solution acide qui passe lorsque la quantité maximale d'adsorption du scandium sur la résine chélatée, c'est-à-dire qmax, Sc, est atteinte est définie comme valeur limite supérieure, et la quantité BV de solution acide qui passe est fixée dans une plage comprise entre la valeur limite inférieure et la valeur limite supérieure.
PCT/JP2025/011857 2024-03-29 2025-03-25 Procédé de production d'un composé de scandium Pending WO2025205842A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2024057955A JP2025154769A (ja) 2024-03-29 2024-03-29 スカンジウム化合物の製造方法
JP2024-057955 2024-03-29

Publications (1)

Publication Number Publication Date
WO2025205842A1 true WO2025205842A1 (fr) 2025-10-02

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PCT/JP2025/011857 Pending WO2025205842A1 (fr) 2024-03-29 2025-03-25 Procédé de production d'un composé de scandium

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JP (1) JP2025154769A (fr)
WO (1) WO2025205842A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014177391A (ja) * 2013-02-15 2014-09-25 Sumitomo Metal Mining Co Ltd スカンジウムの回収方法
JP2017210675A (ja) * 2016-05-27 2017-11-30 住友金属鉱山株式会社 スカンジウムの回収方法
WO2018101039A1 (fr) * 2016-11-30 2018-06-07 住友金属鉱山株式会社 Procédé de traitement par échange d'ions et procédé de récupération de scandium
WO2021059940A1 (fr) * 2019-09-24 2021-04-01 住友金属鉱山株式会社 Procédé de récupération de scandium, et procédé d'échange d'ions
WO2021059941A1 (fr) * 2019-09-24 2021-04-01 住友金属鉱山株式会社 Procédé de récupération de scandium et procédé de traitement par échange d'ions

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014177391A (ja) * 2013-02-15 2014-09-25 Sumitomo Metal Mining Co Ltd スカンジウムの回収方法
JP2017210675A (ja) * 2016-05-27 2017-11-30 住友金属鉱山株式会社 スカンジウムの回収方法
WO2018101039A1 (fr) * 2016-11-30 2018-06-07 住友金属鉱山株式会社 Procédé de traitement par échange d'ions et procédé de récupération de scandium
WO2021059940A1 (fr) * 2019-09-24 2021-04-01 住友金属鉱山株式会社 Procédé de récupération de scandium, et procédé d'échange d'ions
WO2021059941A1 (fr) * 2019-09-24 2021-04-01 住友金属鉱山株式会社 Procédé de récupération de scandium et procédé de traitement par échange d'ions

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