CN108754395B - The preparation method of electrolytic zinc anode plate surface anticorrosion coating - Google Patents

The preparation method of electrolytic zinc anode plate surface anticorrosion coating Download PDF

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CN108754395B
CN108754395B CN201810581533.1A CN201810581533A CN108754395B CN 108754395 B CN108754395 B CN 108754395B CN 201810581533 A CN201810581533 A CN 201810581533A CN 108754395 B CN108754395 B CN 108754395B
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anode plate
sprayed
spraying
plate
powder
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CN108754395A (en
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李强
谈耀宏
刘栢伶
虞志轩
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Fuzhou University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134Plasma spraying
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06Metallic material
    • C23C4/073Metallic material containing MCrAl or MCrAlY alloys, where M is nickel, cobalt or iron, with or without non-metal elements
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11Oxides
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/02Electrodes; Connections thereof

Abstract

The invention discloses a kind of electrolysis (product) zinc anode plate surface corrosion-inhibiting coating and preparation methods, it is the sprayed on material for spraying resistance to sulfuric acid solution, resistance to fluoride ions and chloride ion corrosion in the regional scope of 5cm under anode plate upper end to liquid level line, to obtain band coating corrosion protection anode plate.The sprayed on material chosen in the present invention is sprayed on anode plate, neither influences the electrolytic efficiency of zinc, and can effectively slow down the corrosion of pole plate, so that the service life of anode plate be made to extend 2-3 months.Technology investment involved in the present invention is small, process flow is simple, to equipment without particular/special requirement, low energy consumption, pollution-free, application prospect is extensive.

Description

The preparation method of electrolytic zinc anode plate surface anticorrosion coating
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to a kind of electrolysis (product) zinc anode plate surface corrosion-inhibiting coating and Preparation method.
Background technique
Zinc surface layer protecting film easily generated at normal temperature has excellent weather-resistant performance, therefore zinc is mainly used In the overlay coating (such as galvanized sheet) of steel and steel construction piece, it is related to numerous industries such as automobile, building, ship, light industry.In recent years Come, with the lasting investment of the technologies such as the continuous development of energy storage industry, especially Zn-Mg battery, zinc air battery, zinc is wide General use is in battery industry.
There are three types of the preparation methods of usual zinc: first is that marmatite or zincblende are sintered into zinc oxide in air, so Reduction with carbon is made afterwards;Second is that zinc oxide and coke are mixed, it is heated to 1373K ~ 1573K in blast furnace, goes out zinc distillation Come;Third is that by control pH, zinc is set to be dissolved as zinc sulfate and the hydrolysis of the impurity such as iron arsenic antimony is converted into precipitating, then addition zinc powder removes The impurity such as the copper cadmium in filtrate are removed, then are deposited zinc with electrolysis method.The zinc purity wherein produced in the third method compared with Height, about 99.99%.
In electrolytic zinc, the zinc sulfate of the plate face overwhelming majority submergence of fine aluminium cathode plate and chloride plate in a cell is molten In liquid, extent of corrosion is poor, substantially intact;But the neck above section that cathode plate and the plate face of anode plate connect with bridge due to It is exposed other than solution of zinc sulfate, produced in the more serious environment of acidity for a long time, seriously corroded shortens cathode plate and anode The service life of plate, increases production cost.Wherein, the corrosion characteristics of anode plate are mainly shown as plate face corrosion failure, liquid level The fracture of line position and anode package conductive rod sheet lead part cracking etc..It is found through experiment that this is mainly due to be exposed to air In partially due to directly with the oxygen in air, carbon dioxide, sulfuric acid mist contact, these are rotten at the gas liquid film It loses medium and forms a stronger microenvironment of corrosivity in anode plate surface, make the anode plate in this environment by tight The corrosion of weight will not etc. not scrapped by 10 months using some months generally, cause great waste.In addition, in zinc hydrometallurgy During, the chloride ion and fluorine ion for being mainly derived from calcining and zinc oxide are another major reasons for causing pole plate to corrode. Chloride ion in solution can react with chloride plate, and anode plate is caused to corrode, and reduce the service life of anode plate, and molten The lead for entering electrolyte will lead to lead tolerance in the zinc of precipitation and increase;Meanwhile the Ag in anode plate is also oxidized to Ag+Into electrolysis Liquid, and be precipitated in cathode, Zn-Ag primary battery is formed with Zn, harm is generated to zinc electrolysis.On the other hand, since anode has oxygen It generates, the fluctuation for causing liquidus surface is precipitated in the continuous of gas, impacts the position of anode liquidus surface, and this long-term fluctuation is patted Exacerbate the corrosion of anode liquidus surface position.Through counting, due to the generation of corrosion, one ton of zinc of every production will consume 0.2 ~ 0.3 Block pole plate consumes pole plate 100 ~ 1,500,000 piece pole plate by China's 5,000,000 tons of zinc hydrometallurgy calculating in 2015 in year.Therefore it researchs and develops Zinc electrolysis pole plate aseptic technic meaning processed is very great.
Summary of the invention
The present invention in view of the above problems, provides a kind of electrolysis (product) zinc anode plate surface corrosion-inhibiting coating and preparation Method is to choose the material of energy sulfuric acid corrosion resistant as sprayed on material, is sprayed in the specific region of anode plate, is obtained Band coating corrosion protection anode plate, which neither influences the electrolytic efficiency of zinc, and can effectively slow down the corrosion of pole plate, thus The service life of anode plate is set to extend 2-3 months.Technology investment involved in the present invention is small, process flow is simple, to equipment without spy Different requirement, low energy consumption, pollution-free, application prospect is extensive.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method being electrolysed (product) zinc anode plate surface corrosion-inhibiting coating comprising following steps:
(1) lead-containing alloy for being used as anode plate is chosen, and demarcates its liquid level line position;
(2) decontamination oil removal treatment is carried out to anode plate surface;
(3) spraying area delimited on anode plate, and blasting treatment is carried out to spraying area;
(4) sprayed on material is chosen;
(5) spray treatment is carried out in sand blasted area.
Lead-containing alloy described in step (1) is lead silver bianry alloy or lead-based multi-component alloy;The liquid level line position is sun Pole plate immerses the height in electrolyte.
Decontamination oil removal treatment described in step (2) is specifically first used ethanol anode plate plate face 10 minutes, later with clear Water rinses, then is wiped plate face 15 minutes with acetone, and clear water rinses.
Spraying area described in step (3) is the regional scope of 5cm under anode plate upper end to liquid level line;Due to lead when sandblasting Based alloy is softer, should adjust moderate pressure, there is certain angle between nozzle and anode plate face, just liquidate to avoid strong gravel Hit anode plate surface.
Sprayed on material described in step (4) should have the performance of the burn into of resistance to sulfuric acid solution resistance to fluoride ions and chloride ion corrosion, And there should be similar thermal expansion coefficient with anode plate, such as Ceramics powder, metal alloy powder or two phase stainless steel;The ceramics Powder includes aluminium oxide, zirconium oxide or alumina zirconia mixed powder;The metal alloy powder includes nickel-base alloy powder, cobalt-base alloys Powder, nickel cobalt-based alloy powder, self-melting alloy powder, the chromium carbide compounded powder of nickel chromium triangle-, lead-base alloy powder, acid bronze alloy powder, nickel-chromium- Tungsten-molybdenum system column, nickel-chromium-molybdenum system column (MAT 21, VDM 59, Inconel 686, Hastelloy C alloys -276, Hastelloy B-4 etc.) In any one.
When sprayed on material is ceramic powder, one layer of adhesive layer need to be first sprayed in the anode plate surface after blasting treatment, then It is sprayed on adhesive layer using the method for thermal spraying again and forms ceramic layer;Wherein, adhesive layer with a thickness of 10-1000 μm;Ceramics Layer with a thickness of 10-1000 μm;When sprayed on material is metal alloy powder, the anode plate surface directly after blasting treatment is carried out Spraying;Its coating layer thickness is 10-1500 μm.
The method of the spraying includes supersonic flame spraying, air plasma spraying, cold spray, electric arc spraying, suspension Any one in spraying.
It should ensure that anode plate adequately cools down when spray treatment, i.e., the cooling temperature of anode back should be controlled at 230 DEG C Below, it is ensured that the temperature for spraying to sprayed on material in anode plate plate face is lower than the fusing point of anode plate material.
Remarkable advantage of the invention is:
The present invention chooses the material of energy sulfuric acid corrosion resistant, resistance to fluoride ions and chloride ion corrosion as sprayed on material, in anode One layer of protective coating is sprayed in plate specific region, coating layer thickness is smaller, and cumulative stress is small, so compactness is good, bond strength Height can effectively prevent fluorine ion, chloride ion and other corrosive mediums from spreading into coating, substantially increase the corrosion resistant of anode plate Corrosion energy makes the service life of anode plate extend 2-3 months and (does not spray anode plate average life 19 of protective coating Month), and the electrolytic efficiency of zinc is not influenced.Meanwhile cost is relatively low for the coating material, preparation process is simple, has good application Benefit.The small, process flow of present invention process investment is simple, to equipment without particular/special requirement, low energy consumption, pollution-free, application prospect is wide It is general.
Detailed description of the invention
Fig. 1 is the area schematic of the anode plate handled by the method for the present invention;In figure: 1- anode plate, 2- liquid level line, 3- spray Sand and spraying area.
Fig. 2 is the anode plate sample drawing for being coated with zirconia coating of case study on implementation one of the present invention preparation.
Fig. 3 is the anode plate sample drawing for being coated with Hastelloy C-276 coating of case study on implementation two of the present invention preparation.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention Technical solution is described further, but the present invention is not limited only to this.
Embodiment one:
(1) the lead silver bianry alloy (silver content 0.6%) for being used as anode plate is chosen, and demarcates its liquid level line position;
(2) it is first carefully wiped with ethyl alcohol anode plate plate face 10 minutes, is rinsed later with clear water, then wipe plate face 15 with acetone Minute, clear water rinses;
(3) regional scope for delimiting 5cm under anode plate upper end to liquid level line is spraying area, and is sprayed to spraying area Sand processing;Pressure is 0.3MPa-0.5MPa when sandblasting, and the angle between nozzle and anode plate face is 15 ° -60 °, to avoid strong Gravel face impacts anode plate surface;
(4) NiCoCrAlY powder is chosen as bonding layer material, and the Zirconium oxide powder that partial size is 45~75 μm is as spraying Material;NiCoCrAlY powder and Zirconium oxide powder are respectively placed in baking oven and dried 5 hours for 80 DEG C;
(5) sand blasted area of the plasma spraying method after blasting treatment is used to spray a layer thickness as 50 μm of bonding Layer, then using plasma spraying method again, coating thickness is 100 μm of zirconia ceramic layer on adhesive layer, and specifically spraying is joined Number is shown in Table 1.
1 plasma sprayed ceramic material technology parameter of table
Embodiment two:
(1) the lead silver bianry alloy (silver content 0.6%) for being used as anode plate is chosen, and demarcates its liquid level line position;
(2) it is first carefully wiped with ethyl alcohol anode plate plate face 10 minutes, is rinsed later with clear water, then wipe plate face 15 with acetone Minute, clear water rinses;
(3) regional scope for delimiting 5cm under anode plate upper end to liquid level line is spraying area, and is sprayed to spraying area Sand processing;Pressure is 0.3MPa-0.5MPa when sandblasting, and the angle between nozzle and anode plate face is 15 ° -60 °, to avoid strong Gravel face impacts anode plate surface;
(4) Hastelloy C-276 powder is chosen as sprayed on material, and powder is placed in baking oven and is dried 5 hours for 80 DEG C;
(5) sand blasted area of the plasma spraying method after blasting treatment is used to spray a layer thickness as 150 μm Hastelloy C-276 coating, specific spray parameters are shown in Table 2.
2 plasma spraying nickel-base alloy technological parameter of table
The coating of above-mentioned technique preparation is well combined, surface compact, can effectively stop under acidic environment fluorine ion with Corrosion of the substances such as chloride ion to exposed aerial anode plate.But from electrochemistry angle analysis, in spraying area and liquid level The regional area immersed in acidic electrolysis bath between line there is also all one, which form a faint primary batteries, wherein with For Hastelloy: nickel, cobalt, molybdenum standard electrode potential are respectively -0.241, -0.267, -0.2, the both less than normal electrode of hydrogen Current potential will obviously occur to react as follows from thermodynamics:
Calculate the Gibbs free energy of the reaction;According to △ G=- n E F;E=- 0.2- (- 0.126)=- 0.074 be (lead Standard electrode potential be -0.126), when taking n=2, F=96485.3385C/mol, then G=14279.83 △=14.3KJ/mol > 0, i.e., from the angle of Gibbs free energy, the reaction spontaneous will not occur.Thus, this between spraying area and liquid level line Although one region forms a faint primary battery, but it can't cause to corrode to coating, i.e., the method for the present invention is reliable , it is able to achieve the good resistance to sulfuric acid solution corrosion of anode plate.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (5)

1. a kind of preparation method of electrolytic zinc anode plate surface anticorrosion coating, it is characterised in that: the following steps are included:
(1) lead-containing alloy for being used as anode plate is chosen, and demarcates its liquid level line position;
(2) decontamination oil removal treatment is carried out to anode plate surface;
(3) spraying area delimited on anode plate, and blasting treatment is carried out to spraying area;
(4) sprayed on material is chosen;
(5) spray treatment is carried out in sand blasted area;
Sprayed on material described in step (1) is ceramic powder, metal alloy powder or two phase stainless steel;
The ceramic powder includes aluminium oxide, zirconium oxide or alumina zirconia mixed powder;The metal alloy powder includes Ni-based conjunction Bronze, cobalt-based alloy powder, nickel cobalt-based alloy powder, self-melting alloy powder, the chromium carbide compounded powder of nickel chromium triangle-, lead-base alloy powder, copper-based conjunction Bronze, nickel-chromium-molybdenum system column, any one in nickel-chromium-tungsten-molybdenum system column;
When sprayed on material is ceramic powder, one layer of adhesive layer need to be first sprayed in the anode plate surface after blasting treatment, then adopted again It is sprayed on adhesive layer with the method for thermal spraying and forms ceramic layer;Wherein, adhesive layer with a thickness of 10-1000 μm;Ceramic layer With a thickness of 10-1000 μm;
When sprayed on material is metal alloy powder, the anode plate surface directly after blasting treatment is sprayed;Its coating layer thickness It is 10-1500 μm.
2. the preparation method of electrolytic zinc anode plate surface anticorrosion coating according to claim 1, it is characterised in that: step (1) Described in lead-containing alloy be lead silver bianry alloy or lead-based multi-component alloy.
3. the preparation method of electrolytic zinc anode plate surface anticorrosion coating according to claim 1, it is characterised in that: step (2) Described in decontamination oil removal treatment specifically first use ethanol anode plate plate face 10 minutes, rinsed later with clear water, then use acetone Wiping plate face 15 minutes, clear water rinse.
4. the preparation method of electrolytic zinc anode plate surface anticorrosion coating according to claim 1, it is characterised in that: step (3) Described in spraying area be anode plate upper end to liquid level line under 5cm regional scope.
5. the preparation method of electrolytic zinc anode plate surface anticorrosion coating according to claim 1, it is characterised in that: the spraying Method include supersonic flame spraying, air plasma spraying, cold spray, electric arc spraying, any one in suspension spray.
CN201810581533.1A 2018-06-07 2018-06-07 The preparation method of electrolytic zinc anode plate surface anticorrosion coating Active CN108754395B (en)

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