CN108754395B - Preparation method of anticorrosive coating on surface of electrolytic zinc anode plate - Google Patents
Preparation method of anticorrosive coating on surface of electrolytic zinc anode plate Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/073—Metallic material containing MCrAl or MCrAlY alloys, where M is nickel, cobalt or iron, with or without non-metal elements
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
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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
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
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Abstract
The invention discloses an electrolytic (zinc deposition) anode plate surface anticorrosive coating and a preparation method thereof, wherein a sulfuric acid solution resistant spraying material, a fluorine ion resistant spraying material and a chlorine ion resistant spraying material are sprayed in a region ranging from the upper end of an anode plate to 5cm below a liquid level line, so that the coated anticorrosive anode plate is obtained. The spraying material selected in the invention is sprayed on the anode plate, which does not affect the electrolytic efficiency of zinc, and can effectively slow down the corrosion of the anode plate, thereby prolonging the service life of the anode plate by 2-3 months. The invention has the advantages of small process investment, simple process flow, no special requirements on equipment, low energy consumption, no pollution and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of hydrometallurgy, and particularly relates to an electrolytic (accumulated) zinc anode plate surface anticorrosive coating and a preparation method thereof.
Background
At normal temperature, a layer of protective film is easy to generate on the surface of zinc, and the zinc has excellent atmospheric corrosion resistance, so that the zinc is mainly used for surface coating of steel and steel structural members (such as galvanized plates), and relates to a plurality of industries such as automobiles, buildings, ships, light industry and the like. In recent years, with the continuous development of the energy storage industry, especially the continuous input of technologies such as zinc-manganese batteries and zinc-air storage batteries, zinc is widely used in the battery industry.
There are generally three methods of zinc preparation: firstly, the sphalerite or sphalerite is calcined into zinc oxide in the air and then reduced by carbon to prepare the zinc oxide; secondly, mixing zinc oxide and coke, heating the mixture in a blast furnace to 1373K to 1573K, and distilling out zinc; thirdly, zinc is dissolved into zinc sulfate by controlling pH, impurities such as iron, arsenic, antimony and the like are hydrolyzed and converted into precipitates, then zinc powder is added to remove impurities such as copper, cadmium and the like in the filtrate, and the zinc is deposited by an electrolytic method. The purity of the zinc prepared by the third method is high, about 99.99%.
During zinc electrolysis, most of the surfaces of the pure aluminum cathode plate and the lead anode plate are immersed in a zinc sulfate solution in the electrolytic bath, so that the corrosion degree is poor and basically intact; however, the parts above the necks where the surfaces of the cathode plate and the anode plate are connected with the bridge are exposed outside the zinc sulfate solution, so that the corrosion is serious, the service lives of the cathode plate and the anode plate are shortened, and the production cost is increased. The corrosion characteristics of the anode plate are mainly represented by plate surface corrosion perforation, liquid level line part fracture, cracking of a lead sheath part of the anode-coated conducting rod and the like. Tests show that the part exposed in the air directly contacts with oxygen, carbon dioxide and sulfuric acid mist in the air due to the fact that the part is located at a gas-liquid phase interface, and the corrosive media form a microenvironment with stronger corrosivity on the surface of the anode plate, so that the anode plate in the environment is seriously corroded, and is generally scrapped after being used for several months to 10 months, and great waste is caused. In addition, in the zinc hydrometallurgy process, chloride ions and fluoride ions mainly derived from calcine and zinc oxide are another important cause of corrosion of the electrode plate. Chloride ions in the solution react with the lead anode plate to cause corrosion of the anode plate, so that the service life of the anode plate is shortened, and lead dissolved in the electrolyte can cause the lead content in the separated zinc to be increased; simultaneously, ag in the anode plate is oxidized into Ag + Enters into the electrolyte and is separated out at the cathode to form a Zn-Ag primary battery with Zn, which is harmful to the zinc electrolysis. On the other hand, the anode has oxygen, the continuous separation of gas causes the fluctuation of the liquid surface, and the fluctuation impacts the position of the liquid surface of the anode, and the long-term fluctuation beating aggravates the corrosion of the position of the liquid surface of the anode. According to statistics, 0.2 to 0.3 polar plates are consumed for producing one ton of zinc due to corrosion, and 100 to 150 ten thousand polar plates are consumed annually according to 500 ten thousand tons of zinc hydrometallurgy in 2015 years of China. Therefore, the research and development of the anticorrosion technology of the zinc-making electrolytic pole plate have great significance.
Disclosure of Invention
The invention provides an electrolytic zinc anode plate surface anti-corrosion coating and a preparation method thereof aiming at the existing problems, which selects a material which can resist the corrosion of sulfuric acid as a spraying material, and sprays the material in a specific area of an anode plate to obtain the anti-corrosion anode plate with the coating, wherein the coating does not influence the electrolytic efficiency of zinc, and can effectively slow down the corrosion of the anode plate, thereby prolonging the service life of the anode plate by 2-3 months. The invention has the advantages of small process investment, simple process flow, no special requirements on equipment, low energy consumption, no pollution and wide application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an electrolytic zinc anode plate surface anticorrosive coating comprises the following steps:
(1) Selecting a lead-based alloy used as an anode plate, and calibrating the position of a liquid level line of the lead-based alloy;
(2) Carrying out decontamination and oil removal treatment on the surface of the anode plate;
(3) Defining a spraying area on the anode plate, and carrying out sand blasting treatment on the spraying area;
(4) Selecting a spraying material;
(5) And carrying out spraying treatment on the sand blasting area.
The lead-based alloy in the step (1) is a lead-silver binary alloy or a lead-based multi-element alloy; the liquid level line position is the height of the anode plate immersed in the electrolyte.
The decontamination and oil removal treatment in the step (2) is specifically to wipe the surface of the anode plate by ethanol for 10 minutes, then to wash the anode plate by clear water, and then to wipe the surface of the anode plate by acetone for 15 minutes, and then to wash the anode plate by clear water.
The spraying area in the step (3) is the area range from the upper end of the anode plate to 5cm below a liquid level line; during sand blasting, the lead-based alloy is softer, the pressure is moderate, and a certain included angle is formed between the nozzle and the anode plate surface so as to avoid strong gravel from impacting the anode plate surface.
The spraying material in the step (4) has the performances of resisting corrosion of sulfuric acid solution, resisting corrosion of fluorine ions and chlorine ions, and has a similar thermal expansion coefficient with an anode plate, such as ceramic powder, metal alloy powder or duplex stainless steel; the ceramic powder comprises alumina, zirconia or alumina zirconia mixed powder; the metal alloy powder comprises any one of nickel-based alloy powder, cobalt-based alloy powder, nickel-cobalt-based alloy powder, self-fluxing alloy powder, nickel-chromium carbide composite powder, lead-based alloy powder, copper-based alloy powder, nickel-chromium-tungsten-molybdenum series and nickel-chromium-molybdenum series (MAT 21, VDM 59, inconel 686, hastelloy C-276, hastelloy B-4 and the like).
When the spraying material is ceramic powder, firstly spraying a bonding layer on the surface of the anode plate after sand blasting treatment, and then spraying a ceramic layer on the bonding layer by adopting a thermal spraying method; wherein the thickness of the bonding layer is 10-1000 μm; the thickness of the ceramic layer is 10-1000 μm; when the spraying material is metal alloy powder, directly spraying on the surface of the anode plate after sand blasting; the thickness of the coating is 10-1500 μm.
The spraying method comprises any one of supersonic flame spraying, atmospheric plasma spraying, cold spraying, electric arc spraying and suspension spraying.
The anode plate should be fully cooled during the spraying treatment, i.e. the cooling temperature of the back of the anode plate should be controlled below 230 ℃, and the temperature of the spraying material sprayed on the plate surface of the anode plate is ensured to be lower than the melting point of the anode plate material.
The invention has the following remarkable advantages:
the invention selects the material which can resist the corrosion of sulfuric acid and the corrosion of fluorinion and chloride ion as the spraying material, and sprays a layer of protective coating in the specific area of the anode plate, the coating thickness is smaller, the stress accumulation is small, the compactness is good, the bonding strength is high, the diffusion of fluorinion, chloride ion and other corrosive media into the coating can be effectively prevented, the corrosion resistance of the anode plate is greatly improved, the service life of the anode plate is prolonged by 2-3 months (the average service life of the anode plate which is not sprayed with the protective coating is 19 months), and the electrolytic efficiency of zinc is not influenced. Meanwhile, the coating has the advantages of low raw material cost, simple preparation process and good application benefit. The invention has the advantages of small process investment, simple process flow, no special requirements on equipment, low energy consumption, no pollution and wide application prospect.
Drawings
FIG. 1 is a schematic area view of an anode plate treated in accordance with the method of the present invention; in the figure: 1-anode plate, 2-liquid level line, 3-sand blasting and spraying area.
Fig. 2 is a sample view of an anode plate sprayed with a zirconia coating prepared according to an embodiment of the present invention.
FIG. 3 is a sample of an anode plate coated with a Hastelloy C-276 coating made in accordance with example two of the present invention.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
The first embodiment is as follows:
(1) Selecting a lead-silver binary alloy (silver content is 0.6%) used as an anode plate, and calibrating the position of a liquid level line;
(2) Carefully wiping the surface of the anode plate with ethanol for 10 minutes, then washing with clear water, wiping the surface with acetone for 15 minutes, and washing with clear water;
(3) Defining the area range from the upper end of the anode plate to 5cm below a liquid level line as a spraying area, and carrying out sand blasting treatment on the spraying area; the pressure is 0.3MPa-0.5MPa when sand blasting is carried out, the included angle between the nozzle and the anode plate surface is 15-60 degrees, so as to avoid strong gravel from directly impacting the anode plate surface;
(4) Selecting NiCoCrAlY powder as a bonding layer material, and zirconium oxide powder with the particle size of 45-75 mu m as a spraying material; respectively placing NiCoCrAlY powder and zirconia powder in a drying oven to dry for 5 hours at the temperature of 80 ℃;
(5) And spraying a bonding layer with the thickness of 50 mu m on the sandblasted area after sandblasting by adopting a plasma spraying method, and then spraying a zirconium oxide ceramic layer with the thickness of 100 mu m on the bonding layer by adopting the plasma spraying method, wherein the specific spraying parameters are shown in table 1.
TABLE 1 plasma spraying of ceramic materials Process parameters
The second embodiment:
(1) Selecting a lead-silver binary alloy (silver content is 0.6%) used as an anode plate, and calibrating the position of a liquid level line;
(2) Carefully wiping the surface of the anode plate with ethanol for 10 minutes, then washing with clear water, wiping the surface with acetone for 15 minutes, and washing with clear water;
(3) Defining the area range from the upper end of the anode plate to 5cm below a liquid level line as a spraying area, and carrying out sand blasting treatment on the spraying area; the pressure is 0.3MPa-0.5MPa when sand blasting is carried out, the included angle between the nozzle and the anode plate surface is 15-60 degrees, so as to avoid strong gravel from directly impacting the anode plate surface;
(4) Selecting Hastelloy C-276 powder as a spraying material, and drying the powder in an oven at 80 ℃ for 5 hours;
(5) A Hastelloy C-276 coating with the thickness of 150 mu m is sprayed on the sand blasting area after sand blasting treatment by adopting a plasma spraying method, and specific spraying parameters are shown in Table 2.
TABLE 2 plasma spraying of Ni-base alloy process parameters
The coating prepared by the process has good combination and compact surface, and can effectively prevent substances such as fluorinion, chloride ion and the like from corroding the anode plate exposed in the air in an acidic environment. However, from an electrochemical point of view, there is also a local region immersed in the acid electrolyte between the sprayed region and the liquid level line, which forms a weak galvanic cell, for example a hastelloy: the standard electrode potentials of nickel, cobalt and molybdenum are-0.241, -0.267 and-0.2 respectively, which are all smaller than the standard electrode potential of hydrogen, and the following reactions obviously occur from the thermodynamic point of view:
；
；
；
calculating the gibbs free energy of the reaction; according to Δ G = -nff; e = -0.2- (-0.126) = -0.074 (standard electrode potential for lead is-0.126), when n =2, F =96485.3385C/mol, Δ G =14279.83=14.3kj/mol >0, i.e. the reaction does not occur spontaneously from the point of view of gibbs free energy. Therefore, although a weak galvanic cell is formed in the area between the spraying area and the liquid level line, the coating is not corroded, namely, the method is reliable, and the anode plate can be well resistant to the corrosion of the sulfuric acid solution.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (5)
1. A preparation method of an anticorrosive coating on the surface of an electrolytic zinc anode plate is characterized by comprising the following steps: the method comprises the following steps:
(1) Selecting a lead-based alloy used as an anode plate, and calibrating the position of a liquid level line of the lead-based alloy;
(2) Carrying out decontamination and oil removal treatment on the surface of the anode plate;
(3) Defining a spraying area on the anode plate, and carrying out sand blasting treatment on the spraying area;
(4) Selecting a spraying material;
(5) Carrying out spraying treatment on the sand blasting area;
the spraying material in the step (1) is ceramic powder, metal alloy powder or duplex stainless steel;
the ceramic powder comprises alumina, zirconia or alumina zirconia mixed powder; the metal alloy powder comprises any one of nickel-based alloy powder, cobalt-based alloy powder, nickel-cobalt-based alloy powder, self-fluxing alloy powder, nickel-chromium carbide composite powder, lead-based alloy powder, copper-based alloy powder, nickel-chromium-molybdenum series and nickel-chromium-tungsten-molybdenum series;
when the spraying material is ceramic powder, firstly spraying a bonding layer on the surface of the anode plate after sand blasting treatment, and then spraying a ceramic layer on the bonding layer by adopting a thermal spraying method; wherein the thickness of the bonding layer is 10-1000 μm; the thickness of the ceramic layer is 10-1000 μm;
when the spraying material is metal alloy powder, directly spraying on the surface of the anode plate after sand blasting; the thickness of the coating is 10-1500 μm.
2. The method for preparing the surface anticorrosive coating of the electrolytic zinc anode plate according to claim 1, characterized in that: the lead-based alloy in the step (1) is a lead-silver binary alloy or a lead-based multi-element alloy.
3. The method for preparing the surface anticorrosive coating of the electrolytic zinc anode plate according to claim 1, characterized in that: the decontamination and oil removal treatment in the step (2) is specifically to wipe the surface of the anode plate by ethanol for 10 minutes, then to wash the anode plate by clear water, and then to wipe the surface of the anode plate by acetone for 15 minutes, and then to wash the anode plate by clear water.
4. The method for preparing the surface anticorrosive coating of the electrolytic zinc anode plate according to claim 1, characterized in that: and (4) the spraying area in the step (3) is the area range from the upper end of the anode plate to 5cm below a liquid level line.
5. The method for preparing the surface anticorrosive coating of the electrolytic zinc anode plate according to claim 1, characterized in that: the spraying method comprises any one of supersonic flame spraying, atmospheric plasma spraying, cold spraying, electric arc spraying and suspension spraying.
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| CN102212849B (en) * | 2011-04-22 | 2012-11-07 | 昆明理工恒达科技有限公司 | Method for preparing novel anode plate for electrodeposition of non-ferrous metal |
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