US2931719A - Process and apparatus for the production of metals by dissociation of their carbides - Google Patents

Process and apparatus for the production of metals by dissociation of their carbides Download PDF

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Publication number
US2931719A
US2931719A US682447A US68244757A US2931719A US 2931719 A US2931719 A US 2931719A US 682447 A US682447 A US 682447A US 68244757 A US68244757 A US 68244757A US 2931719 A US2931719 A US 2931719A
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carbides
dissociation
electrodes
residue
carbide
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US682447A
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English (en)
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Menegoz Charles Daniel
Galy Andre Jacques
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Pechiney SA
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Pechiney SA
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    • 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
    • C22B21/00—Obtaining aluminium
    • C22B21/0038—Obtaining aluminium by other processes
    • C22B21/0053—Obtaining aluminium by other processes from other aluminium compounds
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • 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
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • 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
    • C22B47/00—Obtaining manganese
    • 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
    • C22B5/00—General methods of reducing to metals

Definitions

  • the present invention which isthe result of applicants researches, relates to a process. and an apparatus for the. production of metals by the, dissociation of their car bides.
  • the process whichr is the object of the present invention consists in passing an electric current directly throughthe metallic carbide grains during their dissociation, using the resistance of the charge itself for the heating.
  • the carbideutilized for this purpose consists, for example, of grainsv or particles. 7 to 10 millimeters in size which remain discrete, i.e. individually distinct during heating; any agglomeration presentsa risk of preventing the liberation of metallicivapors. 7
  • an important feature of the invention 15 to en sure progressive heating of the carbide charge which,
  • the invention also relates to an apparatus for the commercial manufacture of metals by thermal dissociation of their carbides.
  • This apparatus is illustrated diagrammatically in the annexed drawings, in which Figure 1 is a plan view of a section taken on line I-I of Figure 2;
  • Figure; 2 is a view-in elevation taken on line II-II of Figure 1,, the metal being here condensed to the solid state;-
  • Figure 3 is a view similar to Figure 2'of a modification in which'the metal is condensed to the liquid state.
  • the apparatus has a generally cylindrical form; it is surrounded by a metal jacket, 1.
  • the dissociation zone is; situated at the center; it comprises in its upper part the electrodes 2 symmetrically arranged about the charging tube 7, for the'carbide grains, which is positioned axially in the cylinder and is closed by a plug 6.
  • an empty space S in which the metallic vapors are liberated (disengaged); this space communicates at-itsupper part and at its entire periphery with the condensation zone 10 concentric with the dis sociation zone, from which it is separated by' a heat insulator layer 13.
  • the surfaces 8 and 9 which delimit" the empty space at its upper part, and its peripheral communication with the condensation zone, can be easily scraped from the outside through the openings 11' for the purpose of removing the concreted masses which condense thereon.
  • valve 12 In order to drop a charge of fresh carbide, it is necessary to open valve 12 and to thereupon lower plunger 6, this being accomplished without breaking the vacuum, thetfeed hopper 3v serving asa lock chamber in known manner. Tostop the delivery, the valve 12 is operated first and the plunger 6 is raised afterwards. Hence, normally chargingtube 7 is empty.
  • the circulation of the material from top to bottom in the furnace takes place in a semi-continuous manner as follows: a certain quantity of fresh carbide is dropped from the upper hopper 3. When it is sufiiciently spent, the current is switched off, the lower door 4 is opened-to permit a corresponding quantity of residue to fall into thelarge storage vessels provided in the bottom of the furnace. It will be seen that there is no obstacle opposed to the downward sliding of the residue. If the residue cannot descend by itself, then, it is pushed with the electrodeswhich are movable vertically and, also, by means of the smallplunger 6. Thercupon, the e'lectrodes'are raised above the material, so that part of the more orless spent residueslides under the electrodes, eventually pushed by the small plunger 6.
  • the electrodes are lowered, taking up approximately their initial position, enabling thereby the current to flow again. It will be observed that the pressure exerted bythe electrodes upon the spent residue causesit to be packed.
  • the condensed metal i.e. according to the desirability of condensing it to the liquid or solid state
  • different temperatures are established at the intermediate surfaces 8 and 9 and at the condenser 10.
  • the thickness of: theheatinsulating-walls 13 arid 14 are suitably chosen with that end in view.
  • the outlets 19 connect the condenser with the vacuum pump (not shown).
  • the metal is condensed in the liquid state on the wall 20, which, when necessary, can be cleaned through the openings 21 provided at the top of the furnace.
  • wall 20, as well as the circular vessel 22 which is in contact with liquid aluminum can be made of aluminum nitride; the thickness of the heat insulator 13 between the dissociation and condensation zones is reduced and, in contrast, the thickness of the peripheral heat insulator 14 is increased.
  • the edge-to-edge distance between the electrodes 2 can be greater by about 30% than the distance between these electrodes and the carbon wall 17; experience shows that the amount of current passing through the wall is negligible under these circumstances.
  • a short circuit may occur at for two reasons:
  • the temperature in the electrodes depends on the current density in the electrode, and on the distance from the water-cooled metallic head (not shown) through which the current enters.
  • the use of carbon sleeves can be avoided.
  • the sleeves can be per hour.
  • the examples relate to a three-phase furnace comprising three graphite electrodes 200 mm. in diameter, through which passes a current of 7000 amperes.
  • the edge-to-edge distance between the electrodes ranges between 220 and 300 millimeters; there is thus obtained a potential difference of 30 to 50 volts between electrodes, thereby producing a power of 364 to 607 kilovoltamperes.
  • a distance of 300 millimeters has been adopted.
  • Example I This relates to the production of calcium by the dissociation of CaC in a high vacuum (0.01 mm. mercury), and at a rather high temperature (1500 C. at the surface of the cone of the carbide grains, and 1700 C. at the lower ends of the electrodes).
  • the dew point of calcium at the indicated operating pressure is 600 C., hence, the metal condenses in the solid state upon the sheet 10' ( Figure 2) at the rate of 50 to kilogs.
  • the walls 8 and 9 are at about 1000 C., and the CaO and CaC concretions condense entirely thereon. When the volume of condensed metal amounts to 1000 liters, i.e. 1800 kilogs.
  • the vacuum is broken by introducing an inert gas into the furnace, the annular door 18 is opened (Fig. 2), and the condensed metal is removed.
  • the concretions deposited on surfaces 8 and 9 can then be scraped through the openings 11 and removed through door 18. carbonaceous residues contained in vessel 5 are also removed.
  • the vacuum is reestablished in the furnace and a new operation is started.
  • Example 2 This pertains to the production of manganese by dissociation of manganese carbide Mn C in a vacuum of 0.05 mm. mercury; however, the temperature is about 1200 C. at the surface of the cone of the carbide grains and about 1350 C. in the hottest zone. The dew point of manganese at the adopted pressure is 1050 C. Hence, it condenses in the solid state at the rate of 60 to kilogs. per hour. The surfaces 8 and 9 are at a temperature of about 1000 C.
  • the heat insulating layer at the periphery of the furnace is substantially thicker than in the case of the production of calcium and, in contrast, the thickness of heat insulator between the: dissociation and condensation zones is smaller. The run is continued until the condensate occupies a volume of 500 liters, that is, 3500 kg. manganese.
  • Example 3 Relates to the production of aluminum by dissociation of its carbide Al C at a pressure of 0.5 mm. mercury and a temperature of about 1650" C. at the surface of the cone of thecarbide grains, and l900 C. at the lower end of the electrodes.
  • the aluminum being only slightly volatile, condenses on a rather hot wall (dew point 1400 C.); hence, it is collected in the liquid state (in the apparatus shown in Figure 3) at the rate of 45 to 75 kg. per hour.
  • Suitable inert gases for the purposes of the present invention are argon, helium, krypton, neon, xenon, nitrogen, hydrogen, hydrocarbons, etc.
  • the three latterones may be used with metals which do not form nitrides or hydrides at the operating temperature, or in the cases where the formation of nitride or hydride is not inconvenient.
  • the improvement in said process which comprises the step of: passing an electric current through a charge of metallic carbides in particulate form, whereby the carbides are heated to their dissociation temperatures, said current being supplied by a plurality of vertical, symmetrically disposed electrodes delimiting a polygonal area, while the charge is supplied to the center of said area, and the electrodes have their lower free ends in contact with residue substantially free of carbides and metal.
  • a substantially continuous electrothermic process for producing metals comprising the following steps: supplying by gravity to the upper end of a vertically disposed furnace a charge, in particulate form, of a carbide of the metal to be produced, said charge accumulating on top of a tamped carbonaceous residue formed as described hereafter: passing an inert gas through the furnace to displace the air therefrom; maintaining a pres sure below 1 mm.
  • Apparatus for the electrothermic decomposition of carbides comprising, in combination: a furnace of generally cylindrical shape having disposed in the central portion thereof from the top downwards and in the order named, respectively, a charge supply tube, electrodes surrounding said tube, a dissociation zone, a residue collection zone, outlet means for said residue from said collection zone, and a vapor disengagement space disposed above the dissociation zone and connected at its upper part, and along its entire periphery, with a condensation zone.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US682447A 1956-09-28 1957-09-06 Process and apparatus for the production of metals by dissociation of their carbides Expired - Lifetime US2931719A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3099554A (en) * 1961-02-21 1963-07-30 Union Carbide Corp Process for producing metals
US3208845A (en) * 1962-06-07 1965-09-28 Sueddeutsche Kalkstickstoff Production of calcium metal
US3264097A (en) * 1962-02-28 1966-08-02 Vaw Ver Aluminium Werke Ag Method for producing magnesium
US3649310A (en) * 1968-10-25 1972-03-14 Paul C Yates DENSE, SUBMICRON GRAIN AlN-SiC BODIES
US5173921A (en) * 1991-01-04 1992-12-22 Gaylord E Mervyn J Apparatus and process for activation of carbon by electrical resistance heating in the presence of steam

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US984503A (en) * 1909-08-18 1911-02-14 Gen Electric Producing calcium.
US996474A (en) * 1908-02-07 1911-06-27 Gen Electric Fractional distillation of metals.
US1576883A (en) * 1923-03-02 1926-03-16 Victor M Weaver Process of making graphite
US2122419A (en) * 1936-08-11 1938-07-05 Dow Chemical Co Manufacture of calcium metal
US2213170A (en) * 1939-08-03 1940-08-27 Dow Chemical Co Method of producing metals, such as calcium and magnesium
US2219059A (en) * 1937-12-04 1940-10-22 Magnesium Dev Corp Process for the production of metallic magnesium
GB550732A (en) * 1940-09-23 1943-01-21 Samuel Ralph Keemle Improvements in and relating to electrothermic reduction of volatile metals
US2400000A (en) * 1941-08-02 1946-05-07 Gardner Thermal Corp Production of aluminum
US2550684A (en) * 1948-03-01 1951-05-01 Fouquet Robert Apparatus for production of volatilizable metals
US2582120A (en) * 1946-09-24 1952-01-08 North Carolina Magnesium Dev C Production of magnesium
US2724644A (en) * 1953-09-03 1955-11-22 Astral Soc Method for condensing metal vapors directly to their liquid state
US2769705A (en) * 1951-01-15 1956-11-06 Elektrokemisk As Process of charging fine materials

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US996474A (en) * 1908-02-07 1911-06-27 Gen Electric Fractional distillation of metals.
US984503A (en) * 1909-08-18 1911-02-14 Gen Electric Producing calcium.
US1576883A (en) * 1923-03-02 1926-03-16 Victor M Weaver Process of making graphite
US2122419A (en) * 1936-08-11 1938-07-05 Dow Chemical Co Manufacture of calcium metal
US2219059A (en) * 1937-12-04 1940-10-22 Magnesium Dev Corp Process for the production of metallic magnesium
US2213170A (en) * 1939-08-03 1940-08-27 Dow Chemical Co Method of producing metals, such as calcium and magnesium
GB550732A (en) * 1940-09-23 1943-01-21 Samuel Ralph Keemle Improvements in and relating to electrothermic reduction of volatile metals
US2400000A (en) * 1941-08-02 1946-05-07 Gardner Thermal Corp Production of aluminum
US2582120A (en) * 1946-09-24 1952-01-08 North Carolina Magnesium Dev C Production of magnesium
US2550684A (en) * 1948-03-01 1951-05-01 Fouquet Robert Apparatus for production of volatilizable metals
US2769705A (en) * 1951-01-15 1956-11-06 Elektrokemisk As Process of charging fine materials
US2724644A (en) * 1953-09-03 1955-11-22 Astral Soc Method for condensing metal vapors directly to their liquid state

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3099554A (en) * 1961-02-21 1963-07-30 Union Carbide Corp Process for producing metals
US3264097A (en) * 1962-02-28 1966-08-02 Vaw Ver Aluminium Werke Ag Method for producing magnesium
US3208845A (en) * 1962-06-07 1965-09-28 Sueddeutsche Kalkstickstoff Production of calcium metal
US3649310A (en) * 1968-10-25 1972-03-14 Paul C Yates DENSE, SUBMICRON GRAIN AlN-SiC BODIES
US5173921A (en) * 1991-01-04 1992-12-22 Gaylord E Mervyn J Apparatus and process for activation of carbon by electrical resistance heating in the presence of steam

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DE1120705B (de) 1961-12-28

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