EP1785509A1 - Procédé et appareil de production de métal par électrolyse de sel fondu - Google Patents

Procédé et appareil de production de métal par électrolyse de sel fondu Download PDF

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Publication number
EP1785509A1
EP1785509A1 EP05765165A EP05765165A EP1785509A1 EP 1785509 A1 EP1785509 A1 EP 1785509A1 EP 05765165 A EP05765165 A EP 05765165A EP 05765165 A EP05765165 A EP 05765165A EP 1785509 A1 EP1785509 A1 EP 1785509A1
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EP
European Patent Office
Prior art keywords
metal
negative electrode
electrolysis
molten
electrolytic bath
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.)
Withdrawn
Application number
EP05765165A
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German (de)
English (en)
Other versions
EP1785509A4 (fr
Inventor
Masanori TOHO TITANIUM CO. LTD. YAMAGUCHI
Yuichi c/o TOHO TITANIUM CO. LTD. ONO
Susumu c/o TOHO TITANIUM CO. LTD. KOSEMURA
Eiji c/o TOHO TITANIUM CO. LTD. NISHIMURA
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Toho Titanium Co Ltd
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Toho Titanium Co Ltd
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Publication date
Application filed by Toho Titanium Co Ltd filed Critical Toho Titanium Co Ltd
Publication of EP1785509A1 publication Critical patent/EP1785509A1/fr
Publication of EP1785509A4 publication Critical patent/EP1785509A4/fr
Withdrawn legal-status Critical Current

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    • 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
    • C25C7/007—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells comprising at least a movable electrode
    • 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
    • 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
    • C25C7/08—Separating of deposited metals from the cathode

Definitions

  • the present invention relates to the recovery of metal from a chloride thereof, and in particular, relates to a method and an apparatus for producing metal by electrolysis of molten salts containing metal chlorides.
  • titanium metal which is a simple substance
  • Kroll method in which titanium tetrachloride is reduced by molten magnesium to obtain sponge titanium
  • various kinds of improvements have been made to reduce the cost of production.
  • the Kroll method is a batch process in which a set of operations is repeated noncontinuously, there is a limitation to its efficiency.
  • the present invention has been completed in view of the above situation, and an object of the present invention is to provide a method for production of metal by molten-salt electrolysis, in which a metal used for reducing, such as an oxide or chloride of titanium metal, is recovered in a solid state and at low cost.
  • a metal used for reducing such as an oxide or chloride of titanium metal
  • a method for production of metal by molten-salt electrolysis of the present invention has a step of filling an electrolysis vessel having a positive electrode and negative electrode with a metal chloride, a step of heating to fuse the metal chloride to make an electrolytic bath, and a step of electrolyzing the electrolytic bath to deposit metal in a solid state on the negative electrode.
  • a metal can be deposited on the negative electrode in a solid state, which is a state having low solubility in the molten salt, and it can be recovered. Furthermore, the recovery of the metal can be performed at low cost.
  • An apparatus for production of metal by molten-salt electrolysis of the present invention has an electrolysis vessel having a positive electrode and a negative electrode therein and a metal chloride filled in the vessel, the metal chloride is heated and molten to make an electrolytic bath, and the electrolytic bath is electrolyzed to deposit metal in a solid state on the negative electrode. Furthermore, in the apparatus, the electrolytic bath is divided into an electrolysis chamber and a dissolution chamber by a dividing wall, the positive electrode is arranged in the electrolysis chamber, and the negative electrode is arranged to enable orbital movement in a circle through the electrolysis chamber and the dissolution chamber. Metal which is deposited on the negative electrode in the electrolysis chamber is recovered in the dissolution chamber.
  • electrolysis of metal chloride is promoted and the metal is deposited on the negative electrode while the negative electrode is passing through the electrolysis chamber, and the metal deposited can be recovered during the negative electrode passing through the dissolution chamber. Furthermore, since the negative electrode revolves and passes through the electrolysis chamber and dissolution chamber regularly, deposition and recovery of the metal can be automatically and efficiently performed.
  • Electrolysis vessel 1a
  • Electrolysis chamber 1b
  • Dissolution chamber 2... Electrolytic bath, 3... Positive electrode, 4... Negative electrode, 5... Metal (calcium), 6... Molten salt, 7... Recovery vessel, 8... Chlorine gas, 9... Scraping device, 10... Dividing wall
  • Figs. 1 to 3 show embodiments of an apparatus to perform the present invention. Next, a case in which the electrolytic bath is one of calcium chloride and the metal generated is calcium metal, is explained.
  • reference numeral 1 is an electrolysis vessel, and electrolytic bath 2 comprising calcium chloride is filled therein and heated to a temperature not less than the melting point of calcium chloride by a heating means, which is not shown, to keep the electrolytic bath in a molten state.
  • Reference numeral 3 is a positive electrode and reference numeral 4 is a negative electrode, and they are immersed in the electrolytic bath 2.
  • the positive and negative electrodes 3 and 4 are connected to a direct current power supply, which is not shown, and electrolysis of the electrolytic bath is started. Chloride ions in the electrolytic bath 2 are attracted to the positive electrode 3 and emit electrons to generate chlorine gas which is lost from the system. Calcium ions are attracted to the negative electrode and receive electrons to generate calcium metal 5 which is deposited on the surface of negative electrode 4.
  • the present invention can be efficiently performed even in the cases in which the temperature of the electrolytic bath 2 is above or below the melting point of calcium metal 5 (845°C).
  • the temperature of the electrolytic bath 2 is below the melting point of calcium metal, calcium metal 5 can be deposited in a solid state on the surface of the negative electrode 4.
  • the temperature of the electrolytic bath 2 is above the melting point of calcium metal 5, calcium metal 5 can be deposited in a solid state on the surface of the negative electrode 4 in the case in which a cooling structure is installed in the negative electrode 4.
  • the negative electrode 4 After a certain amount of calcium metal 5 is deposited on the negative electrode 4, the negative electrode 4 is taken out of the electrolytic bath 2 and is immersed in a recovery vessel 7 having molten salt 6 for which the temperature is maintained above the melting point of calcium metal 5 (845°C). The calcium metal 5 deposited on the negative electrode 4 is partially dissolved in the molten salt 6 held in the recovery vessel 7, and the rest floats up from the negative electrode 4 to be condensed around the surface of the liquid. The condensed part is collected and recovered. In this case, since evaporation loss becomes larger as the temperature is increased, the temperature is practically set at not more than 900°C.
  • Calcium can be dissolved, floated and recovered in a liquid state as explained above, and in addition, it can be cooled to not more than the melting point of calcium metal (845°C) as long as the molten salt 6 is not solidified. By performing such a cooling operation, calcium metal 5 floats in a solid state, and it can be efficiently recovered. Since the melting point of calcium chloride is about 780°C and the melting point of calcium metal is about 845°C, by decreasing the temperature of the recovery vessel 7 to about 800°C, calcium metal 5 molten in the molten salt 6 can be recovered in a solid state.
  • the negative electrode 4, after separating and recovering the calcium metal 5 deposited, can be transferred from the recovery vessel 7 to the electrolysis vessel 1 to perform molten-salt electrolysis again. By repeating the above-mentioned set of operations, calcium metal can be efficiently recovered.
  • the calcium metal 5 generated in the recovery vessel 7 in this way can be used in the reduction of titanium tetrachloride using molten salt.
  • calcium metal is not recovered in the recovery vessel 7 leaving the concentration of calcium metal in the molten salt 6 high, and the molten salt containing calcium can be used in the reduction reaction of titanium tetrachloride.
  • Chlorine gas 8 generated on the positive electrode 3 in the electrolysis vessel 1 can be separately recovered and can be reused in a chlorination reaction of titanium ore. Alternatively, it can be used for other purposes.
  • a material of the positive electrode 3 a material having an electrical conductivity which does not dissolve in the electrolytic bath and does not react with chlorine gas, is desirable.
  • carbon is desirable.
  • the negative electrode 4 can be constructed by an electrical conductive material, for example, carbon steel, stainless steel, copper, aluminum or the like can be used.
  • the negative electrode 4 desirably has a structure in which a cooling medium can be circulated therein. The structure can promote deposition of calcium metal on the negative electrode 4.
  • the molten salt 6 in the recovery vessel 7 arbitrarily selected one can be used, and in particular, calcium chloride is desirable. Since calcium chloride is a by-product of molten-salt electrolysis of titanium chloride and calcium metal, if the molten salt 6 is calcium chloride, it will be unnecessary to remove calcium chloride when condensed calcium metal is used in a molten-salt electrolysis process for titanium chloride. In addition, that is because after the molten-salt electrolysis process for titanium chloride, the molten salt 6 can be reused with calcium chloride which is a by-product of this process in the electrolysis vessel 1.
  • the melting point of the electrolytic bath can be decreased by adding potassium chloride to calcium chloride forming the electrolytic bath 2.
  • the amount of potassium chloride added to calcium chloride is desirably in a range from 20 to 80 wt%.
  • the temperature of the electrolytic bath 2 can be arbitrarily controlled within the target temperature range by using a heating burner having a cooling function, which is not shown, immersed in the electrolytic bath. Alternatively, another means can be employed to control the temperature of the electrolytic bath 2.
  • Fig. 2 shows another embodiment of the present invention.
  • Electrolytic bath 2 comprising calcium chloride is filled in the electrolysis vessel 1 of Fig. 2A, is heated to a temperature not less than the melting point of calcium chloride by a heating means, which is not shown, and is held in a molten state.
  • the positive electrode 3 and the negative electrode 4 having cylindrical shape are immersed in the electrolytic bath 2.
  • This negative electrode 4 can be constructed so as to be rotatable, and the scraping device 9 is arranged neighboring to an edge of a side surface of the cylindrical negative electrode 4.
  • Fig. 2B shows a conceptual diagram of the negative electrode 4 and the scraping device 9 seen from the direction A. As shown in the figure, by rotating the negative electrode, calcium metal 5 deposited on the surface of the negative electrode is efficiently scraped by the scraping device 9.
  • Solid calcium metal 5 scraped from the negative electrode 4 floats up to the surface of the electrolytic bath 2 since the density of calcium metal is lower than that of calcium chloride.
  • the calcium metal 5 which floated to the surface of the electrolytic bath 2 is recovered from the electrolytic bath 2.
  • the solid calcium metal recovered from the electrolytic bath 2 is used as a reducing agent for titanium oxide in molten-salt electrolysis.
  • a basket having a net structure can be arranged around the scraping device 9.
  • solid metal deposited can be efficiently recovered.
  • the dividing wall 10 be arranged around the surface of electrolytic bath 2. Calcium metal deposited on the negative electrode 4 is scraped and then floats and diffuses to the bath surface. Finally, calcium metal can reach the positive electrode 3, and it has a tendency to react oppositely with the chlorine gas generated on the positive electrode 3. However, by arranging the dividing wall 10, diffusion of floating calcium metal can be prevented, and the back reaction can be effectively suppressed.
  • the temperature of the electrolytic bath around the scraping device 9 can be maintained, to a limited extent, at a temperature not less than the melting point of calcium metal, by immersing and arranging a heater near the scraping device 9. In this way, calcium metal scraped from the negative electrode 4 can be recovered in a molten state.
  • the calcium metal in a molten state is partially dissolved in calcium chloride, and the rest floats up in the electrolytic bath 2. Therefore, calcium chloride having condensed calcium metal is floating around the surface of the electrolytic bath 2 via the dividing wall 10. By extracting floating calcium chloride having condensed calcium metal, for example, it can be used in reduction reactions for titanium tetrachloride.
  • Figs. 3A to 3C show another embodiment of the present invention.
  • Fig. 3B is a conceptual diagram of Fig. 3A seen from direction A
  • Fig. 3C is a conceptual diagram of Fig. 3A seen from direction B.
  • Electrolytic bath 2 comprising calcium chloride is filled in the electrolysis vessel 1 of Fig. 3, and the electrolytic bath 2 is heated to a temperature not less than the melting point of calcium chloride so as to be maintained in a molten state by a heating means, which is not shown. Furthermore, the positive electrode 3 and the negative electrode 4 are immersed and arranged in the electrolytic bath 2.
  • the electrolysis vessel 1 is divided into the electrolysis chamber 1a in which the positive electrode 3 is immersed and the dissolution chamber 1b is isolated by the dividing wall 10 arranged around the surface of the electrolytic bath 2. It should be noted that only the upper part of the electrolytic bath 2 is divided by the dividing wall 10, and the lower part thereof is unified. As shown in Fig. 3C, plural negative electrodes 4 are arranged to enable orbital movement in a circle through the electrolysis chamber 1a and dissolution chamber 1b. These negative electrodes 4 can be revolved in a circle through the electrolysis chamber and dissolution chamber by passing through a sliced channel arranged at a part of the dividing wall 10.
  • Heating function and cooling function are provided to the negative electrode 4. That is, a flow passage in which a heater and a cooling medium can be circulated is arranged inside the negative electrode 4. In this way, the temperature of the negative electrode 4 can be arbitrarily controlled from a temperature not more than the melting point of calcium metal 5 to a temperature not less than the melting point of calcium metal 5.
  • the temperature of the negative electrode 4 is maintained at a temperature not more than the melting point of calcium metal to deposit the calcium metal on the surface of the negative electrode in a solid state.
  • the temperature of the negative electrode 4 is maintained at a temperature not less than the melting point of calcium metal to fuse the calcium metal deposited.
  • Calcium metal 5 is molten and released from the negative electrode 4 and is partially dissolved in calcium chloride, and the rest floats up in the electrolytic bath, to form a calcium metal condensed layer.
  • the calcium metal condensed layer formed at the bath surface of the dissolution chamber of the electrolytic bath 2 is extracted at appropriate times, and for example, it can be used as a reducing agent for titanium oxide in molten-salt electrolysis.
  • Molten-salt electrolysis of calcium chloride was performed by using both the electrolysis vessel and the recovery vessel shown in Fig. 1.
  • Calcium metal is deposited on the negative electrode by controlling the temperature of the electrolytic bath comprising calcium chloride at 800 ⁇ 5°C. As a result, calcium metal having 85% of the weight of the theoretical weight calculated from electricity applied between the positive electrode and negative electrode was recovered.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
EP05765165A 2004-06-30 2005-06-27 Procédé et appareil de production de métal par électrolyse de sel fondu Withdrawn EP1785509A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004192905 2004-06-30
PCT/JP2005/011747 WO2006003864A1 (fr) 2004-06-30 2005-06-27 Procédé et appareil de production de métal par électrolyse de sel fondu

Publications (2)

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EP1785509A1 true EP1785509A1 (fr) 2007-05-16
EP1785509A4 EP1785509A4 (fr) 2008-06-25

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EP05765165A Withdrawn EP1785509A4 (fr) 2004-06-30 2005-06-27 Procédé et appareil de production de métal par électrolyse de sel fondu

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US (1) US20090211916A1 (fr)
EP (1) EP1785509A4 (fr)
JP (1) JP4658053B2 (fr)
AU (1) AU2005258596A1 (fr)
WO (1) WO2006003864A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2123798A4 (fr) * 2007-02-19 2010-03-17 Toho Titanium Co Ltd Appareil pour produire un métal par électrolyse des sels fondus et procédé pour produire du métal à l'aide de l'appareil
CN107385474A (zh) * 2017-08-04 2017-11-24 中南大学 一种氯化钙熔盐电解制钙用电解质及使用该电解质的电解方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009008121A1 (fr) * 2007-07-12 2009-01-15 Toho Titanium Co., Ltd. Procédé pour produire du calcium métallique de pureté élevée, procédé pour produire du titane métallique avec l'utilisation du calcium, et appareil de production de calcium métallique de pureté élevée
JP4934012B2 (ja) * 2007-12-11 2012-05-16 東邦チタニウム株式会社 金属カルシウムの製造方法
JP5138465B2 (ja) * 2008-05-27 2013-02-06 東邦チタニウム株式会社 金属カルシウムの製造方法および製造装置
EP3875635A1 (fr) 2016-03-25 2021-09-08 Elysis Limited Partnership Configurations d'eletrodes pour cellules electrolytiques et procedes associes
US20230279572A1 (en) * 2022-04-26 2023-09-07 Case Western Reserve University System and process for sustainable electrowinning of metal

Citations (3)

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Publication number Priority date Publication date Assignee Title
US2960397A (en) * 1958-09-03 1960-11-15 Dow Chemical Co Separation of calcium metal from contaminants
US3043756A (en) * 1958-07-31 1962-07-10 Dow Chemical Co Calcium metal production
US3226311A (en) * 1959-05-13 1965-12-28 Solvay Process of producing calcium by electrolysis

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2344859A (en) * 1941-02-07 1944-03-21 Abraham L Fox Method of producing calcium boride
JPS5443811A (en) * 1977-09-16 1979-04-06 Asahi Glass Co Ltd Production of metallic lithium
CA2012009C (fr) * 1989-03-16 1999-01-19 Tadashi Ogasawara Procede pour la production electrolytique du magnesium
JPH1053888A (ja) * 1996-08-12 1998-02-24 Central Res Inst Of Electric Power Ind 溶融塩電解装置における被回収金属物質の回収方法及び装置
GB9812169D0 (en) * 1998-06-05 1998-08-05 Univ Cambridge Tech Purification method
JP2002129250A (ja) 2000-10-30 2002-05-09 Katsutoshi Ono 金属チタンの製造方法
JP2003129268A (ja) * 2001-10-17 2003-05-08 Katsutoshi Ono 金属チタンの精錬方法及び精錬装置
NO318164B1 (no) * 2002-08-23 2005-02-07 Norsk Hydro As Metode for elektrolytisk produksjon av aluminiummetall fra en elektrolytt samt anvendelse av samme.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3043756A (en) * 1958-07-31 1962-07-10 Dow Chemical Co Calcium metal production
US2960397A (en) * 1958-09-03 1960-11-15 Dow Chemical Co Separation of calcium metal from contaminants
US3226311A (en) * 1959-05-13 1965-12-28 Solvay Process of producing calcium by electrolysis

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO2006003864A1 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2123798A4 (fr) * 2007-02-19 2010-03-17 Toho Titanium Co Ltd Appareil pour produire un métal par électrolyse des sels fondus et procédé pour produire du métal à l'aide de l'appareil
CN107385474A (zh) * 2017-08-04 2017-11-24 中南大学 一种氯化钙熔盐电解制钙用电解质及使用该电解质的电解方法

Also Published As

Publication number Publication date
EP1785509A4 (fr) 2008-06-25
WO2006003864A1 (fr) 2006-01-12
JP4658053B2 (ja) 2011-03-23
AU2005258596A1 (en) 2006-01-12
JPWO2006003864A1 (ja) 2008-04-17
US20090211916A1 (en) 2009-08-27

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