EP2123798A1 - Vorrichtung zur herstellung von metall durch schmelzflusselektrolyse und verfahren zur herstellung von metall unter verwendung der vorrichtung - Google Patents

Vorrichtung zur herstellung von metall durch schmelzflusselektrolyse und verfahren zur herstellung von metall unter verwendung der vorrichtung Download PDF

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Publication number
EP2123798A1
EP2123798A1 EP08702801A EP08702801A EP2123798A1 EP 2123798 A1 EP2123798 A1 EP 2123798A1 EP 08702801 A EP08702801 A EP 08702801A EP 08702801 A EP08702801 A EP 08702801A EP 2123798 A1 EP2123798 A1 EP 2123798A1
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EP
European Patent Office
Prior art keywords
metal
electrolysis
cathode
production
molten
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Withdrawn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
EP08702801A
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English (en)
French (fr)
Other versions
EP2123798A4 (de
Inventor
Yuichi Ono
Masanori Yamaguchi
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.)
Toho Titanium Co Ltd
Original Assignee
Toho Titanium 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 Toho Titanium Co Ltd filed Critical Toho Titanium Co Ltd
Publication of EP2123798A1 publication Critical patent/EP2123798A1/de
Publication of EP2123798A4 publication Critical patent/EP2123798A4/de
Withdrawn legal-status Critical Current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
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
    • 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
    • C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline 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
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
    • C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process

Definitions

  • the present invention relates to an apparatus and to a method for production of metal by electrolysis of molten salt, and in particular, relates to a technique for efficient processing for the production of metal that is soluble in an electrolysis bath.
  • Titanium metal has been conventionally widely used as materials and parts for aviation; recently, demand for this titanium metal has greatly increased for consumer uses, for example, and it has also been anticipated that the supply of titanium sponge, which is a raw material of titanium metal, will need to be increased.
  • titanium sponge is industrially produced by the Kroll method, in which titanium tetrachloride is reduced by a reducing metal such as magnesium.
  • a reducing metal such as magnesium
  • an apparatus for molten salt electrolysis of calcium chloride such as is shown in Fig. 3
  • solid calcium metal 8 is deposited on the cathode 3, which is cooled to a temperature of not more than the melting point of calcium metal, the calcium metal 8 is transferred to another container 11, and it is heated to be melted and recovered.
  • another apparatus for recovery is necessary in addition to the electrolysis vessel, the overall process is complicated.
  • An object of the present invention is to provide a process for production of metal by molten salt electrolysis, and in particular, a process for production of metal, in which metal that is soluble in an electrolysis bath can be efficiently produced and recovered.
  • the inventors discovered that in an apparatus and a method for production of metal by molten salt electrolysis, after a cathode having a flow passage for a cooling medium inside is arranged in an electrolysis bath and solid metal is deposited on the cathode, the solid metal deposited on the cathode is melted in the electrolysis bath by disconnecting the electric current to the cathode, and the molten metal is continuously removed to the outside of the electrolysis vessel to efficiently recover the metal, and thus the present invention was completed.
  • the process for production of metal by molten salt electrolysis of the present invention in which an electrolysis vessel is filled with an electrolysis bath, and anode and cathode are immersed and arranged in the vessel, is characterized in that metal is deposited on the cathode having a flow passage for a cooling medium inside, electric current to the cathode is disconnected to melt the deposited metal into the electrolysis bath, and the molten metal is continuously removed to the outside of the electrolysis vessel.
  • the present invention is also characterized in that the temperature of the surface of the cathode is maintained at not less than the melting point of the electrolysis bath and not more than the melting point of the deposited metal, and temperature of the electrolysis bath is maintained at not less than the melting point of the deposited metal.
  • the present invention is also characterized in that the cathode wall and the anode wall are immersed and arranged respectively around the cathode and anode.
  • the present invention is also characterized in that plural electrodes are arranged in the electrolysis bath (hereinafter referred to as a “multiple-electrode electrolysis vessel"), each electrode has a cycle consisting of a connected mode and a disconnected mode of electric current, and molten metal is removed by disconnecting electric current in one electrode during molten salt electrolysis is performed by connecting electric current in another electrode, and by rotating these modes, melt metal can be continuously removed from the multiple-electrode electrolysis vessel.
  • the metal can be produced more efficiently and in an apparatus with simpler structure compared to conventional techniques, and as a result, high efficiency of electric current can be realized.
  • FIG. 1 and 2 show embodiments of an apparatus to perform the present invention. Hereinafter, preferred embodiments are explained by way of these figures.
  • Fig. 1 conceptually shows an apparatus M for molten salt electrolysis used in the present invention.
  • the left part of Fig. 1 is a conceptual diagram of the apparatus M for molten salt electrolysis during electrolysis.
  • the apparatus M for molten salt electrolysis includes an electrolysis vessel 1 and an electrolysis bath 2 filled therein, and melt at a temperature not less than its melting point is maintained in the melt condition by a heating means (not shown).
  • a heating means not shown
  • the electrolysis bath 2 includes a cathode 3 and an anode 4 immersed therein, and a cathode wall 5 and an anode wall 6 immersed therein surrounding respectively around the cathode 3 and anode 4.
  • the lower part of these walls is open, and the electrolysis bath 2 can flow into the inside of the walls.
  • the cathode 3 is shown in a perspective view so as to make the inside visible.
  • the inside of the cathode 3 has a structure enabling the flowing of cooling medium 7 to control the temperature of the cathode itself.
  • the metal can be deposited as a solid metal 8 as shown in the left part of Fig. 1 .
  • the metal can be floated to surface of the electrolysis bath as a molten metal 10 as shown in the right part of Fig. 1 .
  • the molten metal 10 can be removed to the outside by using a removing tube 9.
  • the metal deposited by the molten salt electrolysis is calcium metal and the electrolysis bath is calcium chloride, it is desirable that after the deposited metal on the cathode 3 is melted in the electrolysis bath that it be removed to the outside of the electrolysis vessel 1 immediately.
  • FIG. 1 The right part of Fig. 1 is a conceptual diagram of the metal removing process of the metal generated in the electrolysis bath 2 after the molten salt electrolysis is terminated.
  • reference numeral 9 is a removing tube for the molten metal, and it is used to recover the molten metal.
  • chloride of the deposited metal on cathode 3 be used as the electrolysis bath 2, and that calcium chloride or a complex salt containing calcium chloride be used as the electrolysis bath 2 in a case in which the deposited metal is calcium.
  • a complex salt containing calcium chloride and potassium chloride as the complex salt since the decomposition voltage of potassium chloride is higher than that of calcium chloride, it is desirable that a voltage applied to between electrodes of the present invention be not less than the decomposition voltage of calcium chloride and not greater than the decomposition voltage of potassium chloride.
  • the surface temperature of the cathode 3 immersed in the electrolysis bath 2 be set at a temperature not less than the melting point of the electrolysis bath 2 and not greater than the melting point of the deposited metal, and at the same time, the temperature of the electrolysis bath 2 be set to a temperature not less than the melting point of the deposited metal.
  • the deposited metal is calcium
  • the calcium metal once deposited on the cathode in solid state can be melted in the electrolysis bath 2, and thus, the calcium metal in melt state can be efficiently removed to the outside.
  • a complex salt in which potassium chloride is added to calcium chloride is desirable.
  • the melting point of the electrolysis bath 2 can be decreased compared to a case in which calcium chloride is used alone as the electrolysis bath.
  • a range of controlling temperature of the cathode can be broadened and operation can be facilitated.
  • the operation temperature of the cathode can be set at a lower temperature range compared to the conventional operation, calcium metal can be efficiently deposited on the cathode 3.
  • solubility of the calcium metal in the electrolysis bath 2 can be reduced, and as a result, calcium metal can be efficiently recovered.
  • the temperature of the electrolysis bath 2 is set at 870°C and the surface temperature of the cathode 3 is set at 750°C
  • calcium metal in a solid state can be deposited on the cathode 3. It should be noted that it is desirable that the difference in temperatures between cathode 3 and the melting point of calcium metal be greater.
  • the complex salt having a lower melting point than that of calcium chloride alone as the electrolysis bath 2 as mentioned above the temperature of the cathode 3 can be decreased.
  • the tube 9 for removing molten calcium metal be inserted into the electrolysis bath 2 between the cathode 3 and the cathode wall 5.
  • one end of the tube 9 for removing molten calcium metal be connected to a pressure reducing device (not shown) to enable extracting the molten metal to which the other end of the tube 9 for removing molten calcium metal is immersed.
  • the calcium metal deposited on the cathode 3 can be melted into the electrolysis bath 2.
  • the calcium metal melt in the electrolysis bath 2 can be removed to the outside through the tube 9 for removing molten calcium metal. It should be noted that during removing, the deposited solid metal 8 on the cathode 3 can be smoothly melted by stopping the flow of the cooling medium 7 in the cathode 3.
  • the cathode wall 5 be arranged around the cathode 3. By arranging the wall 5, dispersion of the molten calcium metal 10 from the cathode 3 can be effectively restrained.
  • the amount of electrolysis bath 2 contained in the removed metal be as small as possible.
  • the depth of the tube 9 for removing molten calcium metal immersed in the electrolysis bath 2 be shallower than the depth of the calcium metal expected on the cathode 3. In this way, calcium metal having high purity and being melted in the electrolysis bath can be efficiently removed.
  • Fig. 2 shows another desirable aspect of the present invention.
  • a multiple-electrode molten salt electrolysis apparatus P is constructed by arranging a anode 4 and ten cathodes 3 surrounding the anode in an electrolysis vessel 1.
  • Fig. 2 is a plane view in which the electrolysis vessel 1 is viewed downwardly from its surface to its bottom.
  • each cathode can be easily set in an electrolysis period and a pause period.
  • the electrolysis period means a period in which calcium metal is deposited in a solid phase on the surface of the cathode, as mentioned above, and the pause period means a period in which molten salt electrolysis is stopped by disconnecting the cathode 3 and a power resource, the solid calcium metal 8 deposited on the cathode 3 is melted in the electrolysis bath, and simultaneously the calcium metal is removed from the electrolysis vessel 1 via the tube 9 for removing molten calcium metal to migrate it to the reduction process.
  • the calcium metal can be continuously produced by the multiple-electrode molten salt electrolysis apparatus P.
  • the calcium metal produced can be efficiently used as a reducing agent used in a direct reduction of titanium oxide or in a reduction of titanium tetrachloride.
  • calcium chloride which is a by-product of the reduction process, can be reused as a raw material of calcium metal, which is a reducing agent, by returning it to the electrolysis vessel 1 as shown in Fig. 2 .
  • chlorine gas generated in the anode 4 can be used in a chlorination reaction of titanium oxide to produce titanium tetrachloride, which is a raw material of the reduction reaction of titanium.
  • the cathode 3 on which calcium metal 8 is deposited be made of metal having electric conductivity, and in particular, be of stainless steel or titanium metal.
  • a cathode 3 made of such material can deposit calcium metal having high purity.
  • the cathode 3 have a structure so that the cooling medium 7 can flow inside the electrode.
  • the surface temperature of the cathode 3 can be efficiently maintained at a temperature not greater than or not less than the melting point of calcium metal.
  • the surface temperature of the cathode 3 is maintained at a temperature not greater than the melting point of calcium metal by flowing the cooling medium 7 inside the cathode 3 in a case in which metal is to be deposited on the cathode 3, and the surface temperature of the cathode 3 is maintained at a temperature not less than the melting point of calcium metal by stopping the flow of the cooling medium 7 in a case in which solid metal deposited 8 on the cathode 3 is to be melted in the electrolysis bath 2.
  • the cooling medium that is flowed in the cathode 3 air or inert gas may be used.
  • the anode 4 since chlorine gas is generated on the anode 4, it is desirable that the anode 4 be made of carbon or graphite having corrosion resistance against chlorine gas at high temperature. By the anode 4 being such a material, damage to the anode 4 can be minimized and chlorine gas can be efficiently recovered.
  • the silicon nitride is desirable as a material in the present invention since it has corrosion resistance against chlorine gas in addition to corrosion resistance against calcium metal and calcium chloride.
  • the electrolysis vessel 1 is made of a material having corrosion resistance against calcium chloride or potassium chloride having high temperature, and stainless steel or titanium metal is desirable.
  • the tube 9 for removing molten calcium metal of the electrolysis bath 2 can be made of a metallic material having corrosion resistance such as stainless steel, which can be easily replaced when it is corroded.
  • molten calcium metal can be effectively produced.
  • titanium metal can be produced by effectively reducing titanium tetrachloride or titanium oxide.
  • molten calcium metal was produced by molten salt electrolysis of calcium chloride.
  • molten salt electrolysis was performed by connecting the electric current in the left half area of the electrolysis vessel, and solid calcium metal deposited on the cathode was melted and removed from the electrolysis vessel to supply it to a titanium reducing process by disconnecting the electric current in the right half area of the electrolysis vessel.
  • molten calcium could be substantially and continuously supplied from the electrolysis vessel shown in Fig. 2 to the titanium reducing process.
  • initial investment could be reduced by 90%.
  • the apparatus is easy to use compared to a conventional one, and energy for melting calcium metal deposited on the cathode can be reduced about 88%.

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  • 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)
EP08702801A 2007-02-19 2008-01-22 Vorrichtung zur herstellung von metall durch schmelzflusselektrolyse und verfahren zur herstellung von metall unter verwendung der vorrichtung Withdrawn EP2123798A4 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2007037873 2007-02-19
PCT/JP2008/000060 WO2008102520A1 (ja) 2007-02-19 2008-01-22 溶融塩電解による金属の製造装置およびこれを用いた金属の製造方法

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EP2123798A1 true EP2123798A1 (de) 2009-11-25
EP2123798A4 EP2123798A4 (de) 2010-03-17

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EP08702801A Withdrawn EP2123798A4 (de) 2007-02-19 2008-01-22 Vorrichtung zur herstellung von metall durch schmelzflusselektrolyse und verfahren zur herstellung von metall unter verwendung der vorrichtung

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EP (1) EP2123798A4 (de)
JP (1) JPWO2008102520A1 (de)
WO (1) WO2008102520A1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014202199A (ja) * 2013-04-10 2014-10-27 株式会社エム光・エネルギー開発研究所 火力発電所の温排水と高温廃熱の利用方法
CN106917114A (zh) * 2017-04-12 2017-07-04 攀钢集团研究院有限公司 金属钛粉熔盐电解回收装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6270446B2 (ja) * 2013-12-06 2018-01-31 東邦チタニウム株式会社 溶融塩電解による金属の製造方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006003864A1 (ja) * 2004-06-30 2006-01-12 Toho Titanium Co., Ltd. 溶融塩電解による金属の製造方法および製造装置
WO2006040978A1 (ja) * 2004-10-12 2006-04-20 Toho Titanium Co., Ltd. 溶融塩電解による金属の製造方法および製造装置

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5443811A (en) * 1977-09-16 1979-04-06 Asahi Glass Co Ltd Production of metallic lithium
JPS6237387A (ja) * 1985-08-12 1987-02-18 Sumitomo Light Metal Ind Ltd 高純度リチウムの製造方法
GB9812169D0 (en) 1998-06-05 1998-08-05 Univ Cambridge Tech Purification method
JP4395386B2 (ja) 2003-10-10 2010-01-06 株式会社大阪チタニウムテクノロジーズ Ｃａ源の循環によるＴｉ又はＴｉ合金の製造方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006003864A1 (ja) * 2004-06-30 2006-01-12 Toho Titanium Co., Ltd. 溶融塩電解による金属の製造方法および製造装置
WO2006040978A1 (ja) * 2004-10-12 2006-04-20 Toho Titanium Co., Ltd. 溶融塩電解による金属の製造方法および製造装置

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO2008102520A1 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014202199A (ja) * 2013-04-10 2014-10-27 株式会社エム光・エネルギー開発研究所 火力発電所の温排水と高温廃熱の利用方法
CN106917114A (zh) * 2017-04-12 2017-07-04 攀钢集团研究院有限公司 金属钛粉熔盐电解回收装置

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WO2008102520A1 (ja) 2008-08-28
JPWO2008102520A1 (ja) 2010-05-27
EP2123798A4 (de) 2010-03-17

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