US2987462A - High temperature electrolytic cell - Google Patents

High temperature electrolytic cell Download PDF

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Publication number
US2987462A
US2987462A US663461A US66346157A US2987462A US 2987462 A US2987462 A US 2987462A US 663461 A US663461 A US 663461A US 66346157 A US66346157 A US 66346157A US 2987462 A US2987462 A US 2987462A
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United States
Prior art keywords
muffle
valve
crucible
chamber
cell
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Expired - Lifetime
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US663461A
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English (en)
Inventor
Chauvin Guy
Coriou Henri
Hure Jacques
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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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
    • 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
    • C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts

Definitions

  • the present invention relates to electrolytic cells and in particular to cells for the preparation of high purity metals or alloys by electrolysis of salts in the molten state at high temperature.
  • the chief object of our invention is to provide a cell of this type which permits of easily degassing the vessel in which electrolysis takes place, and possibly the salts which constitute the electrolyte, before electrolysis proper, of performing electrolysis under a vacuum or in an inert atmosphere, and of cooling down the resulting electrolytic deposit under a vacuum or in an inert atmosphere.
  • the electrolytic cell includes a mullie (intended to receive the treatment crucible) and at least one cooling chamber (for cooling down the treated electrode), this mulfie and this chamber being metallic and means being provided for either placing them in communication with each other or separating them from each other, said means including a gastight valve device of the type comprising a sliding unit.
  • a gastight valve device of the type comprising a sliding unit.
  • the mufile and the chamber are each provided with such a valve device and they are connected together in detachable manner by a direct and gastight connection between these two valve devices.
  • a degassing at high temperature from 800 to 1000 C. for instance
  • a vacuum mm. of Hgfor instance of the whole of the cell before electrolysis proper
  • An electrolysis, and subsequently a cooling, of the electrolytic deposit performed in a vacuum or in an inert atmosphere.
  • the metals or alloys thus prepared must, in order to have good mechanical characteristics, a good resistance to corrosion, a low absorption cross section in the case of nuclear applications, and so on, contain as little as possible of impurities and in particular very low amounts of oxygen and nitrogen. Oxygen is particularly difi'icult to eliminate.
  • Patented June 6, 1961 extraction of the salts therefrom is never perfect and these salts may ooze out during the next operation.
  • the cell is made of two metallic parts, to wit, a mufile and a cooling chamber, each preferably including a gastight valve device of the type comprising a sliding unit, said two parts being connected together through this valve device.
  • the metallic mufile is vertical, It is heated externally and is insulated either by means of refractory materials or by means of screens and waterjackets. The whole is surrounded by a metallic casing which may be cooled or not. Furthermore, the mufile is provided at its lower part with a valve device making it possible to ensure either gastightness under a vacuum or circulation of a suitable gas through the mufile. This valve device is protected from the hot source.
  • the cooling chamber which is also metallic, is cooled down by a circulation of fluid. It is provided at its upper part with a valve device making it possible to ensure either gastightness under a vacuum or circulation of a suitable gas through the chamber. It is further provided with a gastight and insulating passage for the electrode.
  • valve device At the upper part of the mufile there is provided a gastight sliding valve device which will be hereinafter called the lower valve device.
  • This device is of the type described in our French patent application No. 715,869 of June 5, 1956.
  • Ilhe chamber has its lower part fixed to another sliding valve device of the same type which will be hereinafter called the upper valve device.
  • Such a sliding valve device essentially includes a casing and a sliding unit movable in said casing under the action of an external control member so as to be able either to close or to clear the opening which is to be controlled.
  • the packing joints which achieve gastightness in such a valve are cooled by means of a circulation of fluid in their vicinity, this circulation advantageously taking place in circuits provided in the casing.
  • the nature of the metals and/or alloys used for the construction of the cell depends essentially upon the temperature to which they are subjected and upon the possible corrosion they may undergo from the gaseous products evolved during electrolysis.
  • the electrolytic cell according to our invention has many advantages over the known systems.
  • FIG. 1 is a sectional View of the electrolytic cell according to our invention.
  • FIG. 2 shows a modification of a part of the cell of FIG. 1.
  • the electrolytic cell of FIG. 1 includes the oven proper 1, the cooling chamber 2 and the two gastight valve devices 3 and 4. a
  • T he'oven 1 includes a metallic muffle 5 resting upon a support 6 and heated by a heating element 7 The whole is surrounded by a heat insulating envelope. Advantageously there is mounted between the heating element 7 and the heat insulating envelope 8 a muffle 9 for protection of said envelope. The whole is .containedin a metal casing 10.
  • crucible 11 which is for instance made of graphite. It rests uponapositioning plate 12 made of a conductor material and resting, through insulating means 13, upon the bottom of muflle 5. Current is fed to said plate 12 through 'a wire 14 which passes through the wall of mufile 5 inside an insulating block 15.
  • valve device 21 which may be cooled in a suitable manner.
  • the cooling chamber 2 includes a metal envelope 22 cooled by a water-jacket 23 and provided with a valve device 24.
  • the electrode, in this case cathode 25, passes through the upper part of said chamber 2, gastightness being ensured by packing joint 26 which is cooled by water-jacket 23.
  • V i i The upper valve device 3 includes a casing made of two portions, the lower one 34 and the upper one 35, between which can move a sliding unit'operated by means of a rod 36 passing through the wall of said casing.
  • Said sliding unit includes a supporting plate 37Vand a cover 38 slidable vertically thereon. This cover 38 can be displaced in a direction at right angles to the direction 4 obtained by rotation of an eccentric cam 40 rigid with rod 36.
  • the packing joints which ensure gastightness between the two portions 34 and 35 of the casing, between the lower portion 34 and the lower valve device 4, between the upper portion 35 and cooling chamber 2, and also joint 40, are preferably toroidal and are cooled by circulation of fluid in their immediate vicinity, this circulation taking place through a circuit preferably provided in the walls of the casing.
  • the lower valve device 4 is made similarly.
  • valve devices achieve a very good gastightness even when they are subjected to the action of high temperatures; they are strong, easy to operate and permit of quickly obtaining great areas of opening.
  • the upper valve device 3 is shown in closed position with its cover 38 applied against the upper casing portion 35.
  • the lower valve device 4 is shown in closing position but with the cover of its sliding unit loosened.
  • FIG. 2. shows a modification of the device for feeding current to positioning plate 12 on which crucible 11 is resting.
  • the metallic muffle 5 carries at its lower end, beyond the cooling jacket 20, a gastight chamber 27.
  • This chamber is provided with a valve device 28 and insulating means 29 for the passage of an electric conductor through the wall of said chamber; electric connection between plate 12 and conduct 30 is ensured by means of a contact rod 31 rigid with plate 12 and a flexible wire 32.
  • valve device 4 is opened by rotating rod 36 through an angle of 90 and then pulling said rod outwardly.
  • Valve device 4 is closed by pushing in rod 36 and rotating it about its axis through an angle of 90 in a direction opposed to that of the above mentioned rotation of said rod.
  • Valve device 17 is closed and the desired vacuum is produced in oven 1 by pumpng out the air present therein through the valve device 21; the oven is heated and degassing is performed at the desired temperature and pressure.' When a sufficient degassing has been obtained, atmospheric pressure is restored by introducing an inert gas through valve device 17. This gas will be evacuated through valve device 21 or possibly through valve device 4.
  • the salts are introduced into crucible 11 for instance throughthe opening of valve device 4, this operation being effected quickly and smoothly so as to introduce the minimum amount of air into the mufile.
  • the salts are then melted in an inert atmosphere or undervacuum. In the latter case, and when it is desired to degas the salts preliminarily under vacuum without waiting for of. movement of the sliding unit so as to ensure a gastight' closing of the valve device by crushing of a toroidal joint 39.
  • This displacement of cover 38 is advantageously their being melted, the operation isidentical to the above described degassing operation.
  • the salts being in the molten state, .the atmosphere inside the oven is constituted by an inert gas, this gas entering through valve device 17 and issuing through valve device 21, sliding valve device 4 being closed.
  • the cooling chamber 2 is then fitted as shown by FIG. 1, the upper electrode 25 (in this case the cathode being in position. Screws, not visible on the drawing. permit of securing valvedevice 3 to valve device'4, gastightness being ensured by toroidal packing joint 33. Chamber'Z is degassed, if so desired, through valve device 24, after which an'inert' atmosphere 'is provided in said chamber.
  • Valve .devices 3' and 4 are opened.
  • Thevalve device 21 of the murate is closed and the valve device124of the chamber is opened.
  • Cathode 25 is lowered and electrolysis is performed either in a vacuum or in an inert atmosphere.
  • cathode 25 with its deposit is lifted into the cooling chamber 2. Sliding valve device 3 is closed. The deposit is left to cool down either in an inert atmosphere (possibly with a light over-pressure), valve device 24 being closed, or in a vacuum.
  • valve device 4 has been closed and valve device '21 opened to permit gas circulation. Chamber 2 is then removed and replaced by another chamber if so desired.
  • An electrolytic cell comprising a metallic muffle, an electrically conductive crucible in said muflle spaced from the walls of said mufile and electrically insulated therefrom, means for heating said muflle, means for electrically heating said crucible, a cooling chamber removably mounted above said muffle, said cooling chamber having an opening at the lower end thereof located above the top end of said crucible, gastight valve means interposed between said muflie and said chamber for either placing them in communication with each other or separating them from each other, said valve means including a gastight valve device carried by said mufile at the top end thereof to control the opening thereof, the valve opening being of such size as to allow introduction and removal of said crucible, a gastight valve device carried by said cooling chamber at the lower end thereof to control the opening thereof, gastight means joining said two valve devices, and an electrode mounted on said cooling chamber and vertically slidable therein for lowering into said crucible when both said valve devices are open.
  • gastight means include a toroidal packing joint and fluid circulation means for cooling said joint.

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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)
US663461A 1956-06-07 1957-06-04 High temperature electrolytic cell Expired - Lifetime US2987462A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1100975X 1956-06-07

Publications (1)

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US2987462A true US2987462A (en) 1961-06-06

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US663461A Expired - Lifetime US2987462A (en) 1956-06-07 1957-06-04 High temperature electrolytic cell

Country Status (7)

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US (1) US2987462A (de)
BE (1) BE558118A (de)
CH (1) CH349793A (de)
DE (1) DE1100975B (de)
FR (1) FR1152244A (de)
GB (1) GB857602A (de)
LU (1) LU36189A1 (de)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3098028A (en) * 1961-02-17 1963-07-16 Jr Lawrence J Mullins Plutonium electrorefining cells
US3201229A (en) * 1961-12-20 1965-08-17 Dow Chemical Co Cesium production
US3226310A (en) * 1960-12-19 1965-12-28 Ciba Ltd Electrolytic fusion cells and method of operating the same
CN103834969A (zh) * 2012-11-23 2014-06-04 宁波创润新材料有限公司 熔盐电解装置
CN103993335A (zh) * 2014-05-29 2014-08-20 东北大学 一种熔盐电解-浇铸直接制备铝合金的装置及方法
CN111398012A (zh) * 2020-03-30 2020-07-10 河北南玻玻璃有限公司 一种矿物原料熔样装置及重金属铬检测方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1295578A (fr) * 1961-04-28 1962-06-08 Electrochimie Soc Dispositif pour formation de bains d'électrolyse ignée
FR1295579A (fr) * 1961-04-28 1962-06-08 Electrochimie Soc Nouvel appareil d'électrolyse ignée

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1838666A (en) * 1925-08-12 1931-12-29 Colin G Fink Electroplating apparatus
US2760930A (en) * 1952-01-31 1956-08-28 Nat Lead Co Electrolytic cell of the diaphragm type
US2838454A (en) * 1954-10-12 1958-06-10 Norton Co Electrolytic cell

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1838666A (en) * 1925-08-12 1931-12-29 Colin G Fink Electroplating apparatus
US2760930A (en) * 1952-01-31 1956-08-28 Nat Lead Co Electrolytic cell of the diaphragm type
US2838454A (en) * 1954-10-12 1958-06-10 Norton Co Electrolytic cell

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3226310A (en) * 1960-12-19 1965-12-28 Ciba Ltd Electrolytic fusion cells and method of operating the same
US3098028A (en) * 1961-02-17 1963-07-16 Jr Lawrence J Mullins Plutonium electrorefining cells
US3201229A (en) * 1961-12-20 1965-08-17 Dow Chemical Co Cesium production
CN103834969A (zh) * 2012-11-23 2014-06-04 宁波创润新材料有限公司 熔盐电解装置
CN103834969B (zh) * 2012-11-23 2016-08-03 宁波创润新材料有限公司 熔盐电解装置
CN103993335A (zh) * 2014-05-29 2014-08-20 东北大学 一种熔盐电解-浇铸直接制备铝合金的装置及方法
CN103993335B (zh) * 2014-05-29 2016-01-20 东北大学 一种熔盐电解-浇铸直接制备铝合金的装置及方法
CN111398012A (zh) * 2020-03-30 2020-07-10 河北南玻玻璃有限公司 一种矿物原料熔样装置及重金属铬检测方法

Also Published As

Publication number Publication date
BE558118A (de)
CH349793A (fr) 1960-10-31
DE1100975B (de) 1961-03-02
FR1152244A (fr) 1958-02-13
LU36189A1 (de)
GB857602A (en) 1961-01-04

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