EP3612654A2 - Herstellungsverfahren für scandiummetall und al-sc-legierungen durch elektrolyse fluorierter scandiumsalze aus der kalzinierung einer scandiumverbindung in form von (nh4)2nascf6 - Google Patents

Herstellungsverfahren für scandiummetall und al-sc-legierungen durch elektrolyse fluorierter scandiumsalze aus der kalzinierung einer scandiumverbindung in form von (nh4)2nascf6

Info

Publication number
EP3612654A2
EP3612654A2 EP18849073.4A EP18849073A EP3612654A2 EP 3612654 A2 EP3612654 A2 EP 3612654A2 EP 18849073 A EP18849073 A EP 18849073A EP 3612654 A2 EP3612654 A2 EP 3612654A2
Authority
EP
European Patent Office
Prior art keywords
scandium
production method
aluminum
ions
fluorinated
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.)
Granted
Application number
EP18849073.4A
Other languages
English (en)
French (fr)
Other versions
EP3612654B1 (de
EP3612654A4 (de
Inventor
Ali Safder IPLIKÇIOGLU
Serif KAYA
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.)
Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret AS
Original Assignee
Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret AS
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 Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret AS filed Critical Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret AS
Publication of EP3612654A2 publication Critical patent/EP3612654A2/de
Publication of EP3612654A4 publication Critical patent/EP3612654A4/de
Application granted granted Critical
Publication of EP3612654B1 publication Critical patent/EP3612654B1/de
Not-in-force 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
    • 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
    • C25C3/34—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
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/36—Alloys obtained by cathodic reduction of all their ions

Definitions

  • the invention relates to scandium metal in its pure or alloy form obtained by removing the NH 4 form present in the scandium compound which is initially in its (NH 4 )2NaScF6 form, by calcination first and then with molten salt electrolysis of fluorinated scandium compounds in NaScF 4 and Na3ScF6 forms that resulted after the calcination process.
  • Scandium is one of the transition metals, which belongs to the 3B group of the periodic table, and known as one of the rare earth elements, which is rarely enriched in nature. Scarcity of the ores which has sufficient grade of scandium for feasible processing, constitutes a great obstacle against production and the usage of this metal in various industries. Until today, scandium has been found in trace amounts among uranium, tin, iron, tungsten, tantalum, zirconium, titanium and other rare earth element ores that are economically processed, within the content of more than 100 minerals; it has been obtained as a byproduct during the production of these metals.
  • molten salt electrolysis method it may be possible to obtain scandium metal alternatively by using molten salt electrolysis method in order to overcome the problems encountered during metallothermic reduction methods realized at high temperatures with calcium metal [1 ].
  • the basic principle of the molten salt method is to dissolve the compound of the desired metal, inside an appropriate salt mixture at high temperature and separate it into its ions, and during the process, reduction of the desired element ions and selectively collect it at the cathode may be achieved by applying electric current to the molten salt mixture.
  • Salts that may be used in this process are fluoride, chloride, bromide and iodide and among them fluoride, chloride and mixtures thereof have been the most preferred alternatives [2].
  • Molten salts containing chloride and fluoride, fluoride containing salts are the most preferred ones due to having higher stability at high temperatures, absence of humidity absorption problem (not being hydroscopic) in contrast to chloride, and having high current efficiency [3].
  • the present invention relates to a production method for scandium metal and Al-Sc alloys from scandium compounds obtained by the calcination of scandium compound in (NH 4 )2NaScF6 form, via molten salt electrolysis method, which meets the aforementioned requirements while overcoming all disadvantages and providing further advantages.
  • the primary objective of the invention is the production of pure scandium metal, directly obtaining aluminum-scandium alloys containing 0.2-0.8% scandium and obtaining aluminum-scandium master alloys containing 1 -20% scandium.
  • Another objective of the invention is to obtain scandium metal by using molten salt method, in order to overcome the technical problems associated with metallothermic reduction method. It is also obtaining fluoride containing salts in order to achieve this.
  • Another objective of the invention is the calcination of the scandium compound in (NH 4 )2NaScF6, form at a temperature between 350-400 ⁇ C; and aft er the calcination process, by removing the (NH 4 ) form from the structure, obtaining fluorinated scandium salts having the forms of NaScF 4 and Na3ScF6, in order to be used in molten salt electrolysis method.
  • a similar objective of the invention is to prevent the use of various high purity salts required to form the molten salt mixture.
  • a production method of pure scandium metal comprising; a) obtaining fluorinated scandium salt mixture in NaScF 4 and Na3ScF6 forms from the scandium compound in (NH 4 )2NaScF6 form via calcination process, b) electrolysis process of the obtained fluorinated scandium salt mixture in NaScF 4 and Na3ScF6 forms via molten salt electrolysis method, process steps.
  • Figure 1 View of the cell system that is used to obtain pure scandium metal
  • Figure 2 View of the cell system that is used to obtain aluminum-scandium metal
  • Figure 3 Graphical representation of DTA/TGA analysis results which is conducted to determine the calcination temperature of (NH 4 )2NaScF6 compound
  • Figure 6 Optical microscope image of the Al-Sc alloy obtained by electrolysis (x190 magnification)
  • Figure 7 Optical microscope image of the Al-Sc alloy obtained by electrolysis (x190 magnification) and micro-hardness measurement of Al and A Sc phases
  • the invention relates to production method for scandium metal in its pure or alloy form.
  • the scandium production method of the invention comprises two steps. In the first step; removing the (NH 4 ) form by applying calcination process to scandium compound in (NH 4 )2NaScFe form for a duration of 1 -3 hours (preferably 1 hour) at 350-400 ⁇ C temperature, after the calcination process obtaining a fluorinated scandium salt mixture in the forms of NaScF 4 and Na3ScF6.
  • the second step is the use of fluorinated scandium salt mixture in the NaScF 4 and Na3ScF6 forms, in molten salt electrolysis method in order to obtain pure scandium metal.
  • FIG. 1 a cell system that is used to obtain pure scandium metal is shown.
  • the calcined fluorinated salt mixture is used directly in order to obtain pure scandium metal. It is desired to maintain the salts, which are used in molten salt electrolysis, in molten phase during the process. Therefore, the obtained salt mixture is desired to have a relatively lower melting temperature. It has been observed that the fluorinated scandium salt mixture in NaScF 4 and Na3ScF6 forms, obtained by calcination, melts at about 600 ⁇ C. Therefore, in this process the temperature duri ng the molten salt electrolysis method should be over 600 ⁇ C.
  • Na, Sc and F elements are in ionic states, generally in Na + , Sc +3 and F " forms. Therefore, when an electric current is applied through the molten mixture at a certain potential, positively charged Na + , Sc +3 ions will be attracted by the cathode, while negatively charged F " ions will be attracted by the anode. Depending on the relative stability of these ions with respect to each other, the applied potential will result in electrochemical oxidation and reduction reactions at the anode and the cathode regions. Mentioned salt mixture is heated until it reaches 600-1 100 as shown in the example drawing of Figure 1 . Depending on the composition of the salt mixture, the preferred temperature should be 10-15 above the melting te mperature of the salt.
  • the circuit is supplied with electric current to maintain 2-8 volts of potential difference.
  • the current density applied to the circuit should be stabilized preferentially between 0.5- 1 .0 A/cm 2 . Due to the relatively lower applied potential, Na + ions are prevented to react, while only Sc 3+ ions are reduced at the cathode (5) and collected on the electrolysis cell in a metallic form. Therefore, limiting the potential applied to the circuit below 3 volts will prevent the Na contamination problem.
  • F " ions will react with the graphite anode (4) and leave the cell as various fluorocarbon gases. These gases leaving the anode are environmentally undesired and hence may be collected and neutralized later.
  • oxygen gas which does not possess any environmental risks may be obtained at by using more stable anode materials which does not react with oxygen,
  • the Sc +3 ions inside the molten salt is reduced and separated from the salt mixture so pure scandium metal (9) can be obtained at the bottom of the cell.
  • both phases are melted by increasing the temperature of the cell over a value where the aluminum and the fluoride salt mixtures are in their molten states (preferably 700-1 100 * €-).
  • a value where the aluminum and the fluoride salt mixtures are in their molten states preferably 700-1 100 * €-.
  • a current may be applied to the circuit in order to create a potential difference between 2 and 8 volts. Applying relatively lower potentials preferably not exceeding 3 volts prevents Na + ions to react, ensuring only Sc 3+ ions to be reduced at the cathode (5) and to be dissolved in the liquid aluminum (10), collected at the bottom of the electrolysis cell in molten state. Due to oxidation reactions occurred at anode, by reacting with the graphite anode (4), F " ions may leave the cell in the form of various fluorocarbon gases. Since these gases emitted at the anode are environmentally undesired, these gases may be collected and disposed of later.
  • more stable anode materials which does not react with fluorine gas may be used instead of the graphite anode (4), resulting in only fluorine gas output (2) at the anode, in order to provide easier disposal of these gases.
  • These residual gases may be converted into more stable and less hazardous fluoride compounds via using a gas collector unit.
  • fluorine gas outlet (2) is not preferred in the circuit during the reduction reactions, SC2O3 or AI2O3 compounds may be added to the system no more than 10% by weight in the salt mixture and scandium oxide may be dissolved into Sc +3 and O "2 ions, or the aluminum oxide may be dissolved into Al +3 and O 2 ions, inside the molten salt (8) phase.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Electrolytic Production Of Metals (AREA)
EP18849073.4A 2017-03-20 2018-03-06 Herstellungsverfahren für scandiummetall und al-sc-legierungen durch elektrolyse fluorierter scandiumsalze aus der kalzinierung einer scandiumverbindung in form von (nh4)2nascf6 Not-in-force EP3612654B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
TR201704146 2017-03-20
PCT/TR2018/050078 WO2019040016A2 (en) 2017-03-20 2018-03-06 PROCESS FOR THE PRODUCTION OF SCANDIUM AND AL-SC ALLOYS BY ELECTROLYSIS OF FLUORINATED SCANDIUM SALTS OBTAINED BY CALCINATION OF A SCANDIUM COMPOUND IN THE FORM OF (NH 4) 2NASCF 6

Publications (3)

Publication Number Publication Date
EP3612654A2 true EP3612654A2 (de) 2020-02-26
EP3612654A4 EP3612654A4 (de) 2020-04-22
EP3612654B1 EP3612654B1 (de) 2021-09-08

Family

ID=65439168

Family Applications (1)

Application Number Title Priority Date Filing Date
EP18849073.4A Not-in-force EP3612654B1 (de) 2017-03-20 2018-03-06 Herstellungsverfahren für scandiummetall und al-sc-legierungen durch elektrolyse fluorierter scandiumsalze aus der kalzinierung einer scandiumverbindung in form von (nh4)2nascf6

Country Status (2)

Country Link
EP (1) EP3612654B1 (de)
WO (1) WO2019040016A2 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TR201704220A2 (tr) * 2017-03-21 2018-03-21 Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret Anonim Sirketi (NH4)2NaScF6 formundaki skandiyum bileşiğinden elde edilen ScF3 bileşiğine, CaCl2 ve/veya MgCl2 bileşiklerinin ilavesiyle oluşturulan, skandiyum tuz karışımlarından elektroliz yöntemi vasıtasıyla skandiyum metali ve Al-Sc alaşımlarının üretim metodu
CN117534111B (zh) * 2023-11-17 2026-03-31 山东省科学院新材料研究所 一种Na3ScF6及其制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3111467A (en) * 1960-06-03 1963-11-19 Nuclear Corp Of America Production of scandium and yttrium
CN1184356C (zh) * 2002-12-03 2005-01-12 中国铝业股份有限公司 一种电解生产铝钪合金的方法
CN1260397C (zh) * 2003-08-21 2006-06-21 中国铝业股份有限公司 一种高纯铝钪合金的生产方法
JP5907187B2 (ja) * 2014-01-27 2016-04-26 住友金属鉱山株式会社 スカンジウム濃縮物の製造方法
KR101724288B1 (ko) * 2015-07-17 2017-04-10 재단법인 포항산업과학연구원 고순도 알루미늄-스칸듐 합금 제조 방법

Also Published As

Publication number Publication date
EP3612654B1 (de) 2021-09-08
WO2019040016A2 (en) 2019-02-28
WO2019040016A3 (en) 2019-04-25
EP3612654A4 (de) 2020-04-22

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