US2148404A - Production of alkali metals - Google Patents

Production of alkali metals Download PDF

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Publication number
US2148404A
US2148404A US68275A US6827536A US2148404A US 2148404 A US2148404 A US 2148404A US 68275 A US68275 A US 68275A US 6827536 A US6827536 A US 6827536A US 2148404 A US2148404 A US 2148404A
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sodium
alkali metal
amalgam
cell
electrolyte
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US68275A
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Harvey N Gilbert
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EIDP Inc
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EI Du Pont de Nemours and Co
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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
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/02—Electrolytic production, recovery or refining of metals by electrolysis of solutions of light metals
    • C25C1/04—Electrolytic production, recovery or refining of metals by electrolysis of solutions of light metals in mercury cathode cells
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
    • C25B1/36—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in mercury cathode cells
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/033—Liquid electrodes
    • 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
    • C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the 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
    • C25C7/02—Electrodes; Connections thereof
    • C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts

Definitions

  • This invention relates to the electrolysis of alkali metal compounds to produce alkali metals and other valuable products and more particularly to electrolysis processes which utilize liquid 5 metal electrodes.
  • a number of methods have been proposed for producing metallic sodium or sodium compounds by the use of a two-cell system employing a'liquid metal electrode whereby a fused sodium salt is first electrolyzed with a liquid metal cathode to form the sodium alloy and this liquid sodium alloy then-is used'as anode in a cell employing a fused sodium compound as electrolyte, e. g., caus- 'tic soda, whereby metallic sodium is released at the cathode.
  • This method of producing sodium has not enjoyedany substantial commercial use and so far as I am aware is not commercially,
  • a significant disadvantage of this two-cell system of producing sodium has been the excessively high temperatures. These high temperatures, e. g., 350 :0. 5 or higher makit impractical to employ mercury as liquid electrode because of the high vapor pressure of'mercury at such elevated temperatures. Further disadvantages of the high temperatures are that thworking life of the equip- 40 ment is seriously shortened because of the tendency of rapid corrosion at high temperatures, relatively massive and expensive equipment is required, and there is considerable loss of energy in the form of radiated heat.
  • An object of the present invention is to pro- 10 vide a. practicable method whereby an aqueous solution of an alkali metal compound may be electrolyzed witha liquid metal cathode to produce a liquid alkali metal alloy and that alloy be utilized as anode in an electrolytic operation to 15 produce alkali metal, e. g., metallic sodium.
  • an,aqueous solution of sodium chloride is electrolyzed in a cell having a flowing stream of mercury or sodium amalgam as cathode.
  • chlorine is liberated at the anode and means are provided for removing the gaseous chlorine as formed.
  • Sodium liberated at the cathode unites with the mercury to form amalgam, so .that'the liquid cathode flowing from the cell is richer in sodium than the mercury or amalgam entering the cell.
  • the concentration of sodium in the amalgam leaving the cold cell may vary widely; aconcentration of around 0.1 to 0.2% by weight is suitable.
  • the liquid amalgam leaving the cell is led to a second cell in which the amalgam is utilized as anode.
  • the amalgam flows constantly through the second cell.
  • the second cell employs as electrolyte the fused, eutectic mixture of sodium hydroxide and sodium iodide which contains about 55% by weight of sodium hydroxide and 45% by weight of sodium iodide and has a melting point of about 225 C. The temperature of this fused electrolyte is maintained at about 240-250" C.
  • the cathode in this second cell may be made of iron or steel or other suitable conductive material. The electrolysis in the second cell results in constant removal of sodium from the flowing amalgam anode and the liberation of molten sodium metal at the cathode.
  • the molten sodium having a lower specific gravity than that of the electrolyte, rises towards the surface and suitable collecting means are provided above the cathode for entrapping the rising sodium and conducting it out to a closed receiver so that it is kept out of contact from the air. From time to time the collected sodium may be removed from the receiver.
  • halide to be mixed with the hydroxide and the proportions thereof will be determined chiefly by the temperature at which it is desired to operate the electrolytic cell.
  • an electrolyte which has a melting point not greater than about 300 C. I prefer to employ an electrolyte which has a melting point not greater than about 300 C. with such ,an electrolyte-the cell may be operated at temperatures slightly above 300 C., e. g. up to 310 6., at which temperatures the vapor pressure of -mercury is around one-third of an atmosphere and hence the loss in mercury due to vaporizatlon at ordinary pressures is small. .11 the melting point of the electrolyte is not over 250 C. the
  • f'eell may be operated at temperatures sufliciently "low that the vapor pressure of the mercury is not over about one tenth of an atmosphere, under which conditions there is little or no loss of mercury due .to vaporization.
  • vari- -ous fused mixtures containing an alkali metal fer to usesubstantially eutectic mixtures of these substances.
  • Eutectic mixture Melting point C.) NaOH ('79 molar %)+NaBr 260 KOH (72 molar%)+KI 250' KQH (65 molar %)+KBr 300 LiOH (45.5 molar %)+LiI 180 LiOH (45 molar +LiBr 2'75 LiOH (63 molar %)+LiCl 290
  • my invention relates to the electrolysis of alow-melting mixture of alkali metal hydroxide and alkali metal halide, utilizing a liquid alkali metal alloy as anode, so as to liberate alkali metal at the cathode.
  • the mixture of alkali metal hydroxide and halide may be an eutectic mixture or some mixture approximating or approaching the eutectic, i. e., a mixture having a melting point lower than that of its lowest melting component.
  • the invention is not restricted to using alkali metal amalgam as the anode, since other low melting alloys of alkali metals are utilized for this purpose. Examples of such are "Woods metal" and other similar alloys of bismuth, lead, tin and/or cadmium. It is preferable, however, in most cases to use an amalgam electrode.
  • the cell in a bath containing iodide, there is no formation of either iodate or per iodine. Hence the cell may be operated practically indefinitely without changing or replacing the electrolyte or readjusting the composition thereof.
  • I claim: 1. A process for the recovery of an alkali metal from an alloy of said metal having a melting point not higher than about C. comprising employing said alloy in the liquid state as anode in an electrolytic cell which contains as electrolyte a fused mixture of alkali metal hydroxide and alkali metal halide having a melting point below 300 C.
  • a process for the recovery of an alkali metal from an alkali metal amalgam comprising'employing said amalgam as anode in an electrolytic cell which contains asvelectrolyte a fused mixture of alkali metal hydroxide and alkali metal halide, said mixture having a melting point below 3 00 C.
  • a process for the recovery of an alkali metal from an alkali metal amalgam comprising employing said amalgam as anode in an electrolytic cell which contains as electrolyte a fused, substantially eutectic mixture 01. an alkali metal hydroxide and an alkali metal halide.
  • a process for the recovery of sodium from sodium amalgam comprising employing said amalgam as anode in an electrolytic, cell which contains as electrolyte a fused eutectic mixture of sodium hydroxide and sodium iodide,

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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)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Description

Patented Feb. 21, 1939 UNITED STATES 2.148.404 PRODUCTION or ALKALI METALS' Harvey N. Gilbert, Niagara Falls, N. Y., assignor to E. I. du Pont de Nemours & Gompany, Wilmington, Del., a corporation of Delaware No Drawing. Application March 11, 1936,
Serial No. 68,275
. Claims. 204--21) This invention relates to the electrolysis of alkali metal compounds to produce alkali metals and other valuable products and more particularly to electrolysis processes which utilize liquid 5 metal electrodes.
Various methods 'for electrolysis of alkali metal compounds either in the fused state or in aqueous'solutions with the use of circulating liquid metal electrodes are well known. An example of this is the well-known Castner cell used for the production of caustic "soda, wherein mercury serves as the cathode for the electrolysis of aqueous sodium chloride solution. In processes of this nature the alkali metal released at the liquid metal cathode alloys therewith and the liquid alloy then is circulated either to react chemically with water or other substances to produce caustic soda orother sodium compounds.
A number of methods have been proposed for producing metallic sodium or sodium compounds by the use of a two-cell system employing a'liquid metal electrode whereby a fused sodium salt is first electrolyzed with a liquid metal cathode to form the sodium alloy and this liquid sodium alloy then-is used'as anode in a cell employing a fused sodium compound as electrolyte, e. g., caus- 'tic soda, whereby metallic sodium is released at the cathode. This method of producing sodium has not enjoyedany substantial commercial use and so far as I am aware is not commercially,
used at the present time. A significant disadvantage of this two-cell system of producing sodium has been the excessively high temperatures. These high temperatures, e. g., 350 :0. 5 or higher makit impractical to employ mercury as liquid electrode because of the high vapor pressure of'mercury at such elevated temperatures. Further disadvantages of the high temperatures are that thworking life of the equip- 40 ment is seriously shortened because of the tendency of rapid corrosion at high temperatures, relatively massive and expensive equipment is required, and there is considerable loss of energy in the form of radiated heat.
50 in a non-aqueous secondary cell which may be" operated at a low temperature. In such arrangement, mercury (or alkali metal amalgam) would be a suitable metal to serve as the liquid electrode. So far as I am aware, no one heretofore 55 has prepared a commercially feasible method of doing this. It has been proposed to electrolyze aqueous salt solution with a mercury. cathode and employ a. second cell having a liquid ammonia solution of salt as electrolyte, where the amalgam resulting from the first electrolysis 5 7 serves as anode. However, this method has not proved practicable for commercial operation, partly because of the difliculties attending the use of liquid ammonia solution as electrolyte.
An object of the present invention is to pro- 10 vide a. practicable method whereby an aqueous solution of an alkali metal compound may be electrolyzed witha liquid metal cathode to produce a liquid alkali metal alloy and that alloy be utilized as anode in an electrolytic operation to 15 produce alkali metal, e. g., metallic sodium. A
further object is to provide a commercially feasible method for producing sodium metal or other alkali metal) by electrolysis utilizing an v alkali metal amalgam as anode attemperatures 20 at which the vapor pressure of mercury is rela; tively low. Other objects will be hereinafter apparent. I The above objects are accomplished in accordance with the present invention by producing 25 alkali metal amalgam by electrolysis of'an aqueous'alkali metal compound solution with a mercury (or amalgam) cathode and using the amalproduction of sodium) has a melting point of 40 about 225 C. and this mixture may be fused and utilized as molten electrolyte at temperatures of for example 230-250 C. At such relatively low temperatures, the vapor pressure of mercury is less than 1/10 atmosphere.
In one method of practicing the present invention for. the production of sodium which is given by way of example, an,aqueous solution of sodium chloride is electrolyzed in a cell having a flowing stream of mercury or sodium amalgam as cathode. As a result of this electrolysis, chlorine is liberated at the anode and means are provided for removing the gaseous chlorine as formed. Sodium liberated at the cathode unites with the mercury to form amalgam, so .that'the liquid cathode flowing from the cell is richer in sodium than the mercury or amalgam entering the cell. The concentration of sodium in the amalgam leaving the cold cell may vary widely; aconcentration of around 0.1 to 0.2% by weight is suitable. The liquid amalgam leaving the cell is led to a second cell in which the amalgam is utilized as anode. Preferably, the amalgam flows constantly through the second cell. The second cell employs as electrolyte the fused, eutectic mixture of sodium hydroxide and sodium iodide which contains about 55% by weight of sodium hydroxide and 45% by weight of sodium iodide and has a melting point of about 225 C. The temperature of this fused electrolyte is maintained at about 240-250" C. The cathode in this second cell may be made of iron or steel or other suitable conductive material. The electrolysis in the second cell results in constant removal of sodium from the flowing amalgam anode and the liberation of molten sodium metal at the cathode. The molten sodium, having a lower specific gravity than that of the electrolyte, rises towards the surface and suitable collecting means are provided above the cathode for entrapping the rising sodium and conducting it out to a closed receiver so that it is kept out of contact from the air. From time to time the collected sodium may be removed from the receiver.
In addition to the above described eutectic mixture of sodium hydroxide and sodium iodide,
- other'mixtures of these two compounds and varivous other mixtures of alkali metal hydroxides corresponding hydroxides and halides preferably having the proportions of the alkali metals in the electrolyte at least roughly equivalent to the proportions in which these metals occur in the ,alkali metal amalgam anode.
The selection of the halide to be mixed with the hydroxide and the proportions thereof will be determined chiefly by the temperature at which it is desired to operate the electrolytic cell. When using a mercury base anode, I prefer to employ an electrolyte which has a melting point not greater than about 300 C. with such ,an electrolyte-the cell may be operated at temperatures slightly above 300 C., e. g. up to 310 6., at which temperatures the vapor pressure of -mercury is around one-third of an atmosphere and hence the loss in mercury due to vaporizatlon at ordinary pressures is small. .11 the melting point of the electrolyte is not over 250 C. the
f'eell may be operated at temperatures sufliciently "low that the vapor pressure of the mercury is not over about one tenth of an atmosphere, under which conditions there is little or no loss of mercury due .to vaporization. Obviously vari- -ous fused mixtures containing an alkali metal fer to usesubstantially eutectic mixtures of these substances.
lnladditloh to the eutectic mixture 0), hydroxide and sodium iodide which has been mentioned above, the eutectic mixtures shown in the following table illustrate thevariety of compositions which may be utilized to produce electrolytes having relatively low melting points:
Eutectic mixture: Melting point C.) NaOH ('79 molar %)+NaBr 260 KOH (72 molar%)+KI 250' KQH (65 molar %)+KBr 300 LiOH (45.5 molar %)+LiI 180 LiOH (45 molar +LiBr 2'75 LiOH (63 molar %)+LiCl 290 In its broader aspects; my invention relates to the electrolysis of alow-melting mixture of alkali metal hydroxide and alkali metal halide, utilizing a liquid alkali metal alloy as anode, so as to liberate alkali metal at the cathode. In order to obtain a sufficiently low melting point, the mixture of alkali metal hydroxide and halide may be an eutectic mixture or some mixture approximating or approaching the eutectic, i. e., a mixture having a melting point lower than that of its lowest melting component. The invention is not restricted to using alkali metal amalgam as the anode, since other low melting alloys of alkali metals are utilized for this purpose. Examples of such are "Woods metal" and other similar alloys of bismuth, lead, tin and/or cadmium. It is preferable, however, in most cases to use an amalgam electrode.
In carrying out the herein described process in a continuous manner over extended periods of time to produce alkali metals 1' have found that substantially no decomposition of the fusedelectrolyte occurs. The composition of the electrolyte remains substantially unchanged over extended periods of time and there is no evidence of anodic oxidation of the halide. For example,
in a bath containing iodide, there is no formation of either iodate or per iodine. Hence the cell may be operated practically indefinitely without changing or replacing the electrolyte or readjusting the composition thereof.
In practicing the present invention, I prefer to utilize-the method and-i paratusdisclosed and claimed in my copending application flled of even date herewith, whereby the liquid metal electrode is applied on the cell in the form of a thin film on a moving metal surface. In the preferred .form of this method as disclosed in the aforesaid copending application the liquid alkali metal amalgam anode is flowed through-a reservoir in the lower portion of the cell while the fused electrolyte floats on the surface of the amalgam in' the reservoir. A disc rotating on its horizontal axis or other suitable moving surface is arranged partly immersed in the reservoir of amalgam and partly projecting into the electrolyte. By this means the disc is coated with a film of the amalgam and the rotation of the disc constantly brings a thin film of the amalgam from the reservoir into contact with the electrolyte, re-.
turning a thin film of amalgam from which a portion of the alkali metal has been removed by electrolytic action. 1
I claim: 1. A process for the recovery of an alkali metal from an alloy of said metal having a melting point not higher than about C. comprising employing said alloy in the liquid state as anode in an electrolytic cell which contains as electrolyte a fused mixture of alkali metal hydroxide and alkali metal halide having a melting point below 300 C.
2. A process for the recovery of an alkali metal from an alkali metal amalgam comprising'employing said amalgam as anode in an electrolytic cell which contains asvelectrolyte a fused mixture of alkali metal hydroxide and alkali metal halide, said mixture having a melting point below 3 00 C.
3. A process for the recovery of an alkali metal from an alkali metal amalgam comprising employing said amalgam as anode in an electrolytic cell which contains as electrolyte a fused, substantially eutectic mixture 01. an alkali metal hydroxide and an alkali metal halide.
4. A process for the recovery of sodium from sodium amalgam comprising employing said amalgam as anode in an electrolytic, cell which contains as electrolyte a fused eutectic mixture of sodium hydroxide and sodium iodide,
- HARVEY N. GILBERT.
US68275A 1936-03-11 1936-03-11 Production of alkali metals Expired - Lifetime US2148404A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2660514A (en) * 1949-04-08 1953-11-24 Frederick A Rohrman Removal of nitrogen from mixtures of combustible gases
US2867568A (en) * 1955-09-01 1959-01-06 Horizons Inc Electrolytic production of hydrides
US3472745A (en) * 1967-03-08 1969-10-14 North American Rockwell Fusible alkali-metal salt electrolyte
US4156635A (en) * 1978-03-29 1979-05-29 The United States Of America As Represented By The United States Department Of Energy Electrolytic method for the production of lithium using a lithium-amalgam electrode
US20040011662A1 (en) * 2002-03-15 2004-01-22 Millennium Cell, Inc. Hydrogen-assisted electrolysis processes
US20060102491A1 (en) * 2004-11-10 2006-05-18 Kelly Michael T Processes for separating metals from metal salts

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2733202A (en) * 1956-01-31 Electrolytic cells
US2542523A (en) * 1941-08-27 1951-02-20 Ici Ltd Electrolysis of aqueous salt solutions in liquid cathode cells
DE871063C (en) * 1942-12-13 1953-03-19 Lech Chemie Gersthofen Process for the extraction of alkali metals
US2773824A (en) * 1944-09-14 1956-12-11 Robert Q Boyer Electrolytic cells
US2598228A (en) * 1945-02-03 1952-05-27 Wyandotte Chemicals Corp Electrolytic apparatus
US2539743A (en) * 1946-01-03 1951-01-30 Reynolds Metals Co Electrolytic refining of impure aluminum
US2812304A (en) * 1946-01-09 1957-11-05 John A Wheeler Means for cooling reactors
US2840520A (en) * 1954-07-26 1958-06-24 Wurbs Alfred Production of amalgams
DE1009172B (en) * 1954-10-07 1957-05-29 Habil Ludwig Kandler Dipl Phys Process for the electrical use of the decomposition energy of amalgams
US3311504A (en) * 1960-05-02 1967-03-28 Leesona Corp Fuel cell
US3085968A (en) * 1960-08-16 1963-04-16 Olin Mathieson Cathode sealing means for electrolytic cell
US3265490A (en) * 1963-04-09 1966-08-09 Tekkosha Co Production of alkali metals from alkali amalgam
US3427237A (en) * 1967-05-01 1969-02-11 Thomas M Morris Electrolysis method and electrolytic cell
GB1226036A (en) * 1967-10-14 1971-03-24
US9163297B2 (en) * 2012-08-07 2015-10-20 Justin Langley Method for the integration of carbochlorination into a staged reforming operation as an alternative to direct residue oxidation for the recovery of valuable metals

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE158574C (en) *
DE73304C (en) * C. TH. J. VAUTIN in London, England Mercury cathode for electrolytic cells
GB190317640A (en) * 1903-08-14 1904-08-13 Edgar Arthur Ashcroft Improvements in or relating to the Production of Alkali Metals.
DE410180C (en) * 1920-12-13 1925-03-02 Gualtiero Poma Process for the reduction of organic or inorganic substances using sodium amalgam
DE630145C (en) * 1934-06-02 1936-05-22 I G Farbenindustrie Akt Ges Process for the production of inorganic and organic salts of alkali or alkaline earth metals

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2660514A (en) * 1949-04-08 1953-11-24 Frederick A Rohrman Removal of nitrogen from mixtures of combustible gases
US2867568A (en) * 1955-09-01 1959-01-06 Horizons Inc Electrolytic production of hydrides
US3472745A (en) * 1967-03-08 1969-10-14 North American Rockwell Fusible alkali-metal salt electrolyte
US4156635A (en) * 1978-03-29 1979-05-29 The United States Of America As Represented By The United States Department Of Energy Electrolytic method for the production of lithium using a lithium-amalgam electrode
US20040011662A1 (en) * 2002-03-15 2004-01-22 Millennium Cell, Inc. Hydrogen-assisted electrolysis processes
US20060169593A1 (en) * 2002-03-15 2006-08-03 Jianguo Xu Hydrogen-assisted electrolysis processes
US7108777B2 (en) * 2002-03-15 2006-09-19 Millennium Cell, Inc. Hydrogen-assisted electrolysis processes
US20060102491A1 (en) * 2004-11-10 2006-05-18 Kelly Michael T Processes for separating metals from metal salts

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FR818993A (en) 1937-10-07
US2234967A (en) 1941-03-18
BE420511A (en) 1937-04-30
DE891027C (en) 1953-09-24
DE898815C (en) 1953-12-03

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