EP3081670B1 - Scandium concentrate production method - Google Patents
Scandium concentrate production method Download PDFInfo
- Publication number
- EP3081670B1 EP3081670B1 EP15740662.0A EP15740662A EP3081670B1 EP 3081670 B1 EP3081670 B1 EP 3081670B1 EP 15740662 A EP15740662 A EP 15740662A EP 3081670 B1 EP3081670 B1 EP 3081670B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- scandium
- aluminum
- electrolysis
- cathode
- potential
- 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.)
- Not-in-force
Links
- 229910052706 scandium Inorganic materials 0.000 title claims description 81
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims description 79
- 239000012141 concentrate Substances 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000005868 electrolysis reaction Methods 0.000 claims description 55
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 51
- 229910052782 aluminium Inorganic materials 0.000 claims description 50
- 150000003839 salts Chemical class 0.000 claims description 34
- 238000006263 metalation reaction Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- 230000005496 eutectics Effects 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 14
- 239000000956 alloy Substances 0.000 claims description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 13
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- DVMZCYSFPFUKKE-UHFFFAOYSA-K scandium chloride Chemical compound Cl[Sc](Cl)Cl DVMZCYSFPFUKKE-UHFFFAOYSA-K 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 2
- 229910000542 Sc alloy Inorganic materials 0.000 description 26
- 239000010453 quartz Substances 0.000 description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 21
- 150000001805 chlorine compounds Chemical class 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 5
- 210000001787 dendrite Anatomy 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910013618 LiCl—KCl Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910000480 nickel oxide Inorganic materials 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 150000003325 scandium Chemical class 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LUKDNTKUBVKBMZ-UHFFFAOYSA-N aluminum scandium Chemical compound [Al].[Sc] LUKDNTKUBVKBMZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
Definitions
- the present invention relates to a scandium concentrate production method, and in more detail, relates to a method of reusing an alloy containing scandium and aluminum as aluminum and scandium concentrates.
- Aluminum scandium alloys containing aluminum and scandium have a characteristic of being light weight and high strength, and in addition to sports articles, have been used in fields requiring shock resistance. Additionally, in the future, applications as a structural material for aircraft, electric vehicles, high-speed rail, etc. are also expected. However, since the production volume of scandium is very small, scandium is extremely high cost. For this reason, it is not easy to broadly apply scandium industrially.
- Patent Document 1 Japanese Unexamined Patent Application, Publication No. 2003-171724
- the scandium quality of these disposed articles, etc. is far higher than the scandium quality of nickel oxide ores, etc., and recovering scandium from the disposed articles, etc. and reusing is expected to be an effective means.
- an element contained in Al-Sc alloy is aluminum, and the content of scandium is a very small amount comparing with the content of aluminum; therefore, it is not possible to effectively recover scandium concentrate by simply melting Al-Sc alloy.
- the present invention has been made in order to solve the above such problems, and the object thereof is to effectively recover scandium concentrate from Al-Sc alloy.
- the Al-Sc alloy in structures, etc. is widely used by concentrating to 0.1 to 1% Sc.
- the Sc concentration of the Al-Sc master alloy is 1 to 2%.
- the present invention has an object of efficiently recovering scandium concentration of a degree that can be used as is as an Al-Sc master alloy from scrap articles of Al-Sc alloy having an Sc concentration on the order of 0.1 to 1%.
- the present inventors found that the above-mentioned object could be achieved by bringing chlorine into contact with an alloy containing aluminum and scandium, melting, followed by subjecting the molten mixture to electrolysis at predetermined conditions, thereby arriving at completion of the present invention.
- the present invention provides the following matters.
- a first aspect of the present invention is a scandium concentrate production method including: a molten mixture generation step of bringing chlorine into contact with an alloy containing aluminum and scandium, and melting to generate a molten mixture of aluminum chloride and scandium chloride; a first electrolysis step of subjecting the molten mixture to first electrolysis using a first cathode at a potential between a metalation potential of aluminum and a metalation potential of scandium to generate aluminum at the periphery of the first cathode; and a second electrolysis step of subjecting the molten mixture after the molten aluminum generation step to second electrolysis using a second cathode at a potential capable of recovering scandium to generate a scandium concentrate at the periphery of the second cathode.
- the molten mixture generation step is a step of melting the alloy brought into contact with the chlorine into a melt of a chloride-based salt or eutectic salt having a melting point or eutectic temperature of no higher than 500°C
- the first electrolysis step is a step of generating solid aluminum at the periphery of the first cathode
- the second electrolysis step is a step of generating a solid scandium concentrate at the periphery of the second cathode.
- the present invention it is possible to effectively recover a scandium concentrate from Al-Sc alloy.
- This scandium concentration can be used as is as a high-quality Al-Sc master alloy.
- by passing through solvent extraction, etc. it is also possible to recover scandium very efficiently compared to a case of recovering from nickel oxide ore.
- FIG. 1 is a schematic view showing a scandium concentrate production method according to the present invention.
- This method includes a molten mixture generation step S1 of generating a molten mixture of aluminum chloride and scandium chloride by bringing chlorine into contact with an alloy containing aluminum and scandium and melting; a first electrolysis step S2 of subjecting the molten mixture to first electrolysis using a first cathode at a potential between the metalation potential of aluminum and the metalation potential of scandium to generate aluminum at the periphery of the first cathode; and a second electrolysis step S3 of subjecting the molten mixture, after the molten aluminum generation step S2, to a second electrolysis using a second cathode at a potential capable of recovering scandium to generate a scandium concentrate on the periphery of the second cathode.
- the present invention first brings chlorine gas into contact with an Al-Sc alloy that is the raw material (disposed article, manufacturing defect, etc.) to obtain chlorides of the Al-Sc alloy having a low melting point compared to the Al-Sc alloy. Next, the chlorides of Al-Sc alloy are melted. It is possible to sufficiently dissolve at a temperature on the order of 450°C if chlorides of Al-Sc alloy.
- Salts or eutectic salts used upon melting the above-mentioned mixture require consideration in both aspects of the viewpoint of the melting point or eutectic temperature, and the viewpoint of the metalation potentials of metals that are the separation targets; however, the former viewpoint will be explained first.
- the stability is high at a temperature about 10°C higher than the temperature that can melt the chlorides of Al-Sc alloy, and is not particularly limited so long as not being a temperature at which a change in the salt composition arises due to volatilization. More specifically, the melting point or eutectic temperature are preferably 360°C to 500°C, more preferably 380°C to 450°C, and even more preferably 390°C to 400°C.
- the melting point or eutectic temperature is too low, it is not preferable because a change in the salt composition due to volatilization can occur when heating the salt or eutectic salt to an extent that can melt the chlorides of Al-Sc alloy. If the melting point or eutectic temperature is too high, it is not preferable because it will heat the salt or eutectic salt up to an unnecessarily high temperature.
- the molten salt requires there to be a difference of at least 0.8 V between the metalation potential of aluminum and the metalation potential of scandium.
- the electrolytic potentials of elements differ according to the type and composition of the molten salt.
- the molten salt since aluminum and scandium coexist, since it is configured so that only aluminum is generated in the first electrolysis, and scandium is first generated in the second electrolysis, the molten salt requires to have at least a certain difference between the metalation potential of aluminum and the metalation potential of scandium. A greater difference is preferable, and it is more preferably at least 1.0 V.
- the metalation potential of Al 3+ is -1.04 V
- the metalation potential of Sc 3+ is -1.83 V.
- the difference between the two is about 0.8 V, and is sufficient to suppress both the aluminum and scandium from generating in the first electrolysis.
- detailed data for the metalation potential is not known, even if the type of metal element constituting the salt differs, a great difference in the metalation potentials does not arise so long as being chloride-based salts.
- the above-mentioned chlorides of Al-Sc alloy are dissolved in the molten salt heated to an extent capable of sufficiently melting the chlorides of Al-Sc alloy. Since the saturated vapor pressure of aluminum chloride and the saturated vapor pressure of scandium chloride differ, when dissolving the above-mentioned chlorides of Al-Sc alloy in the above-mentioned molten salt, while a part of the aluminum chloride (AlCl 3 ) volatilizes, the remaining aluminum chloride and scandium chloride (ScCl 3 ) easily melt into the eutectic salt to form a uniform melt.
- the first electrolysis step S2 subjects the molten mixture obtained in the molten mixture generation step S1 to the first electrolysis using a first cathode at a potential between the metalation potential of aluminum and the metalation potential of scandium to generate solid aluminum at the periphery of this first cathode in a dendrite form (arborescent crystal).
- the type of electrode is not particularly limited, for example, establishing silver as the reference electrode, graphite as the anode, and nickel as the first cathode can be exemplified.
- the potential in the first electrolysis is required to be between the metalation potential of aluminum and the metalation potential of scandium, and in more detail, no more than the metalation potential of aluminum and at least the metalation potential of scandium. If not in this range, it is not preferable because not only molten aluminum, but also scandium can generate at the cathode.
- the potential in the first electrolysis is preferably closer to the metalation potential of aluminum, and specifically, is preferably within the range of -1.50 V to -1.04 V, and is more preferably within the range of -1.30 V to -1.10 V.
- the temperature of the molten salt is not particularly limited so long as being able to melt the chlorides of Al-Sc alloy and being lower than the melting point of aluminum; however, from the point of curbing the energy cost to a minimum, the point of suppressing the generated aluminum from becoming liquid, etc., it is preferably 360°C to 500°C, and more preferably 380°C to 450°C.
- Chlorine gas is generated at the anode during the first electrolysis. In order to raise the current efficiency, it is preferable to quickly remove the generated chlorine gas from the anode.
- the scandium concentration contained in the molten salt rises.
- the second electrolysis step S3 subjects the molten mixture to the second electrolysis using a second cathode differing from the first cathode at a potential capable of recovering scandium, after the molten aluminum generation step S2. By doing this, solid scandium concentrate is generated in dendrite form (arborescent crystal) at the periphery of the first cathode.
- the material of the electrode is not particularly limited, and it is acceptable to use the same as the electrode used in the first electrolysis; however, it is necessary for at least the first cathode and second cathode to be two different cathode bars.
- the potential in the second electrolysis it is required for the potential in the second electrolysis to generate scandium on the cathode in dendrite form along with aluminum, more specifically, to be no more than the metalation potential of scandium. If not in this range, it is not preferable because solid scandium concentrate will not satisfactorily generate at the cathode.
- the potential in the second electrolysis is sufficient so long as being no more than -1.83 V; however, when considering the stability of operation, it is preferably no more than -2.0 V, and more preferable no more than -2.2 V.
- FIG. 2 is a schematic view illustrating the configuration of an electrolysis apparatus 1 used in the present examples.
- the electrolysis apparatus 1 includes: the two of a small and large quartz container 21, 22 that enclose the Al-Sc alloy along with molten salt; a quartz tube 3 with one side open, and accommodating the quartz containers 21, 22 from this opening; a rubber stopper 4 that seals this quartz tube 3; a reference electrode (silver) 5, anode (graphite) 6 and first or second cathode (nickel) 71, 72 inserted inside of the large quartz container 21; a gas substitution unit 8 that substitutes the inside of the quartz tube 3 with gas; a thermocouple 9 that is inserted inside of the large quartz container 21; an electric furnace 10 that keeps the temperature inside of the quartz tube 3 at a predetermined temperature; and an insulation board 11 that keeps the adiabaticity of the inside of the quartz tube 3.
- the reference electrode (silver) 5, anode (graphite) 6 and first cathode (nickel) 71 were immersed to the positions shown in FIG. 2 , and the first electrolysis was performed while holding at the potential of -1.15 V for the potential of the Ag + /Ag reference electrode 5. Solid aluminum of dendrite form was thereby recovered from the first cathode 71.
- the first cathode 71 was replaced with the second cathode 72, and the second electrolysis was performing while maintaining a potential of -1.95 V for the potential of the Ag + /Ag reference electrode 5. Both aluminum and scandium were thereby precipitated from the first cathode 71, a result of which solid scandium concentrate 13 of dendrite form was obtained.
- the inside of the quartz tube 3 was cooled to room temperature. Then, the salt 12 and scandium concentrate 13 that solidified from cooling were retrieved.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2014012666A JP5907187B2 (ja) | 2014-01-27 | 2014-01-27 | スカンジウム濃縮物の製造方法 |
PCT/JP2015/051827 WO2015111697A1 (ja) | 2014-01-27 | 2015-01-23 | スカンジウム濃縮物の製造方法 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP3081670A1 EP3081670A1 (en) | 2016-10-19 |
EP3081670A4 EP3081670A4 (en) | 2016-12-21 |
EP3081670B1 true EP3081670B1 (en) | 2017-09-13 |
Family
ID=53681494
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP15740662.0A Not-in-force EP3081670B1 (en) | 2014-01-27 | 2015-01-23 | Scandium concentrate production method |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP3081670B1 (ja) |
JP (1) | JP5907187B2 (ja) |
WO (1) | WO2015111697A1 (ja) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3612654B1 (en) * | 2017-03-20 | 2021-09-08 | Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret Anonim Sirketi | Production method for scandium metal and al-sc alloys via electrolysis of fluorinated scandium salts obtained by the calcination of scandium compound in the form of (nh4)2nascf6 |
CN108486610B (zh) * | 2018-05-30 | 2019-09-10 | 河南大学 | 一种熔盐电解制备耐腐蚀Al-Ni合金的方法 |
CN110129836B (zh) * | 2019-04-25 | 2020-11-24 | 赣南师范大学 | 一种利用分段式加热减少熔盐挥发的方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2874039A (en) * | 1954-06-17 | 1959-02-17 | Pechiney Prod Chimiques Sa | Extraction of scandium from its ores |
US6808695B1 (en) * | 2000-05-22 | 2004-10-26 | Toth Aluminum Corporation | Process for continuously producing aluminum from clays |
JP4224532B2 (ja) | 2001-12-07 | 2009-02-18 | 青森県 | Al−Sc母合金の製造法およびその方法によって得られたAl−Sc母合金 |
US6767444B1 (en) * | 2002-08-26 | 2004-07-27 | The United States Of America As Represented By The United States Department Of Energy | Method for processing spent (TRU, Zr)N fuel |
JP5094031B2 (ja) * | 2006-03-23 | 2012-12-12 | 大平洋金属株式会社 | スカンジウム含有合金の製造方法 |
JP5472897B2 (ja) * | 2008-12-09 | 2014-04-16 | 株式会社東芝 | 画像処理装置 |
JP2012136766A (ja) * | 2010-12-28 | 2012-07-19 | Kyoto Univ | 電気分解による金属の製造方法 |
-
2014
- 2014-01-27 JP JP2014012666A patent/JP5907187B2/ja active Active
-
2015
- 2015-01-23 EP EP15740662.0A patent/EP3081670B1/en not_active Not-in-force
- 2015-01-23 WO PCT/JP2015/051827 patent/WO2015111697A1/ja active Application Filing
Non-Patent Citations (1)
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Also Published As
Publication number | Publication date |
---|---|
WO2015111697A1 (ja) | 2015-07-30 |
JP2015140445A (ja) | 2015-08-03 |
EP3081670A1 (en) | 2016-10-19 |
JP5907187B2 (ja) | 2016-04-26 |
EP3081670A4 (en) | 2016-12-21 |
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