WO2018038058A1 - スカンジウムの精製方法、スカンジウム抽出剤 - Google Patents
スカンジウムの精製方法、スカンジウム抽出剤 Download PDFInfo
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- WO2018038058A1 WO2018038058A1 PCT/JP2017/029807 JP2017029807W WO2018038058A1 WO 2018038058 A1 WO2018038058 A1 WO 2018038058A1 JP 2017029807 W JP2017029807 W JP 2017029807W WO 2018038058 A1 WO2018038058 A1 WO 2018038058A1
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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
- C22B59/00—Obtaining rare earth metals
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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
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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
- 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
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/381—Phosphines, e.g. compounds with the formula PRnH3-n, with n = 0-3
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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
- 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
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
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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
- 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
- C22B3/40—Mixtures
- C22B3/408—Mixtures using a mixture of phosphorus-based acid derivatives of different types
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- 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 recovering scandium, for example, a method for purifying scandium by separating impurities including iron from an acidic solution containing scandium produced in a hydrometallurgical process of nickel oxide ore. .
- rare earth elements is scandium.
- nickel oxide ores such as laterite ores are known to contain trace amounts of scandium, and scandium contained in nickel oxide ores is leached under pressure by adding sulfuric acid to nickel oxide ores. Can be recovered from the leachate obtained by
- Patent Document 1 discloses (a) a leaching step of leaching an oxide ore with an acid under high temperature and high pressure to obtain a leachate containing nickel and scandium; and (a) adding a neutralizing agent to the leachate to adjust the pH to 2 By adjusting to the range of ⁇ 4, the first neutralization step of removing iron and aluminum in the leachate as precipitates, and (c) neutralizing the solution after removing the precipitates in the first neutralization step A second neutralization step of recovering scandium in the solution as a precipitate by adjusting the pH to a range of more than 4 to 7.5 by adding an agent, and (d) adding a neutralizing agent to adjust the pH to 7. It has been shown that nickel and scandium can be recovered from oxide ore by performing a third neutralization step of recovering nickel in the solution as a precipitate by adjusting to more than 5.
- Patent Document 2 there is a method described in Patent Document 2 as a method for selectively separating only scandium by means such as solvent extraction.
- an organic solvent is added to a scandium-containing solution in an aqueous phase containing at least one of iron, aluminum, calcium, yttrium, manganese, chromium, and magnesium in addition to scandium, and the scandium component is added to the organic solvent.
- To extract in order to separate the trace component extracted together with scandium in the organic solvent, scrubbing by adding an aqueous hydrochloric acid solution, removing the trace component, adding an aqueous sodium hydroxide solution in the organic solvent, The remaining scandium is made into a slurry containing Sc (OH) 3.
- Sc (OH) 3 obtained by filtering this slurry is dissolved with hydrochloric acid to obtain an aqueous scandium chloride solution, and oxalic acid is added thereto to form a scandium oxalate precipitate.
- impurities are separated into the filtrate, and then calcined to obtain high-purity scandium oxide.
- Patent Document 3 by utilizing a cooperative effect, a mixture of two or more kinds of extractants can be used in a higher yield than the case where one kind of extractant is used alone, from an electroless nickel waste liquid.
- a method for recovering nickel has been proposed. According to this Patent Document 3, when one kind of extractant is used alone, nickel can hardly be extracted, but by using two or more kinds of extractants in combination, without adjusting the pH, It is said that 98% to 99% of nickel can be recovered by one batch extraction.
- Patent Document 4 proposes a method of extracting cobalt and manganese from a mixed solution of cobalt, manganese, calcium and magnesium by mixing a carboxylic acid-based extractant and an oxime-based extractant.
- Patent Document 3 nor Patent Document 4 has a report on the extraction behavior of scandium, and only scandium is selectively extracted and separated from a solution (leaching solution) obtained by acid leaching of nickel oxide ore. No possible solvent has been found.
- the present invention has been proposed in view of such circumstances, and a method for efficiently purifying scandium by separating scandium and impurities from an acidic solution containing scandium and containing iron.
- the purpose is to provide.
- the present inventors have intensively studied to solve the above-mentioned problems. As a result, it has been found that scandium can be selectively extracted by performing solvent extraction using a mixed extractant containing a phosphate extractant and a neutral extractant, and the present invention has been completed.
- an acidic solution containing scandium and at least an elemental component containing iron is used as a solvent by a mixed extractant containing a phosphate extractant and a neutral extractant.
- This is a method for purifying scandium, which is subjected to extraction to extract scandium from the acidic solution.
- the second invention of the present invention is the method for purifying scandium according to the first invention, wherein the phosphate extractant is 2-ethylhexylphosphonic acid-1-ethylhexyl.
- the third invention of the present invention is a method for purifying scandium according to the first or second invention, wherein the neutral extractant is tri-n-octylphosphine oxide.
- the phosphoric acid extractant in any one of the first to third aspects, is mixed in a molar ratio of 5% to 50%. Is a method for purifying scandium.
- the pH of the acidic solution is adjusted to a range of 0.0 or more and 2.0 or less, and the acid after pH adjustment is adjusted.
- This is a method for purifying scandium, wherein the solution is subjected to the solvent extraction.
- the acidic solution is a solution obtained by leaching scandium by adding an acid to nickel oxide ore, or a scandium oxide or A solution obtained by dissolving scandium hydroxide with an acid, adjusting the pH of the acidic solution to a range of 0.0 to 2.0, and subjecting the acidic solution after pH adjustment to the solvent extraction
- This is a method for purifying scandium.
- the seventh invention of the present invention is a scandium purification method according to any one of the first to sixth inventions, wherein the acidic solution further contains at least one of zirconium and thorium.
- the eighth invention of the present invention is an extractant for extracting scandium from an acidic solution containing elemental components containing at least iron and containing scandium, and a phosphate extractant; A scandium extractant containing a neutral extractant.
- a ninth invention of the present invention is the scandium extractant according to the eighth invention, wherein the phosphoric acid extractant is contained in a molar ratio of 5% to 50%.
- scandium can be efficiently purified from an acidic solution containing scandium and impurities containing iron.
- FIG. It is a figure which shows the relationship between pH and an extraction rate when mixed extractant (PC88A + TOPO) is used in Example 1.
- FIG. It is a figure which shows the relationship between pH and an extraction rate when the extractant which consists only of a neutral extractant (TOPO) in the comparative example 1 is used.
- TOPO neutral extractant
- PC88A phosphate type extractant
- FIG. It is a figure which shows the relationship between pH and a separation factor when the scandium extractant which is a mixed extractant in Example 1 is used.
- the scandium purification method is a method of extracting (recovering) scandium by extracting the scandium from an acidic solution containing scandium (Sc) by solvent extraction.
- scandium is extracted from an acidic solution containing scandium and containing an impurity element containing at least iron (Fe) while separating it from those impurities.
- a mixed extract containing a phosphate extractant and a neutral extractant was used for an acidic solution containing scandium and an impurity element containing at least iron. It is characterized by extracting scandium from the acidic solution by subjecting it to solvent extraction.
- At least iron-containing impurities, scandium, and impurity elements can be efficiently separated, and only scandium can be selectively extracted.
- scandium can be extracted with excellent selectivity even in acidic solutions with a low pH range. Can do.
- scandium can be extracted selectively by separating efficiently from impurities, the amount of neutralizing agent used in the neutralization treatment for the acidic solution can be effectively reduced. It is possible to prevent the product from being generated.
- An acidic solution containing scandium (hereinafter simply referred to as “acidic solution”) is a solution to be subjected to solvent extraction treatment, and contains scandium and an impurity element containing at least iron.
- the acidic solution a solution obtained by leaching a valuable metal containing scandium by adding an acid such as sulfuric acid to nickel oxide ore in a hydrometallurgical process of nickel oxide ore can be given.
- the acidic solution include a solution obtained by dissolving scandium oxide or scandium hydroxide with an acid such as sulfuric acid.
- Examples of the acid solution obtained by acid leaching of nickel oxide ore include, for example, a leachate obtained by acid leaching of nickel oxide ore, or a sulfiding agent added to the leachate to separate and remove nickel, cobalt, etc.
- a post-sulfurized solution after the treatment Specifically, the sulfidized solution is leached by adding an acid such as sulfuric acid to nickel oxide ore, and the obtained leached solution is neutralized using a neutralizing agent, and then hydrogen sulfide gas. This is a solution after adding a sulfurizing agent such as to cause a sulfurization reaction and separating and removing nickel and cobalt sulfides.
- the acidic solution obtained by acid leaching of such nickel oxide ore contains one or more elements of zirconium (Zr) and thorium (Th) in addition to iron.
- the mixed extractant contains a phosphate extractant and a neutral extractant.
- a mixed extractant is used to perform the solvent extraction process on the acidic solution described above.
- the phosphate extractant is not particularly limited, and examples thereof include 2-ethylhexylphosphonic acid-1-ethylhexyl.
- this phosphoric acid type extractant the brand name PC88A by Daihachi Chemical Industry Co., Ltd. is marketed.
- the neutral extractant is not particularly limited, and examples thereof include tri-n-octylphosphine oxide.
- the brand name TOPO etc. by Dojin Chemical Co., Ltd. is marketed.
- the ratio of the phosphoric acid extractant in the mixed extractant is preferably in the range of 5% to 50% in terms of molar ratio. Taking into account the ease of handling, it is more preferable that the molar ratio is in the range of 15% to 30%.
- the mixing ratio of the phosphoric acid extractant is in the range of 5% or more and 50% or less in terms of molar ratio, it is possible to more efficiently separate scandium and impurity elements including iron. Selectivity can be increased.
- an extractant other than the above-described phosphate extractant and neutral extractant may be included as long as the effect is not impaired.
- the extractant used for solvent extraction has a high viscosity, and if used as it is in the extraction process, there is an adverse effect on the operation such as poor phase separation from the aqueous phase. Therefore, in order to reduce the viscosity of the extractant, it is generally performed to dilute the extractant with a diluent.
- the diluent is not particularly limited as long as it can dissolve the mixed extractant to be used and the complex of scandium which is a rare earth element.
- examples thereof include chlorinated solvents such as chloroform and dichloromethane, aromatic hydrocarbons such as benzene, toluene and xylene, and aliphatic hydrocarbons such as hexane.
- chlorinated solvents such as chloroform and dichloromethane
- aromatic hydrocarbons such as benzene, toluene and xylene
- aliphatic hydrocarbons such as hexane.
- Such a diluent may be used individually by 1 type, and may mix and use 2 or more types.
- alcohols such as 1-octanol may be mixed and used.
- the acidic solution to be treated and the mixed extractant are mixed and stirred. Then, scandium ions are selectively extracted into the organic phase by separating the mixed solution of the acidic solution and the mixed extractant into an aqueous phase and an organic phase using a separatory funnel.
- the mixed extractant with the mixing ratio of the phosphate extractant in the range of 5% or more and 50% or less, the selectivity of scandium can be improved and the extraction can be performed more efficiently can do.
- the stirring operation in the solvent extraction treatment may be performed at a sufficient number of rotations such that the organic phase and the aqueous phase are not separated when the mixed extractant and the acidic solution are mixed.
- the stirring time is not particularly limited, but is preferably 20 minutes or more from the viewpoint of allowing scandium to be extracted from the acidic solution with a higher yield.
- an alkaline aqueous solution such as an aqueous sodium hydroxide solution is appropriately added to suppress the decrease in pH. It is preferable.
- the pH of the acidic solution to be treated it is preferable to adjust to a range of 0.0 or more and 2.0 or less, and 1.3 or more and 2.0 or less. It is more preferable to adjust, and it is particularly preferable to adjust to 1.7 to 2.0.
- an acidic solution containing a large amount of iron ions for example, a solution obtained by acid leaching of nickel oxide ore
- an acidic solution containing iron for example, a solution obtained by acid leaching of nickel oxide ore
- the pH exceeds 2.5 to 3.0
- rare earth elements such as scandium coprecipitate, and inclusions called clads are produced during the extraction process, making operation difficult.
- an acidic solution containing iron for example, when the pH is 2.5 or more, iron hydroxide is generated and phase separation is significantly deteriorated.
- the pH is adjusted to a range of 0.0 to 2.0, and after pH adjustment Solvent extraction is preferably performed on the acidic solution.
- scandium can be extracted at a sufficiently high extraction rate. It can be extracted and can be operated stably. In this way, after pH adjustment within a predetermined range, by subjecting the acidic solution after pH adjustment to solvent extraction, only scandium is purified from an acidic solution containing an impurity element including iron. And can be extracted in high yield.
- the mixed extractant used in Example 1 has a phosphate extractant (PC88A) molar concentration of 0.1 mol / L and a neutral extractant (TOPO) molar concentration of 0.5 mol / L.
- PC88A phosphate extractant
- TOPO neutral extractant
- the extractant used in Comparative Example 1 was obtained by dissolving in swazole so that the molar concentration of the neutral extractant (TOPO) was 0.5 mol / L.
- the extractant used in Comparative Example 2 was obtained by dissolving in swazole so that the molar concentration of the phosphate extractant (PC88A) was 0.6 mol / L.
- the extractant used in Comparative Examples 1 and 2 is a single extractant based on a phosphate extractant or a neutral extractant.
- Example 1 and Comparative Examples 1 and 2 a sulfuric acid solution (acidic solution) containing scandium (Sc), iron (Fe), and zirconium (Zr) or thorium (Th) at concentrations shown in Table 2 below, respectively. Prepared.
- Example 1 In Example 1, the sulfuric acid solution was divided into five 2.5 ml portions, and the pH of the sulfuric acid solution was adjusted to a constant value within the range of 0.0 to 2.0. Each sulfuric acid solution was mixed with 2.5 ml of a mixed extractant for extracting scandium (PC88A + TOPO), and the mixed solution was stirred at a rotational speed of 650 rpm for 20 minutes. At this time, in order to maintain the pH in the sulfuric acid solution at the same value as that before mixing with the mixed extractant, a 1 mol / L aqueous sodium hydroxide solution was appropriately added.
- PC88A + TOPO a mixed extractant for extracting scandium
- the aqueous phase and the organic phase of the mixed solution are separated with a separatory funnel, and the extraction residual liquid (aqueous phase) is subjected to elemental analysis using an induction plasma emission spectrometer (ICP-AES).
- ICP-AES induction plasma emission spectrometer
- Comparative Example 1 In Comparative Example 1, the sulfuric acid solution was divided into five 2.5 ml portions, and the pH of the sulfuric acid solution was adjusted to a constant value within the range of 0.0 to 2.5, and for scandium extraction. Except that a neutral extractant (TOPO) was used as the extractant, the extraction rate of various metals from the aqueous phase to the organic phase was determined in the same manner as in Example 1. Table 4 below and FIG. 1 show the relationship between pH and the extraction rate of various metals.
- TOPO neutral extractant
- Comparative Example 2 In Comparative Example 2, the sulfuric acid solution was divided into three 2.5 ml portions, and the pH of the sulfuric acid solution was adjusted to a constant value within the range of 0.0 to 1.0, and for scandium extraction. Except that a phosphoric acid-based extractant (PC88A) was used as the extractant, the extraction rate of various metals from the aqueous phase to the organic phase was determined in the same manner as in Example 1. Table 5 below and FIG. 1 show the relationship between the pH and the extraction rate of various metals.
- PC88A phosphoric acid-based extractant
- the pH of the acidic solution to be treated is 0.0 or more and 2.
- Scandium alone can be extracted at a high yield by subjecting it to solvent extraction in a state of being adjusted to 0 or less, preferably 1.7 or more and 2.0 or less.
- FIG. 4 shows the separation coefficient between scandium and impurity elements Fe 3+ and Zr 4+ when the mixed extractant is used in Example 1.
- FIG. 5 shows the separation coefficient between scandium and the impurity elements Fe 3+ and Zr 4+ when an extractant composed only of the neutral extractant is used in Comparative Example 1.
- the sulfuric acid solution that was the subject of solvent extraction treatment was pressure sulfuric acid leaching of the actual nickel oxide ore by a known method, and a sulfurizing agent was added to the obtained leachate to separate nickel and cobalt by a sulfurization reaction. Then, a sulfuric acid solution (post-sulfurized solution) was prepared. As shown in Table 7, this sulfuric acid solution contains scandium (Sc), and impurities such as aluminum (Al), chromium (Cr), thorium (Th), and trivalent iron (Fe); Contains trace amounts of residual nickel (Ni).
- the sulfuric acid solution was divided into six 30 ml portions, and the pH of the sulfuric acid solution was adjusted to a constant value within the range of 1.0 to 2.0.
- Each sulfuric acid solution was mixed with 30 ml of a mixed extractant for extracting scandium (PC88A + TOPO), and the mixed solution was stirred at a rotational speed of 650 rpm for 20 minutes.
- a 1 mol / L aqueous sodium hydroxide solution was appropriately added.
- the aqueous phase and the organic phase of the mixed solution are separated with a separatory funnel, and the extraction residual liquid (aqueous phase) is subjected to elemental analysis using an induction plasma emission spectrometer (ICP-AES).
- ICP-AES induction plasma emission spectrometer
- the extraction rate of various metals from the aqueous phase to the organic phase was determined.
- the relationship between pH and the extraction rate of various metals contained in nickel oxide ore is shown in Table 8 and FIG. 6 below for Example 2, and Table 9 and FIG.
- the solvent extraction operation was carried out using the same sulfuric acid solution (Table 7) as in Example 2 as the treatment target, and adjusting the pH of the sulfuric acid solution to three patterns of 1.0, 1.6, and 1.8, respectively. Performed in the same manner as 2. Then, the aqueous phase and the organic phase of the mixed solution are separated with a separatory funnel, and the elemental analysis using an induction plasma emission spectroscopic analyzer (ICP-AES) is performed on the extraction residual liquid (aqueous phase) to obtain various metals. The extraction rate from the aqueous phase to the organic phase was determined. Table 11 below and FIGS. 8 and 9 show the relationship between pH and the extraction rate of various metals.
- ICP-AES induction plasma emission spectroscopic analyzer
- Example 4 Solvent extraction with mixed extractants using other phosphate extractants >> [Example 4] As Example 4, the following mixed extractant was prepared and subjected to solvent extraction. That is, as shown in Table 12 below, di (2,4,4-trimethylpentyl) phosphinic acid (trade name: Cyanex 272) was used as the phosphate extractant, and the molar concentration of the phosphate extractant was 0. A mixed extractant was prepared by dissolving each extractant in swazole so that the molar concentration of 0.1 mol / L and neutral extractant (TOPO) was 0.5 mol / L.
- Table 12 di (2,4,4-trimethylpentyl) phosphinic acid (trade name: Cyanex 272) was used as the phosphate extractant, and the molar concentration of the phosphate extractant was 0.
- a mixed extractant was prepared by dissolving each extractant in swazole so that the molar concentration of 0.1 mol / L and neutral extractant (TO
- a sulfuric acid solution containing scandium (Sc), iron (Fe), and zirconium (Zr) at the concentrations shown in Table 13 below is prepared, and the sulfuric acid solution is divided into six 30 ml portions.
- the pH was adjusted to a constant value within the range of 1.0 to 2.0.
- Solvent extraction was performed in the same manner as in Example 1. Then, the aqueous phase and the organic phase of the mixed solution are separated with a separatory funnel, and the elemental analysis using an induction plasma emission spectroscopic analyzer (ICP-AES) is performed on the extraction residual liquid (aqueous phase) to obtain various metals. The extraction rate from the aqueous phase to the organic phase was determined. Table 14 below and FIG. 10 show the relationship between the pH and the extraction rate of various metals.
- ICP-AES induction plasma emission spectroscopic analyzer
- Example 4 From the results of Example 4, even with a mixed extractant using a phosphate-based extractant different from that used in Example 1, scandium and impurity elements can be efficiently separated, and scandium is highly purified. could be purified.
- FIG. 11 shows the separation coefficient between scandium and impurity elements Fe 3+ and Zr 4+ .
Abstract
Description
本実施の形態に係るスカンジウムの精製方法は、スカンジウム(Sc)を含有する酸性溶液から溶媒抽出によりスカンジウムを抽出して精製(回収)する方法である。特に、このスカンジウムの精製方法では、スカンジウムを含有するとともに、少なくとも鉄(Fe)を含む不純物元素を含有する酸性溶液から、それら不純物と分離してスカンジウムを抽出する。
スカンジウムを含有する酸性溶液(以下、単に「酸性溶液」という)は、溶媒抽出処理の対象となる溶液であり、スカンジウムを含有するとともに、少なくとも鉄を含む不純物元素を含有するものである。
混合抽出剤は、リン酸系抽出剤と中性抽出剤とを含有するものである。本実施の形態に係るスカンジウムの精製方法では、このような混合抽出剤を用いて、上述した酸性溶液に対する溶媒抽出処理を行う。
本実施の形態に係るスカンジウムの精製方法においては、上述したように、鉄を含む不純物元素とスカンジウムとを含有する酸性溶液を、リン系抽出剤と中性抽出剤とを含有する混合抽出剤による溶媒抽出に付し、スカンジウムを抽出する。
下記の実施例、比較例にて用いたスカンジウム抽出用の溶媒抽出剤を、下記表1に示すように調製した。なお、リン酸系抽出剤として、2-エチルヘキシルホスホン酸-1-エチルヘキシル(商品名:PC88A)を用い、中性抽出剤として、トリ-n-オクチルホスフィンオキシド(商品名:TOPO)を用いた。
実施例1、比較例1及び2において、スカンジウム(Sc)、鉄(Fe)、及び、ジルコニウム(Zr)又はトリウム(Th)をそれぞれ下記表2に示す濃度で含有する硫酸溶液(酸性溶液)を用意した。
実施例1では、硫酸溶液を2.5mlずつ5つに分取し、その硫酸溶液のpHを0.0~2.0の範囲内で一定の値に調整した。そして、各々の硫酸溶液についてスカンジウム抽出用の混合抽出剤(PC88A+TOPO)2.5mlと混合し、その混合溶液を回転数650rpmで20分間撹拌した。このとき、硫酸溶液中のpHを、混合抽出剤との混合前と同じ値に維持するため、1mol/Lの水酸化ナトリウム水溶液を適宜添加した。
比較例1では、硫酸溶液を2.5mlずつ5つに分取し、その硫酸溶液のpHを0.0~2.5の範囲内で一定の値に調整したこと、及び、スカンジウム抽出用の抽出剤として中性抽出剤(TOPO)を用いたこと以外は、実施例1と同じ手法にて各種金属の水相から有機相への抽出率を求めた。下記表4及び図1に、pHと各種金属の抽出率との関係を示す。
比較例2では、硫酸溶液を2.5mlずつ3つに分取し、その硫酸溶液のpHを0.0~1.0の範囲内で一定の値に調整したこと、及び、スカンジウム抽出用の抽出剤としてリン酸系抽出剤(PC88A)を用いたこと以外は、実施例1と同じ手法にて各種金属の水相から有機相への抽出率を求めた。下記表5及び図1に、pHと各種金属の抽出率との関係を示す。
[実施例2、実施例3]
実施例2及び3として、下記表6に示すように調製した混合抽出剤(リン酸系抽出剤と中性抽出剤との混合抽出剤)を用いて、ニッケル酸化鉱石に対して酸浸出処理を施してスカンジウムを浸出させた硫酸溶液(下記表7)を溶媒抽出に付した。
[参考例1]
参考例1として、リン酸系抽出剤(PC88A)と中性抽出剤(TOPO)とを含有する混合抽出剤において、下記表10のように、PC88A:5mMに対してTOPO:500mMを混合することによって、リン酸系抽出剤の混合割合をモル比で1%とした混合抽出剤を用いて溶媒抽出を行った。
[実施例4]
実施例4として、以下に示す混合抽出剤を調製し、溶媒抽出を行った。すなわち、下記表12に示すように、リン酸系抽出剤として、ジ(2,4,4-トリメチルペンチル)ホスフィン酸(商品名:Cyanex272)を用い、そのリン酸系抽出剤のモル濃度が0.1mol/L、中性抽出剤(TOPO)のモル濃度が0.5mol/Lとなるように、各々の抽出剤をスワゾールに溶解させることによって、混合抽出剤を調製した。
Claims (9)
- スカンジウムを含有するとともに、少なくとも鉄を含む元素成分を含有する酸性溶液を、リン酸系抽出剤と中性抽出剤とを含有する混合抽出剤による溶媒抽出に付し、該酸性溶液からスカンジウムを抽出する
スカンジウムの精製方法。 - 前記リン酸系抽出剤が、2-エチルヘキシルホスホン酸-1-エチルヘキシルである
請求項1に記載のスカンジウムの精製方法。 - 前記中性抽出剤が、トリ-n-オクチルホスフィンオキシドである
請求項1又は2に記載のスカンジウムの精製方法。 - 前記混合抽出剤においては、前記リン酸性抽出剤がモル比で5%以上50%以下の範囲の混合割合で含まれている
請求項1乃至3のいずれか1項に記載のスカンジウムの精製方法。 - 前記酸性溶液のpHを0.0以上2.0以下の範囲に調整し、pH調整後の該酸性溶液を前記溶媒抽出に付す
請求項1乃至4のいずれか1項に記載のスカンジウムの精製方法。 - 前記酸性溶液は、
ニッケル酸化鉱石に酸を添加してスカンジウムを浸出した溶液、又は、スカンジウム酸化物若しくはスカンジウム水酸化物を酸で溶解して得られた溶液であり、
前記酸性溶液のpHを0.0以上2.0以下の範囲に調整し、pH調整後の該酸性溶液を前記溶媒抽出に付す
請求項1乃至4のいずれか1項に記載のスカンジウムの精製方法。 - 前記酸性溶液は、さらに、ジルコニウム、トリウムのいずれか1種以上を含む
請求項1乃至6のいずれか1項に記載のスカンジウムの精製方法。 - スカンジウムを含有するとともに、少なくとも鉄を含む元素成分を含有する酸性溶液から、該スカンジウムを抽出するための抽出剤であって、
リン酸系抽出剤と、中性抽出剤とを含有する
スカンジウム抽出剤。 - 前記リン酸性抽出剤がモル比で5%以上50%以下の範囲の割合で含まれている
請求項8に記載のスカンジウム抽出剤。
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