US20200063279A1 - Anode apparatus and methods regarding the same - Google Patents

Anode apparatus and methods regarding the same Download PDF

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Publication number
US20200063279A1
US20200063279A1 US16/334,134 US201716334134A US2020063279A1 US 20200063279 A1 US20200063279 A1 US 20200063279A1 US 201716334134 A US201716334134 A US 201716334134A US 2020063279 A1 US2020063279 A1 US 2020063279A1
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Prior art keywords
anode
sealing material
anode body
pin
hole
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US16/334,134
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English (en)
Inventor
Lance SWORTS
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Elysis LP
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Elysis LP
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Publication of US20200063279A1 publication Critical patent/US20200063279A1/en
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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
    • C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
    • C25C3/12—Anodes
    • 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
    • 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
    • C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • 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
    • C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
    • 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
    • C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • C25C3/16—Electric current supply devices, e.g. bus bars
    • 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
    • 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

  • An inert anode is electrically connected to the electrolytic cell, such that a conductor rod is connected to the inert anode in order to supply current from a current supply to the inert anode, where the inert anode directs current into the electrolytic bath to produce non-ferrous metal (where current exits the cell via a cathode).
  • corrosive bath and/or vapor interacts with the anode assembly and can impact the effectiveness and longevity of the anode assembly (e.g. by weakening the mechanical connection, and/or increasing resistivity at the electrical connection).
  • the instant disclosure is directed towards an inert anode apparatus. More specifically, the instant disclosure is directed towards an inert anode apparatus configured to reduce, prevent, and/or eliminate corrosion of the pin and/or anode material (e.g. by corrosive vapors and/or molten electrolyte) in an electrolysis cell.
  • an inert anode apparatus configured to reduce, prevent, and/or eliminate corrosion of the pin and/or anode material (e.g. by corrosive vapors and/or molten electrolyte) in an electrolysis cell.
  • one or more embodiments of the anode-pin-protective sealing material connection in the instant disclosure provide enhanced corrosion resistance to the anode assembly when measured in at least one of the following locations: (a) at the pin, inside the hole in the anode body; (b) at the anode body, along the inner diameter of the hole for the anode pin; and/or (c) in the vapor zone where the pin extends above the anode body (i.e., above the bath, and/or in the refractory package).
  • the sealing material when utilized in the anode assembly, it provides protection to (1) mechanical attachment site of the anode to pin and/or (2) the anode assembly components (e.g. pin, anode body, filler material, cement material) as the sealing material is configured to accept reactive fluoride species that are present in situ in the bath and/or bath vapor.
  • the sealing material is transformed (at least partially) from a solid to a liquid material.
  • a sealing material is configured to extend between the inner surface of the hole in the anode body and the outer diameter of the pin.
  • an anode assembly comprising: an anode support; and an anode apparatus mechanically attached to the anode support, wherein the anode apparatus comprises: (a) an anode body comprising at least one outer sidewall, wherein the outer sidewall is configured to define a shape of the anode body, and to perimetrically surround a hole in the anode body, wherein the hole comprises an upper opening in a top surface of the anode body and wherein the hole axially extends into the anode body; (b) a pin comprising: a first end connected to a current supply, and a second end opposite the first end, wherein the second end extends downward into the upper end of the anode body and into the hole of the anode body; and (c) a sealing material comprising an aggregate and a matrix, wherein the sealing material is configured to cover at least a portion of at least one of the following: (1) an inner sidewall of the anode body; (2) the top surface of
  • the sealing material comprises at least one of: water, polymers, organics, dispersants, or diluents.
  • a sealing material is configured to cover at least a portion of at least one of the following: (1) an inner sidewall of the anode body; (2) the pin; and (3) a filler material.
  • the first end of the pin is configured to be retained within an anode support.
  • the filler is retained in the hole between the inner sidewall of the anode body and the pin.
  • the sealing material is configured to enclose the conductive filler into the anode body between the inner sidewall of the anode body and the pin.
  • the sealing material is cast in place.
  • the sealing material is pre-cast and screwed into the anode body.
  • the sealing material is sintered into place during the sintering of the green form anode body into the final anode body.
  • the sealing material is retained above the top surface of the anode body.
  • the sealing material is retained in the hole.
  • above the top surface of the anode body includes extending along the pin.
  • above the top surface of the anode body includes extending along the pin and into the anode support.
  • above the top surface includes extending across the top surface of the upper portion of the anode body.
  • above the top surface includes extending across the top surface and extending down around the outer sidewall of the anode body.
  • the sealing material is applied to the anode hole between the pin and the inner surface of the anode body in a gradient, such that the concentration of sealing material varies in a radial direction.
  • the gradient is configured such that the concentration of sealing material is higher adjacent to the pin as compared to adjacent to the inner surface of the anode body.
  • the gradient is configured such that the concentration of sealing material is lower adjacent to the pin as compared to adjacent to the inner surface of the anode body.
  • the sealing material is applied to the anode hole between the pin and the inner surface of the anode body in a gradient, such that the concentration of sealing material varies in a lateral direction.
  • the gradient is configured such that the concentration of sealing material is higher adjacent to the upper end as compared to adjacent to the lower end of the anode body.
  • the gradient is configured such that the concentration of sealing material is lower adjacent to the upper end as compared to adjacent to the lower end of the anode body.
  • the sealing material is configured with a higher concentration at a position adjacent to the bath-vapor interface, as compared to either the upper end in the vapor phase or the lower end in the bath of the anode body.
  • the concentration of sealing material from a position just below the bath-vapor interface to a position adjacent to the upper end of the anode is higher than the portion of sealing material in the submerged portion of the anode body.
  • an electrolysis cell comprising: a cell structure comprising a cell bottom and a cell sidewall, wherein the cell sidewall is configured to perimetrically surround the cell bottom and extend in an upward direction from the cell bottom to define a control volume, wherein the control volume is configured to retain a molten electrolyte bath; and an anode assembly configured to direct current into the molten electrolyte bath, wherein the anode assembly comprises: an anode support; and an anode apparatus mechanically attached to the anode support, wherein the anode apparatus comprises: (a) an anode body comprising at least one outer sidewall, wherein the outer sidewall is configured to define the anode shape and to perimetrically surround a hole in the anode body, wherein the hole comprises an upper opening in the top of the anode body and wherein the hole axially extends into the anode body; and (b) an pin comprising: a first end connected to a current supply, and a second
  • FIG. 1 depicts a block diagram of a generic anode assembly in accordance an embodiment of the instant disclosure.
  • FIG. 2 depicts a schematic cut-away side view of an anode apparatus in accordance with an embodiment of the instant disclosure.
  • FIG. 3 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 4 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 5 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 6 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 7 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 8 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 9 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 10 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 11 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 12 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 13 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 14 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 15 depicts a cut-away side view of an embodiment of an anode apparatus of the instant disclosure.
  • FIG. 1 depicts a block diagram of a generic anode assembly 10 in accordance an embodiment of the instant disclosure.
  • the anode assembly 10 comprises an anode support and an anode apparatus.
  • the anode apparatus is mechanically attached to the anode support (e.g. refractory package, structural support member, combination thereof).
  • the anode apparatus comprises: an anode body, a pin, and a sealing material.
  • the anode assembly is a part of an electrolysis cell comprising a cell structure comprising a cell bottom and a cell sidewall.
  • the cell sidewall is configured to perimetrically surround the cell bottom and extend in an upward direction from the cell bottom to define a control volume.
  • the control volume is configured to retain a molten electrolyte bath.
  • the anode body comprises at least one outer sidewall.
  • the outer sidewall is configured to define a shape of the anode body and to perimetrically surround a hole in the anode body.
  • the hole comprises an upper opening in a top surface of the anode body and the hole axially extends into the anode body.
  • the pin comprises a first end and a second end.
  • the first end is connected to a current supply.
  • the second end is opposite the first end.
  • the second end extends downward into the upper end of the anode body and into the hole of the anode body.
  • the sealing material is configured to cover at least a portion of at least one of the following: an inner sidewall of the anode body; the top surface of the anode body; the pin; and the anode support. In some embodiments, the sealing material is configured to cover at least a portion of at least one of the following: an inner sidewall of the anode body; the pin; and a filler material.
  • the sealing material is configured to reduce, prevent, or eliminate corrosive constituents of the electrolysis process from contacting (and corroding) (1) the pin and/or (2) the mechanical attachment site of the anode body to the pin.
  • the sealing material is configured to be tailored (i.e. matched) to the composition of the anode body.
  • the sealing material is configured such that aggregate present in the sealing material is compositionally consistent with the anode body composition.
  • the sealing material is configured to substantially overlap with the coefficient of thermal expansion of the anode body.
  • the sealing material is inserted into the anode body (between the inside of the anode body and the pin) as a particulate material. In some embodiments, the sealing material is inserted into the anode body (between the inside of the anode body and the pin) as a liquid/slurry applied to the anode body or pin. In some embodiments, when the sealing material is inserted into/added onto the anode body, it undergoes a chemical and/or thermal cure in order to form a solid sealing material. In some embodiments, the sealing material is positioned between the pin and the anode body.
  • a sealing material is utilized around the upper end of the anode body, surrounding the outer surface of the pin and contacting the anode body (e.g. inner portion of the hole in the anode body, top surface of the anode body, upper portion of the anode body, and/or combinations thereof).
  • the sealing material comprises a cement.
  • the sealing material comprises a grout.
  • the sealing material is configured to prevent corrosive vapors from entering into the inner surface of the anode body, proximal to the portion of the pin that is retained within the anode body.
  • cement includes aggregate and a binder or matrix.
  • the aggregate is replaced with a sealing material in accordance with the instant disclosure (e.g. utilizing the commercially available binder and/or matrix).
  • the matrix or binder is replaced with a sealing material in accordance with the instant disclosure (e.g. utilizing the commercially available aggregate).
  • the matrix or binder and aggregate is replaced with a sealing material in accordance with the instant disclosure.
  • Some non-limiting commercial examples of binders, matrices, aggregates, and/or combinations thereof include: Al 2 O 3 , SiO 2 , MgO, CaO, or the like.
  • the sealing material includes at least one of: water, polymers, organics, dispersants, and/or diluents in order to promote a flowable sealing material such that the sealing material is formable/flowable into its desired location (e.g. in the anode assembly and/or anode body).
  • the sealing material is configured to enclose the conductive filler into the anode body (i.e. between the inner sidewall of the anode body and the pin). In some embodiments, the sealing material is configured to provide a mechanical attachment of the anode body to the pin. In some embodiments, the sealing material is configured to provide structural support to the anode assembly and/or anode apparatus.
  • the sealing material is cast in place.
  • an accelerant is utilized in combination with the sealing material in order to reduce the curing time.
  • the sealing material is pre-cast and screwed into the anode body (e.g. upper portion of the anode body).
  • the sealing material is sintered into place while/during the sintering of the green form anode body into the final anode body/anode assembly (anode body, pin, and sealing material).
  • the sealing material is retained above the hole, proximal to the top surface of the upper end of the anode.
  • sealing material is retained in the hole (i.e. extending between the pin and the inner sidewall of the anode body) and above the top surface of the anode body.
  • above the top surface of the anode body includes extending along the pin (i.e. portion of the pin that extends out of the anode body). In some embodiments, above the top surface of the anode body includes extending along the pin and into the anode support (i.e. portion of the pin that extends into the anode support, where the pin is mechanically attached). In some embodiments, above the top surface includes extending across the top surface of the upper portion of the anode body. In some embodiments, above the top surface includes extending across the top surface and extending down around the outer sidewall of the anode body (i.e. creating a collar around the upper end of the anode surface).
  • anode means the positive electrode (or terminal) by which current enters an electrolytic cell.
  • the anodes i.e. anode bodies
  • the anode comprises an inert anode (e.g. non-reactive, dimensionally stable, and/or having a dissolution rate (e.g. at the cell operating parameters) less than that of a corresponding carbon anode).
  • anode body means: the physical structure of the anode (e.g. including the top, bottom, and sidewall(s)).
  • anode materials include: metals, metal alloys, metal oxides, ceramics, cermets, and combinations thereof.
  • the anode body is oval, cylindrical, rectangular, square, plate-shaped (generally planar), other geometrical shapes (e.g. triangular, pentagonal, hexagonal, and the like
  • anode apparatus means the anode or positive electrode in the electrolysis cell.
  • the anode apparatus includes: the anode body and anode pin.
  • the anode apparatus includes the anode body, anode pin, and filler/sealing materials (e.g. individually, or in combination: conductive filler and/or sealing material).
  • anode assembly means at least one anode apparatus (anode body, pin, conductive filler, and/or sealing material) and an anode support, where the at least one anode apparatus is connected (e.g. mechanically and/or electrically) to the anode support.
  • support means a member that maintains another object(s) in place.
  • the support is the structure that retains the anode(s) in place.
  • the support facilitates the electrical connection of the electrical bus work to the anode(s).
  • the support is constructed of a material that is resistant to attack from the corrosive bath.
  • the support is constructed of insulating material, including, for example refractory material.
  • multiple anodes are connected (e.g. mechanically and electrically) to the support (e.g. removably attached), which is adjustable and can be raised, lowered, or otherwise moved in the cell.
  • the anode support includes a refractory material (e.g. block or assembly), other bath resistant materials, rail or beam support members, vertical adjustment components and apparatuses, and/or electrical bus work.
  • electrical bus work refers to the electrical connectors of one or more component.
  • the anode, cathode, and/or other cell components can have electrical bus work to connect the components together.
  • the electrical bus work includes pin connectors in the anodes, the wiring to connect the anodes and/or cathodes, electrical circuits for (or between) various cell components, and combinations thereof.
  • sidewall means: a surface that forms the wall of an object.
  • perimetrically surrounding means: surrounding the outside edge of a surface.
  • perimetrically surrounding includes different geometries (e.g. concentrically surrounding, circumscribing) and the like.
  • electrolytic bath refers to a liquefied bath having at least one species of metal to be reduced (e.g. via an electrolysis process).
  • a non-limiting example of the electrolytic bath composition includes: NaF—AlF 3 , NaF, AlF 3 , CaF 2 , MgF 2 , LiF, KF, and combinations thereof—with dissolved alumina.
  • molten means in a flowable form (e.g. liquid) through the application of heat.
  • the electrolytic bath is in molten form (e.g. at least about 750° C.).
  • the metal product that forms at the bottom of the cell e.g. sometimes called a “metal pad” is in molten form.
  • the molten electrolyte bath/cell operating temperature is: at least about 750° C.; at least about 800° C.; at least about 850° C.; at least about 900° C.; at least about 950° C.; or at least about 975° C. In some embodiments, the molten electrolyte bath/cell operating temperature is: not greater than about 750° C.; not greater than about 800° C.; not greater than about 850° C.; not greater than about 900° C.; not greater than about 950° C.; or not greater than about 975° C.
  • vapor means: a substance that is in the form of a gas.
  • vapor comprises ambient gas mixed with caustic and/or corrosive exhaust from the electrolysis process.
  • vapor space refers to the head space in an electrolysis cell, above the surface of the electrolyte bath.
  • interface refers to a surface regarded as the common boundary of two bodies, spaces, or phases.
  • bath-vapor interface refers to the surface of bath, which is the boundary of two phases, the vapor space and the liquid (molten) electrolyte bath.
  • metal product means the product which is produced by electrolysis. In one embodiment, the metal product forms at the bottom of an electrolysis cell as a metal pad. Some non-limiting examples of metal products include: aluminum, nickel, magnesium, copper, zinc, and rare earth metals.
  • hole means: an opening into something.
  • pin means: a piece of material used to attach things together.
  • the pin is an electrically conductive material.
  • the pin is configured to electrically connect the anode body to the electrical buswork in order to provide current to an electrolysis cell (via the anode).
  • a first end of the pin is configured to fit into/be retained within an anode support (e.g. anode support and at least one anode apparatus is an anode assembly)
  • the pin is configured to overlap with the anode body.
  • the pin is configured to structurally support the anode body, as it is attached to and suspended from the pin.
  • the pin is stainless steel, nickel, nickel alloy, Inconel, or a corrosion protected steel.
  • the pin is configured to extend into the anode body (e.g. into a hole) to a certain depth, in order to provide mechanical support and electrical communication to the anode body.
  • the length of the pin is sufficient (long enough) to provide mechanical support to the anode body and sufficient to (short enough) to prevent corrosion on the pin inside the hole (i.e. locate the pin above the bath-vapor interface)
  • the pin is oval, cylindrical, rectangular, square, plate-shaped (generally planar), other geometrical shapes (e.g. triangular, pentagonal, hexagonal, and the like).
  • the pin is attached to the anode body.
  • the pin is mechanically attached to the anode body by: fastener(s), screw(s), a threaded configuration (e.g. on pin), a mating threaded configuration (e.g. on inner surface of hole in anode body and on pin), or the like.
  • the pin is attached to the anode body via welding (e.g. resistance welding or other types of welding).
  • the pin is attached to the anode body via a direct sinter (i.e. sintering the anode body onto the pin directly).
  • electrically conductive material means: a material that has an ability to move electricity (or heat) from one place to another.
  • filler means: a material that fills a space or void between two other objects.
  • the filler is configured to connect (e.g., electrically connect) the anode body to the pin.
  • non-limiting examples of filler include: a particulate material, a liquid/slurry material, and combinations thereof.
  • the filler is incorporated/inserted into the desired location in a flowable form, which then hardens over time to yield a solid filler material.
  • the filler is a conductive material, also referred to as conductive filler.
  • the filler is configured to electrically connect the pin to the anode body.
  • electrically conductive filler materials include: iron oxides (hematite, magnetite, wustite), copper, copper alloys, nickel, nickel alloys, precious metals, (e.g., Pt, Pd, Ag, Au) and combinations thereof.
  • sealing material means: a substance used to close or secure an object or component (e.g. in order to reduce, prevent, and/or eliminate the transmittal of vapor or liquid to the object or component).
  • the filler is configured to seal the upper portion hole in the anode body from corrosive vapors present in the vapor space.
  • Non-limiting examples of a sealing material include: castable cement, concrete, grout, mortar, and combinations thereof.
  • the sealing material is a substance/material that includes at least two components: (1) aggregate and (2) matrix cement (e.g., grout), where the aggregate includes large and/or fine aggregate sizes.
  • the sealing material is applied to an area in order to act as an adhesive, as it is configured to adhere components together upon hardening.
  • castable means: a substance/material that includes at least two components: aggregate and cement, where the aggregate includes large and fine aggregate sizes.
  • the castable is applied to an area such in order to act as an adhesive, as it is configured to adhere components together upon hardening.
  • grout means: a castable with matrix and finer aggregate (as compared to concrete or cement).
  • the grout includes a viscosity configured to fill cracks and crevices in the anode assembly and/or anode apparatus.
  • the grout is configured as a bonding material that hardens in place and is used to bind things together.
  • particulate material means: a material composed of particles.
  • the particulate material is electrically conductive.
  • the particulate material is copper shot.
  • Other non-limiting examples of particulate materials include: precious metals (e.g. platinum, palladium, gold, silver, and combinations thereof).
  • the particulate material includes: metal foam (e.g. Cu foam), large or small shot (e.g., configured to fit between the pin and the anode body and/or in the anode hole), paint, and/or powder.
  • particulate materials are utilizable, provided they fill the void between the pin and the anode body (or portion below the pin, in the hole of the anode body) and promote an electrical connection between the anode body and the pin to provide current to the anode.
  • the sealing material is configured to reduce, prevent, or eliminate corrosion from the anode apparatus (e.g. pin, anode body, conductive filler, and/or combinations thereof).
  • anode apparatus e.g. pin, anode body, conductive filler, and/or combinations thereof.
  • the sealing material includes aggregate that is configured as an anode-matched aggregate. In some embodiments, the sealing material is configured as an off-gas compatible aggregate (e.g., configured to react but not substantially degrade the effectiveness of the sealing material.
  • anode-matched aggregate means aggregate that has an overlapping performance characteristics as the anode composition.
  • anode matched aggregate is aggregate having the same compositional constituent as the anode body (e.g. hematite, magnetite).
  • anode matched aggregate is aggregate having a composition that is consistent with at least one major species (or compound) present in the anode (e.g. >30 wt. %).
  • anode matched aggregate is aggregate having a compound or component of an off-gas compatible aggregate (e.g. NiFe 2 O 4 , NiO, CuAl 2 O 4 , CuO).
  • Some non-limiting examples of aggregating sealing materials include: spinels, magnetite, hematite, copper aluminate, nickel ferrite, or tin oxide, and combinations thereof.
  • the sealing material comprises a castable ceramic or cermet plug, where the aggregates (or at least a portion thereof) are replaced with an anode-matched aggregate and/or an off-gas compatible aggregate as the primary seal.
  • the sealing material comprises a castable ceramic or cermet containing Al 2 O 3 , SiO 2 , MgO, CaO, Na 2 O, and combinations thereof, where at least some of the silicates and/or aluminates are replaced with an aggregate specifically tailored/matched to the anode body and/or pin material, in accordance with the instant disclosure.
  • the aggregate is about 40 wt. % of the sealing material (e.g. as cured). In some embodiments, the matrix/binder is about 60 wt. % of the sealing material (e.g. as cured). In some embodiments, the aggregate is from about 5 wt. % to 100 wt. % of the sealing material. In some embodiments, the binder/matrix is from about 5 wt. % to 100 wt. % of the sealing material.
  • the percentage and/or quantity of aggregate or binder/matrix is quantified via SEM (scanning electron microscope) or EDS (energy dispersive spectroscopy), via viewing/observing a polished cross-section of sealing material.
  • EDS is configured to provide the chemical make-up of the cross-section.
  • the filler is conductive filler (e.g. configured to promote electrical communication between the pin and the anode body).
  • the filler is configured to extend between the inner sidewall of the anode body and the pin (e.g. beneath the sealing material).
  • the sealing material comprises a thickness of: from 1 mm to not greater than 50 mm.
  • the sealing material has a thickness of: at least 1 mm; at least 2 mm; at least 3 mm; at least 4 mm; at least 5 mm; at least 6 mm; at least 7 mm; at least 8 mm; at least 9 mm; or at least 10 mm.
  • the sealing material has a thickness of: at least about 5 mm; at least about 10 mm; at least about 15 mm; at least about 20 mm; at least about 25 mm; at least about 30 mm; at least about 35 mm; at least about 40 mm; at least about 45 mm; or at least about 50 mm.
  • the sealing material has a thickness of: not greater than 1 mm; not greater than 2 mm; not greater than 3 mm; not greater than 4 mm; not greater than 5 mm; not greater than 6 mm; not greater than 7 mm; not greater than 8 mm; not greater than 9 mm; or not greater than 10 mm.
  • the sealing material has a thickness of: not greater than about 5 mm; not greater than about 10 mm; not greater than about 15 mm; not greater than about 20 mm; not greater than about 25 mm; not greater than about 30 mm; not greater than about 35 mm; not greater than about 40 mm; not greater than about 45 mm; or not greater than about 50 mm.
  • the sealing material has a thickness of: at least about 50 mm; at least about 100 mm; at least about 150 mm; at least about 200 mm; or at least about 250 mm. In some embodiments, the sealing material has a thickness of: not greater than about 50 mm; not greater than about 100 mm; not greater than about 150 mm; not greater than about 200 mm; or not greater than about 250 mm.
  • the sealing material is configured as a coating applied to the anode pin. In some embodiments, the sealing material is configured as a coating to the inner surface of the anode body. In some embodiments, the sealing material is configured as a coating applied to the upper surface (e.g. top end) of the anode body.
  • the sealing material is applied to one or more components of the anode apparatus and/or anode assembly via washing (e.g., painting) the component directly with the material.
  • the sealing material is applied to one or more components of the anode apparatus and/or anode assembly via applying the sealing material to the component(s) as a slurry/suspension in combination with a binder or liquid.
  • the sealing material is applied to one or more of the anode apparatus and the pin via applying/directing the aggregate into the desired located (e.g. pouring powder, particulate, or pellets), followed by adding the matrix, mechanically agitating/combining, and allowing the sealing material to set/dry.
  • the desired located e.g. pouring powder, particulate, or pellets
  • the sealing material is applied to one or more of the anode apparatus and the pin via spraying.
  • the sealing material is applied to one or more of the anode apparatus and the pin via gunning.
  • the sealing material is applied to one or more of the anode apparatus and the pin via slip casting. In some embodiments, the sealing material is applied to one or more of the anode apparatus and the pin via pressure casting. In some embodiments, the sealing material is applied to one or more of the anode apparatus and the pin via vacuum casting. In some embodiments, the sealing material is applied to one or more of the anode apparatus and the pin via slurry pressing. In some embodiments, the sealing material is applied to one or more of the anode apparatus and the pin via gel casting. In some embodiments, the sealing material is applied to one or more of the anode apparatus and the pin via electrophoretic casting.
  • the anode matched aggregate and/or off-gas compatible aggregate is present in mixed form with the sealing material, where the aggregate is from at least 1 vol. % sealing material to not greater than 99.5 vol. % sealing material.
  • the aggregate is present in mixed form with the sealing material, where the aggregate is from at least 1 vol. % sealing material to not greater than 100 vol. % sealing material.
  • the aggregate comprises: at least 1 vol. %; at least 5 vol. %; at least 10 vol. %; at least 15 vol. %; at least 20 vol. %; at least 25 vol. %; at least 30 vol. %; at least about 35 vol. %; at least 40 vol. %; at least 45 vol. %; at least 50 vol. %; at least 55 vol. %; at least 60 vol. %; at least 65 vol. %; at least 70 vol. %; at least 75 vol. %; at least 80 vol. %; at least 85 vol. %; at least 90 vol. %; or at least 95 vol. %; or at least 99 vol. % of the sealing material.
  • the aggregate comprises: not greater than 1 vol. %; not greater than 5 vol. %; not greater than 10 vol. %; not greater than 15 vol. %; not greater than 20 vol. %; not greater than 25 vol. %; not greater than 30 vol. %; not greater than about 35 vol. %; not greater than 40 vol. %; not greater than 45 vol. %; not greater than 50 vol. %; not greater than 55 vol. %; not greater than 60 vol. %; not greater than 65 vol. %; not greater than 70 vol. %; not greater than 75 vol. %; not greater than 80 vol. %; not greater than 85 vol. %; not greater than 90 vol. %; or not greater than 95 vol. %; or not greater than 99 vol. % of the sealing material.
  • a mixture of anode matched aggregate and/or off-gas compatible aggregate and sealing material includes an amount of aggregate which is sufficient to maintain the ability of the sealing material to adhere components of the anode apparatus (e.g., anode body to pin) and/or anode assembly together (e.g., pin to anode support).
  • the sealing material is applied to the anode hole (i.e. between the pin and the inner surface of the anode body) in a gradient, such that the concentration of sealing material (with anode-matched aggregate and/or off-gas compatible aggregate) varies in a radial direction (i.e. differs from a position adjacent to the pin vs. a position adjacent to the anode sidewall).
  • the gradient is configured such that the concentration of sealing material is (with anode-matched aggregate and/or off-gas compatible aggregate) higher adjacent to the pin as compared to adjacent to the inner surface of the anode body.
  • the gradient is configured such that the concentration of sealing material (with anode-matched aggregate and/or off-gas compatible aggregate) is lower adjacent to the pin as compared to adjacent to the inner surface of the anode body.
  • the sealing material is applied to the anode hole (i.e. between the pin and the inner surface of the anode body) in a gradient, such that the concentration of sealing material varies in a lateral direction (i.e. differs from a position adjacent to the opening of the hole/upper surface of the anode body as compared to a position adjacent to the lower end of the anode body).
  • the gradient is configured such that the concentration of sealing material is higher adjacent to the upper end as compared to adjacent to the lower end of the anode body.
  • the gradient is configured such that the concentration of sealing material is lower adjacent to the upper end as compared to adjacent to the lower end of the anode body.
  • the sealing material is configured with a higher concentration at a position adjacent to the bath-vapor interface, as compared to either the upper end (in the vapor phase) or lower end (in the bath) of the anode body.
  • the concentration of sealing material from a position just below the bath-vapor interface to a position adjacent to the upper end of the anode is higher than the portion of (anode-matched aggregate and/or off-gas compatible aggregate in the) sealing material in the submerged portion of the anode body (e.g. submerged below the bath-vapor interface).
  • FIGS. 2-15 depict schematic cut-away side view of an exemplary anode apparatus in accordance with some embodiments of the instant disclosure.
  • FIG. 2 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 and an entire top surface of the anode body 30 .
  • FIG. 3 depicts an anode apparatus wherein the sealing material 50 covers an entirety of the pin 12 in vapor space 24 , the opening 32 and a portion of the top surface of the anode body 30 .
  • FIG. 4 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 , and a portion of the top surface of the anode body 30 .
  • FIG. 2 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 , and a portion of the top surface of the anode body 30 .
  • FIG. 5 depicts an anode apparatus wherein the sealing material 50 covers an entirety of the pin 12 above the top surface of the anode body 30 (i.e. within the vapor space 24 and refractory portion 18 ), the opening 32 , and a portion of the top surface of the anode body 30 .
  • FIG. 6 depicts an anode apparatus wherein the sealing material 50 covers an entirety of the pin 12 in vapor space 24 , the opening 32 and an entire top surface of the anode body 30 .
  • the sealing material 50 extends beyond a peripheral edge of the top surface of the anode body and covers a portion of the sidewall 40 of the anode body 30 .
  • FIG. 7 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 , and an entire top surface of the anode body 30 .
  • the sealing material 50 extends beyond a peripheral edge of the top surface of the anode body and covers a portion of the sidewall 40 of the anode body 30 .
  • FIG. 8 depicts an anode apparatus wherein the sealing material 50 covers an entirety of the pin 12 in vapor space 24 .
  • the sealing material 50 covers opening 32 and an entire top surface of the anode body 30 .
  • the sealing material 50 extends beyond a peripheral edge of the top surface of the anode body and covers a portion of the sidewall 40 of the anode body 30 .
  • Sealing material 50 is also disposed between the vapor space 24 and the refractory 18 to prevent corrosive chemicals from corroding exposed portions of the pin 12 (i.e. not covered by sealing material 50 ).
  • FIG. 9 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 , and an entire top surface of the anode body 30 .
  • the sealing material 50 extends beyond a peripheral edge of the top surface of the anode body and covers a portion of the sidewall 40 of the anode body 30 .
  • a portion of the pin 12 in the vapor phase 24 is not covered by sealing material 50 .
  • Sealing material 50 is also disposed between the vapor space 24 and the refractory 18 to prevent corrosive chemicals from corroding exposed portions of the pin 12 in the refractory 18 .
  • FIG. 10 depicts an anode apparatus wherein the sealing material 50 covers an entirety of the pin 12 in vapor space 24 .
  • the sealing material 50 covers opening 32 and an entire top surface of the anode body 30 .
  • the sealing material 50 does not extend beyond a peripheral edge of the top surface of the anode body to cover a portion of the sidewall 40 of the anode body 30 .
  • Sealing material 50 is also disposed between the vapor space 24 and the refractory 18 to prevent corrosive chemicals from corroding exposed portions of the pin 12 (i.e. not covered by sealing material 50 ).
  • FIG. 11 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 , and an entire top surface of the anode body 30 .
  • the sealing material 50 extends beyond a peripheral edge of the top surface of the anode body and covers a portion of the sidewall 40 of the anode body 30 .
  • the sealing material extends down the sidewall 40 of the anode body 30 proximate to the interface 22 .
  • FIG. 12 depicts an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 and an entire top surface of the anode body 30 .
  • FIG. 13 depict an anode apparatus wherein the sealing material 50 covers a portion of the pin 12 in vapor space 24 , the opening 32 and an entire top surface of the anode body 30 .
  • the sealing material is also disposed within the hole 34 to cover a portion of the pin 12 within the anode body 30 .
  • the sealing material 50 covers a portion of the pin 12 within the anode body 30 that is above the interface 22 .
  • FIG. 14 depicts an anode apparatus wherein the sealing material 50 is disposed within the hole 34 to cover a portion of the pin 12 within the anode body 30 .
  • the sealing material 50 covers a portion of the pin 12 within the anode body 30 that is above the interface 22 .
  • FIG. 15 depicts an anode apparatus wherein the sealing material 50 is disposed within the hole 34 to cover a portion of the pin 12 within the anode body 30 .
  • the sealing material 50 covers a portion of the pin 12 within the anode body 30 that is above the interface 22 .
  • a filler material is disposed within the hole 34 below the sealing material 50 .
  • Non-limiting examples of producing the anode body include: press sintering, fuse casting, and casting, which is disclosed in corresponding U.S. Pat. No. 7,235,161, which contents are incorporated by reference herein by their entirety.
  • the pin and filler materials are incorporated into the anode body.
  • a filler e.g. conductive filler
  • the pin is placed in the hole of the anode body and filler (e.g. in the form of particulate material) is inserted into the void between the pin and the inner surface of the hole in the anode body.
  • the sealing material i.e., in order to provide a mechanical attachment and/or seal the pin and/or filler material into the hole in the anode body
  • the sealing material is configured to extend at least partially into the hole in the anode body.
  • the sealing material is configured to sit on top of the anode body, proximal to the upper end of the hole, and surrounding the pin as it extends upward from the anode body. In some embodiments, the sealing material is placed on top of the anode body in a position surrounding the pin.
  • the sealing material is configured to extend a portion of the way into the hole at the upper end of the anode. In some embodiments, the sealing material is configured to cover the top portion of the anode body. In some embodiments, the sealing material is configured to contact at least a portion of the outer perimetrical sidewall of the anode body. In some embodiments, the sealing material is configured to contact the pin, the inner portion of the anode body (hole), the upper portion/top surface of the anode body, and the upper portion of at least a portion of the outside perimetrical wall of the anode body.
  • the sealing material is in accordance with the disclosure of U.S. Pat. No. 7,169,270.
  • the sealing material has 5 wt. % to 100 wt. % the sealing material is a castable ceramic or cermet containing Al 2 O 3 , SiO 2 , MgO, CaO, Na 2 O, and combinations thereof, where at least some of the silicate and/or aluminate aggregates in the sealing material (e.g. castable ceramic) are replaced with a magnetite aggregate (e.g. anode-matched/anode compatible aggregate), configured with comparable sizing as the aggregate appropriate sizing as the aggregate in the prior art run.
  • a magnetite aggregate e.g. anode-matched/anode compatible aggregate
  • Both anode assemblies are configured as the embodiment shown in FIG. 2 . Both anode assemblies were incorporated into an aluminum electrolysis cell and operated as electrodes (anodes) extending across the bath-vapor interface for a sufficient length of time in order to evaluate whether any reactions occur as a result of the interaction of the reactive species present in the vapor space of the cell with the sealing material and/or components thereof.
  • Anode assemblies are pulled out of the cell and evaluated in order to evaluate and/or quantify corrosion on the various anode apparatus components (e.g. sealing material).
  • sealing material of AA 2 i.e. sealing material with aggregate tailored (i.e. matched) to the anode body, performed better (exhibits less corrosion) than the prior art sealing material.
  • pin of AA 2 performed better (exhibits less corrosion) than the pin of AA 1 (the prior art anode apparatus).
  • the silica e.g. SiO 2 present as aggregate in the sealing material
  • the silica creates pockets of reactive silicates available to interact with the reactive species present in the vapor space.
  • the reactive silicates in the aggregates of the sealing material will react with fluoride gas present in the vapor space of the cell, in turn creating silicon tetrafluoride, which is in turn corrosive to the pin.
  • the reactive silicon fluoride species further interacts/reacts with the pin, pockets or holes are created in the sealing material (i.e. reducing the mechanical strength/structural support of the sealing material, and yielding pores/holes where the reactive species can further penetrate into and react with the sealing material, or other components of the anode apparatus.
  • the silicon fluoride species react with the pin materials, initiation sites of corrosion occur on the pin and the structural integrity of the anode apparatus and/or the electrical efficiency of this component are further reduced).
  • the magnetite aggregate e.g. SiO 2 and/or Al 2 O 3 replacement in the sealing material
  • the magnetite aggregate creates pockets of aggregate tailored to not undergo significant reactions with the reactive species (and thus, will not form pores in the sealing material and/or further attribute to pin corrosion).
  • inert anode apparatuses having a pin which provides a mechanical and electrical connection to the anode body, where the pin extends down into the hole of the anode body and is positioned such that the lower end of the pin is located above the vapor-bath interface.

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electron Sources, Ion Sources (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US16/334,134 2016-09-19 2017-09-19 Anode apparatus and methods regarding the same Pending US20200063279A1 (en)

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US16/334,134 US20200063279A1 (en) 2016-09-19 2017-09-19 Anode apparatus and methods regarding the same
PCT/US2017/052289 WO2018053515A1 (fr) 2016-09-19 2017-09-19 Appareil à anode et procédés associés

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AU2017327000A1 (en) 2019-04-18
CN109715862B (zh) 2021-11-16
WO2018053515A1 (fr) 2018-03-22
AU2017327000B2 (en) 2023-06-15
DK201970168A1 (da) 2019-04-01
CA3037199A1 (fr) 2018-03-22
EP3516094A4 (fr) 2020-07-15
EP3516094A1 (fr) 2019-07-31
BR112019005313B1 (pt) 2023-11-21
CA3037199C (fr) 2022-01-04
ZA201902264B (en) 2022-06-29
DK181019B1 (en) 2022-09-27
CN109715862A (zh) 2019-05-03
BR112019005313A2 (pt) 2019-09-17
SA519401348B1 (ar) 2022-05-22

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