EP3904563A1 - Dispositif de dissolution, panier de dissolution, installation de galvanisation et procédé de dissolution de zinc - Google Patents

Dispositif de dissolution, panier de dissolution, installation de galvanisation et procédé de dissolution de zinc Download PDF

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Publication number
EP3904563A1
EP3904563A1 EP20171777.4A EP20171777A EP3904563A1 EP 3904563 A1 EP3904563 A1 EP 3904563A1 EP 20171777 A EP20171777 A EP 20171777A EP 3904563 A1 EP3904563 A1 EP 3904563A1
Authority
EP
European Patent Office
Prior art keywords
dissolving
zinc
section
release
electrolyte
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20171777.4A
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German (de)
English (en)
Inventor
Hartmut Schöfisch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dr Ing Max Schloetter GmbH and Co KG
Original Assignee
Dr Ing Max Schloetter GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dr Ing Max Schloetter GmbH and Co KG filed Critical Dr Ing Max Schloetter GmbH and Co KG
Priority to EP20171777.4A priority Critical patent/EP3904563A1/fr
Publication of EP3904563A1 publication Critical patent/EP3904563A1/fr
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/18—Regeneration of process solutions of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc

Definitions

  • the invention relates to a release device with a release basket for receiving zinc elements and for an electrolyte to flow through them.
  • the invention also relates to an electroplating system with such a release device and a method for releasing zinc.
  • insoluble anodes are usually used in the zinc deposition baths, and the zinc is added to the bath in dissolved form as Zn (II).
  • electrolyte is usually removed from the bath and fed into a separate zinc dissolving device.
  • metallic zinc is anodically dissolved to form Zn (II) in the electrolyte, and the electrolyte thus enriched with Zn (II) is returned to the treatment bath.
  • the prior art attempts to solve this problem by bringing zinc into direct contact or electrically conductive contact with a material that has a lower overvoltage for hydrogen, such as steel, in order to increase the zinc dissolution rate.
  • steel baskets are usually filled with pieces of zinc and immersed in the alkaline electrolyte.
  • the zinc pieces can be designed as spheres, hemispheres or pellets, for example.
  • reaction equations can be formulated as follows, for example: (1) Zn (0) ⁇ Zn (II) + 2 e - (2) 2 H + + 2 e - ⁇ H 2 respectively. 2 H 2 O + 2 e - ⁇ H 2 + 2 OH -
  • the electrolyte is introduced from the treatment bath into a dissolving device with a basket-like dissolving container (dissolving basket) in such a way that the electrolyte passes through the dissolving basket in a horizontal direction flows.
  • the zinc-enriched electrolyte is then fed back into the zinc plating bath in order to replace the zinc consumed in the electrodeposition process and to maintain the target value for the zinc content in the zinc plating bath.
  • An essential parameter for the constant regulation of the zinc content in the electrolyte is the variable size of the dissolution rate of the zinc to be dissolved.
  • the amount of zinc to be dissolved is regulated by changing the anode surface, i.e. the surface of the zinc in contact with the electrolyte. This is done by changing the fill level of the electrolyte in the zinc dissolving device or on the dissolving basket by changing the zinc surface that is in contact with the electrolyte by pumping in or out or by immersing or lifting the dissolving basket.
  • the release device is spatially relatively large and also expensive.
  • the dissolution rate is influenced by other factors, in particular the speed at which the electrolyte flows onto the zinc surface, the dirt in the dissolving baskets and the oxidation of the zinc surface. With the current state of the art, however, these factors are not or only insufficiently taken into account for regulating the release rate.
  • the invention aims to provide a release basket for receiving zinc elements and a release device with which a refined influencing and / or regulation the dissolution rate is made possible while at the same time increasing the efficiency of the dissolution system.
  • the invention provides a release basket with the features according to claims 1-5 and a release device with the features according to claims 6-13.
  • the invention also relates to an electroplating system with such a release device and a method for releasing zinc.
  • the dissolving basket according to the invention has a housing which is provided for receiving pieces of zinc, preferably in the form of spheres, hemispheres, pellets or other shapes and through which the electrolyte flows during operation.
  • a feed section is provided which is designed in such a way that, when the dissolving basket is in use, an electrolyte introduced into the housing by means of the feed section has or forms a flow direction component in the dissolving basket that is initially at least partially aligned in a vertical direction.
  • the feed line section can be attached to the upper or lower end of the housing.
  • the flow direction component can be partially inclined in relation to a vertical direction, or the flow can initially take place vertically and then be deflected laterally or radially. This can be done in particular by means of a tube which is attached vertically in the release cage and provided with radial openings.
  • the electrolyte flows vertically into the pipe from the feed section and exits the radial openings, so that the vertical flow changes into a horizontal flow from the inside to the outside.
  • the flow rate by setting the flow rate, a targeted control of the release rate is made possible.
  • the flow rate of the electrolyte through the dissolving basket can be regulated directly.
  • a plurality of dissolving baskets can be used, and the electrolyte flow is switched on or off or regulated individually for each basket in order to obtain a desired total flow rate.
  • a cleaning effect can be significantly improved during the process.
  • a targeted and intensive flow removes dirt and degradation products that have accumulated in the dissolving basket.
  • the release basket preferably has a substantially basket-shaped or cage-shaped shape, so that dirt particles can settle through the openings in the bottom of the basket or cage outside the basket in areas provided for this purpose.
  • the loosening device preferably has a calming area downstream of the actual loosening area, in which dirt particles whirled up or suspended by the flow during the zinc loosening can settle.
  • release device (100) The structure of the release device (100) is described below with reference to the FIGS Figures 1 and 2 embodiment shown in more detail.
  • the release device (100) is designed to operate in conjunction with a galvanic zinc plating bath (not shown). It is preferably a bath that uses an alkaline zinc electrolyte.
  • the electrolyte is typically removed from the zinc deposition bath (not shown) and is to be enriched with zinc in the dissolving device and then returned to the zinc deposition bath. This can be done, for example, continuously while the deposition bath is in operation, in order to keep the zinc concentration in the zinc deposition bath within a specified working range.
  • the release device (100) comprises at least one release section (110) which is provided for receiving one or more of the release baskets (10) described below and in which the actual release process takes place.
  • the release device further comprises, as in FIG Figure 1 shown, a sludge chamber (120) arranged in the vertical direction below the release section (110), a calming section (130) arranged adjacent to the release section (110) and an exchange section (140) arranged adjacent to the calming section (130).
  • a sludge chamber 120
  • a calming section 130
  • an exchange section 140
  • the electrolyte is introduced into the dissolving section (110) and enriched with Zn (II) by anodic dissolution of the zinc pieces contained in the dissolving baskets (10).
  • the electrolyte enriched with Zn (II) then reaches the calming section (130), in which any suspended dirt particles can settle as a result of the flow.
  • the electrolyte then enters the exchange section (140) and is returned from there to the zinc plating bath.
  • the release section (110) preferably comprises one or more chambers (110a) - (110x), each of which is arranged adjacent to one another or in several rows.
  • the chambers (110a) - (110x) are each separated from one another by a partition.
  • Each of the chambers is provided for receiving an individual dissolving basket, and the dissolving baskets can be removed from the respective chamber.
  • the number of chambers is not particularly limited and can be selected appropriately depending on the bath volume and throughput or on the amount of zinc to be dissolved. It can be, for example, between 1 and 100, preferably 3 to 50, in particular 5 to 20.
  • the chambers can be arranged in a row or in several rows.
  • the release baskets are thus arranged in separate chambers, the amount of hydrogen produced is kept low in the event of an emergency standstill due to the comparatively small amount of electrolyte in each chamber, and thus the risk of hydrogen deflagration is minimized.
  • the chambers can also be emptied independently of one another in an emergency standstill of the release device (100) or also outside of the operation of the release device (100). This prevents or minimizes the further development of hydrogen, but also the oxidation processes between the electrolyte and the anodes.
  • An emergency drain (117) is also preferably provided, which can be opened, for example, in the event of a power failure, in order to remove the electrolyte from the chambers (110a) - (110x).
  • a currentless openable valve is used on the emergency drain (117), which opens with a previously defined time delay if necessary.
  • the chambers (110a) - (110x) have feed lines (111a) - (111x) for the electrolyte to be enriched with zinc, each of which ends at a feed line opening (112a) - (112x).
  • the feed line opening is opened upwards in the vertical direction in order to conduct the electrolyte through the dissolving baskets described below.
  • the feed lines are each provided with a shut-off valve so that the electrolyte supply in the chambers can be individually regulated or switched on and off.
  • the rate of zinc dissolution can be regulated, for example by only having the electrolyte flow through some of the chambers.
  • the electrolyte flow rate in the supply lines can preferably be regulated. This can be done, for example, with the aid of the pump (s) provided for the electrolyte supply (not shown) and / or via the shut-off valves (not shown).
  • the release basket (10) is intended to receive the zinc pieces to be released and, during operation, the electrolyte flows through it, which exits vertically upwards from the feed opening (112a).
  • the dissolving basket is preferably made at least partially from a metal which, under the dissolving conditions, has a lower hydrogen overvoltage than zinc and is in contact with the zinc pieces. This allows a local element to form, with the zinc pieces acting as the anode and the metal as the cathode: (1) Zn (0) ⁇ Zn (II) + 2 e - (2) 2 H 2 O + 2 e - ⁇ H 2 + 2 OH -
  • the metal is preferably iron or an iron alloy such as, in particular, steel.
  • the surface of the metal is provided with a thermally sprayed iron layer to further improve the dissolution rate, as in FIG EP 3,222,757 described.
  • the dissolving basket can be made entirely of the metal. Alternatively, only parts of the basket (e.g. the side wall) can consist of the metal, or the basket can also be made of a different material and is provided with an insert made of the metal.
  • the release basket is preferably like a basket or cage and is open at the top so that zinc pieces can be easily refilled.
  • the shape of the cross section is not particularly limited and may, for example, be substantially round, rectangular, or square.
  • the bottom is provided with openings so that impurities and sludge can escape downwards, in particular into the sludge chamber (120) described below.
  • the release basket (10) comprises a housing (11) with a base plate (11a) (first end section), a circumferential side wall (11b) and an upper section (11c) (second end section).
  • the bottom plate (11a) faces downward and the side wall (11b) extends in a vertical direction.
  • the side wall (11b) of the dissolving basket (10) is provided with a large number of passages (11b-1) so that the electrolyte can flow in or out of the housing (11) of the dissolving basket (10) from the side.
  • the bottom plate (11a) of the dissolving basket (10) has a feed section (12) which forms a through opening which is essentially centrally arranged in the plan view of the dissolving basket (10) and is opposite the feed opening (112a).
  • the electrolyte fed in via the feed opening (112a) is introduced into the dissolving basket (10) through this passage opening.
  • outlet openings (11a-1) are provided on the base plate (11a), through which a sludge formed when dissolving zinc in the electrolyte is disposed under the dissolving section (110) and thus also under the dissolving basket (10) Mud chamber (120) can reach.
  • the sludge that has accumulated can thus be easily removed from a dirty area of the release device. A filtration can therefore be omitted, even if it is conceivable that such a filtration is provided in addition.
  • the zinc pieces located further down may act as a flow obstacle, so that the flow of the zinc pieces is reduced from bottom to top. This can lead to a stronger passivation of zinc pieces lying on top, which are less exposed to the flow, and thus to a reduction in the rate of dissolution.
  • a tube (15) is integrated in the release cage on the feed section (12), which tube extends in the housing (11) preferably centrally along the vertical alignment of the side wall (11b) of the housing (11).
  • the tube (15) has a multiplicity of radial openings (15a) through which the electrolyte guided through the tube (15) can flow out radially. In this way, a uniform flow of the zinc pieces over the entire vertical axis of the dissolving basket ensured from the inside to the outside.
  • the electrolyte flow also has a cleaning effect in that it washes away impurities or passivating oxides that form during the dissolution process from the zinc surface. Most of the particles released in this way settle downwards and thus get into the sludge chamber described in the following section. Depending on the flow rate, a certain proportion of particles can also remain suspended and are retained in the calming compartment described below.
  • the outlet openings (11a-1) in the bottom of the dissolving basket prevent the settling particles from remaining in the dissolving basket as sludge. This significantly reduces the maintenance effort.
  • a sludge chamber (120) is preferably attached in the vertical direction below the release section (110), and thus also below the release basket (10).
  • the sludge chamber (120) extends along the entire dissolving section (110) and can thus be used by several dissolving baskets if several dissolving baskets are required due to the required amount of zinc.
  • the sludge produced during the dissolving process can enter the sludge chamber (120) through the outlet openings (11b-1) of the base plate (11a) of the dissolving basket.
  • a cleaning opening (125) is provided for cleaning the sludge chamber.
  • the electrolyte typically contains dispersed gas (hydrogen and / or air bubbles) and possibly also impurity particles. By lingering in the calming section (130), these are removed by means of outgassing or sedimentation, or they are deposited on the bottom of the calming section (130).
  • the electrolyte enriched with dissolved zinc flows over a first partition (115) formed between the release section (110) and the calming section (130) and thus flows into the calming section (130).
  • the calming section (130) is delimited by the partition (115) provided between the calming section (130) and the release section (110) and a barrier (135) which extends parallel to the first partition (115).
  • An overflow weir (116) is preferably provided on the first partition (115) on the side facing the calming section (130).
  • the overflow weir acts as a flow sheet for the electrolyte to facilitate outgassing and to reduce any foam formation.
  • the overflow weir (116) forms an angle to the vertically oriented first partition wall (115), for example in the range of approx. 30-60 °.
  • An exchange section (140) is preferably provided adjacent to the calming section (130). In the embodiment shown, these sections are separated from one another by a second partition (135), the upper edge of which acts as an overflow weir.
  • a shielding wall (141) can be attached parallel to the second partition (135), so that a passage (142) is created between the second partition (135) and the shielding wall (141).
  • the shielding wall (141) extends higher than the barrier (135), so that the electrolyte that passes from the calming section (130) into the exchange section (140) in a lower section of the exchange section (140) passes through an area between the barrier (135) and the opening provided in the shielding wall (141) passes through.
  • the exchange section (140) can be provided with an inlet (144) for the direct supply of electrolyte from the zinc deposition bath.
  • the electrolyte circulation between the dissolving device and the zinc deposition bath can be maintained.
  • the zinc concentration can also be used if necessary can be reduced in the exchange compartment in order to set a certain setpoint.
  • a changeover valve (not shown) is preferably also provided, with which the electrolyte removed from the zinc deposition bath can optionally be fed to the inlets of the release section (111a) - (111x) or via the inlet (144) directly into the exchange compartment.
  • the release device also preferably has a suction device with one or more suction channels (150), which is preferably attached above the calming section (130) and can thus suck out several adjacent areas of the release device.
  • the release device is preferably provided with a cover which, for example, can be composed of a plurality of cover elements.
  • the release section in the filling area above the release baskets can be provided with one or more hinged lids (160), and the replacement compartment can be covered with a plurality of removable lids (170). The suction then takes place from the gas space formed by the cover above the release device.
  • the zinc dissolving process according to the invention is carried out with the dissolving device according to the invention in connection with a galvanic zinc deposition bath.
  • a galvanic zinc deposition bath Preferably an alkaline zinc or zinc alloy bath (e.g. Zn / Ni) is used.
  • the release baskets (10) are filled with metallic zinc, preferably in the form of pellets, spheres or hemispheres.
  • the electrolyte to be enriched with zinc is removed from the zinc deposition bath and introduced into a respective chamber (110a) - (110x) via the supply lines (111a) - (111x) with the aid of one or more pumps (not shown).
  • the electrolyte flow rate is regulated with the aid of the pump (s) and, if necessary, the valves attached to the supply lines. It is also possible to use only some of the release chambers and to switch off the rest or not to equip them with release baskets (10).
  • the electrolyte flows into the tube (15) of the dissolving basket (10) arranged in the respective chamber and exits in the radial direction through the radial openings (15a) of the tube (15).
  • the zinc pieces are exposed to a uniform lateral flow along the entire length of the dissolving basket. This prevents passivation of the zinc surface and improves the uniformity of the dissolution rate of the entire amount of zinc in the dissolving basket.
  • the zinc pieces preferably form a local element with the metal of the container, so that the zinc goes into solution as Zn (II), while the hydrogen evolution mainly takes place on the metal.
  • the electrolyte thus enriched with zinc which typically contains hydrogen bubbles and possibly also air and / or dispersed dirt particles, then flows over the first partition (115) and, after flowing over the overflow weir (116), reaches the calming section (130) of the release device (100). By lingering in the calming section, gases and particles can separate out.
  • the electrolyte then flows over the second partition (135) and is introduced into the exchange section (140) through the passage (142) provided between the second partition (135) and the shielding wall (141) and is pumped out from there by means of a pump.
  • the zinc-enriched electrolyte pumped out of the exchange section (140) is returned to the zinc plating bath.
  • the electrolyte removed from the zinc deposition bath can also be fed directly into the exchange section (144) via the inlet (144), bypassing the dissolving and calming section. This may be necessary, for example, in order to maintain the electrolyte circulation in the event of an interruption of the zinc dissolution process, or in order to reduce the zinc concentration in the exchange section (140) to a desired target value.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
EP20171777.4A 2020-04-28 2020-04-28 Dispositif de dissolution, panier de dissolution, installation de galvanisation et procédé de dissolution de zinc Pending EP3904563A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP20171777.4A EP3904563A1 (fr) 2020-04-28 2020-04-28 Dispositif de dissolution, panier de dissolution, installation de galvanisation et procédé de dissolution de zinc

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP20171777.4A EP3904563A1 (fr) 2020-04-28 2020-04-28 Dispositif de dissolution, panier de dissolution, installation de galvanisation et procédé de dissolution de zinc

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EP3904563A1 true EP3904563A1 (fr) 2021-11-03

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4401522A (en) * 1980-09-29 1983-08-30 Micro-Plate, Inc. Plating method and apparatus
DE29605315U1 (de) * 1996-03-21 1996-05-30 Surtec Gmbh Vorrichtung zum Auflösen von unedlen Metallen
US5932077A (en) * 1998-02-09 1999-08-03 Reynolds Tech Fabricators, Inc. Plating cell with horizontal product load mechanism
EP3222757A1 (fr) 2016-03-23 2017-09-27 Dr.Ing. Max Schlötter GmbH & Co. KG Procede et dispositif destines a la dilution de zinc

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4401522A (en) * 1980-09-29 1983-08-30 Micro-Plate, Inc. Plating method and apparatus
DE29605315U1 (de) * 1996-03-21 1996-05-30 Surtec Gmbh Vorrichtung zum Auflösen von unedlen Metallen
US5932077A (en) * 1998-02-09 1999-08-03 Reynolds Tech Fabricators, Inc. Plating cell with horizontal product load mechanism
EP3222757A1 (fr) 2016-03-23 2017-09-27 Dr.Ing. Max Schlötter GmbH & Co. KG Procede et dispositif destines a la dilution de zinc

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
R. LUDWIGR. HOLLAND: "Zinc Generator Tanks for the Alkaline Cyanide-Free Zinc Plater", METAL FINISHING, vol. 6, 1998, pages 106 - 112

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