CN110938840A - Preparation method of lead-based anode plate for non-ferrous metal electrodeposition - Google Patents
Preparation method of lead-based anode plate for non-ferrous metal electrodeposition Download PDFInfo
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- CN110938840A CN110938840A CN201911284805.2A CN201911284805A CN110938840A CN 110938840 A CN110938840 A CN 110938840A CN 201911284805 A CN201911284805 A CN 201911284805A CN 110938840 A CN110938840 A CN 110938840A
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/02—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D19/00—Casting in, on, or around objects which form part of the product
- B22D19/16—Casting in, on, or around objects which form part of the product for making compound objects cast of two or more different metals, e.g. for making rolls for rolling mills
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/12—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of lead or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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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
-
- 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
- C23C4/126—Detonation spraying
-
- 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
- C25D3/30—Electroplating: Baths therefor from solutions of tin
Abstract
The invention discloses a preparation method of a lead-based anode plate for non-ferrous metal electrodeposition, belonging to the field of non-ferrous metal hydrometallurgy. The invention comprises the following steps: (1) taking as-cast lead-based alloy as a raw material, and carrying out calendering pretreatment on the taken raw material; the rolling pretreatment is that the lead alloy cast ingot is placed in a resistance furnace to carry out diffusion annealing and/or modification heat treatment; (2) calendering, namely calendering the pretreated alloy by a two-roller or four-roller rolling mill; (3) and (4) electric field aging treatment, namely placing the rolled anode plate in an electric field aging device for aging treatment. The rolled anode prepared by the method has better mechanical property, corrosion resistance and electrochemical property, and can replace the lead alloy rolled anode in the prior art; the method is applied to the non-ferrous metal electrodeposition process, can reduce the bath voltage in the electrolytic process, reduce the anode cost and prolong the service life of the anode.
Description
Technical Field
The invention belongs to the technical field of metal electrodes, and relates to a preparation method of a lead-based anode plate for non-ferrous metal electrodeposition.
Background
In the wet extraction process of nonferrous metals, the electrodeposition process is an important process. The lead-based anode can form a layer of oxide protective film with good conductivity on the surface under the conditions of high current density and high sulfuric acid concentration, and is widely applied to the hydrometallurgy electrodeposition industry as an insoluble anode. However, Pb-based alloy anodes have the following disadvantages: 1) the oxygen evolution overpotential is high, resulting in a large amount of useless energy consumption. Taking metal Zn as an example, the energy consumption of the zinc hydrometallurgy electrowinning process is about 3200kWh/t-Zn, and the lead-silver alloy anode is adopted, so that the useless electricity consumption is about 1000kWh/t-Zn, which accounts for about 30% of the energy consumption in the electrowinning process; 2) noble metal silver needs to be added into the anode, so that the cost of the anode is high; 3) the lead-based alloy anode has high density, low strength and easy bending and creeping, and reduces the service life.
In order to overcome the defects of the lead-based anode, the preparation process of the lead-based alloy anode is improved at home and abroad, and the anode is prepared by adopting a calendering method. The texture structure of the as-cast lead alloy can be destroyed in the rolling process, fine and uniform crystal grains are obtained, the segregation degree of secondary phases is reduced, and the defects of cracks, holes and the like are reduced. The existing anode calendering process comprises the following steps: and pouring the lead alloy liquid, solidifying to obtain a blank plate, rolling to obtain a lead alloy plate, leveling, shearing and welding the lugs to obtain a finished plate. The prior art has the following defects: 1) because the surface of the anode material forms a crystal structure with consistent orientation, slender shape and less crystal boundary number in the rolling direction, the surface of the anode material lacks a corrosion center and is difficult to quickly form an oxidation product protective layer with excellent binding force. 2) The surface of the rolled anode plate is smooth, anode mud can not be well adhered to the surface of the anode plate in the electrolysis process, and most of the anode mud is flaky and falls off, so that the surface of fresh lead is exposed in electrolyte, the anode plate can not be well protected, the service life of the anode plate is shortened, and meanwhile, the separated zinc sheet is high in lead content, and the product quality is reduced. 3) The randomness of the metallographic structure of the blank plate before rolling is large, and the metallographic structure of the blank plate is not well regulated, so that the metallographic phase of the anode plate alloy obtained after rolling is not ideal, and the mechanical property of the Pb-based alloy can be possibly deteriorated. Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The invention aims to provide a preparation method of a lead-based anode plate for non-ferrous metal electrodeposition, which solves the problem that the metallographic phase of an anode plate alloy obtained after rolling is not ideal in the prior art.
The invention adopts the technical scheme that the preparation method of the lead-based anode plate for the non-ferrous metal electrodeposition is implemented according to the following steps:
step 1, lead substrate pretreatment: quenching the lead matrix material for 3-5 hours at 200-350 ℃, and then performing surface increasing treatment and oil removal on the surface;
step 2, tinning: tin plating lead on the base material;
step 3, casting a lead alloy layer: placing the substrate processed in the step 2 in a preheated cast steel vertical die, and pouring the molten lead alloy liquid into a die to obtain a blank plate;
and 4, extruding or exploding and spraying active particles: rolling the blank plate obtained in the step 3, and then embedding active solid particles through extrusion or explosion spraying to obtain a metal-based ceramic composite anode plate;
step 5, rolling the metal-based ceramic composite anode plate obtained in the step 4 to obtain a preformed product with a set size;
and 6, carrying out electric field aging treatment on the preformed product obtained in the step 5 to obtain a finished product.
The invention is also characterized in that:
in the step 4, the active solid particles are WC, SiC and B4C. Or Si4N4One or more of the particles.
The plating solution in the step 2 consists of 85-100 g/L sodium stannate, 10-15 g/L sodium hydroxide, 5-15 g/L sodium acetate and 0-1.5 g/L additive gelatin.
The process conditions of the step 2 are as follows: the current density is 2-3A/dm2(ii) a The temperature is 55-70 ℃; the electroplating time is 10-50 min.
In the step 3, the lead alloy is the existing lead-silver binary alloy or one of lead-silver-calcium, lead-tin-calcium and lead-antimony-tin binary alloy.
And 6, performing electric field aging treatment, wherein the temperature is controlled to be 60-100 ℃, the electric field intensity is 2-9 kV/cm, and the time is 40-90 min.
And 4, the diameter of the active particles is 20-1000 mu m.
The invention has the beneficial effects that:
1. the composite anode material is prepared by taking a lead plate as a base material and adopting a method combining casting, rolling, extruding or explosive spraying, and the obtained composite anode plate is formed by reinforcing and compounding a layer and active solid particles; the outside of the lead base material is sequentially provided with a tin plating layer, a lead-based alloy layer and an active solid particle layer from inside to outside.
2. The composite anode plate adopts a rolling method, which does not require that the alloy has enough low melting point and good fluidity after being melted, thereby greatly reducing the porosity of the anode plate and prolonging the service life of the anode plate; and the aluminum plate and the lead alloy both have better ductility, and the defect that local bonding between the aluminum plate and the lead alloy is weak is overcome.
3. The composite anode plate of the invention introduces active particles WC and B on the surface of the electrode on the basis of the prior art4C and Si4N4The particles have strong acid and alkali corrosion resistance, and the prepared anode has the advantage of long service life in a strong acid solution compared with the traditional anode.
4. The composite anode prepared by the invention is used in the colored electrodeposition process, has good conductivity and high stability, solves the deformation problem existing when the known lead alloy is simply used as the outer layer, and simultaneously the novel metal-based ceramic composite anode contains the conductive WC particles with excellent electrocatalytic activity and the nano ceramic particles B with acid and alkali resistance, oxidation and reduction resistance, good thermal stability, high-temperature oxidation resistance and mechanical strength in a plating layer4C, they can not only catalyze the oxygen discharge, but also make the cell voltage low after the electrode is used in the electrolysis of large current for a long time.
5. The metal-based ceramic composite anode prepared by the invention has simple preparation method and low electrode price, and can replace the lead anode of the prior art; the method is applied to the electrodeposition process of nonferrous metals such as copper, zinc, nickel, manganese and the like, can obviously reduce the cell voltage in the electrolysis process, reduce the cost of the anode plate, improve the cathode current efficiency and prolong the service life of the anode plate.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
The invention adopts the technical scheme that the preparation method of the lead-based anode plate for the non-ferrous metal electrodeposition is implemented according to the following steps:
step 1, lead substrate pretreatment: quenching the lead matrix material for 3 hours at the temperature of 200 ℃, and then performing surface increasing treatment and oil removal on the surface;
step 2, tinning: tin plating lead on the base material;
step 3, casting a lead alloy layer: placing the substrate processed in the step 2 in a preheated cast steel vertical die, and pouring the molten lead alloy liquid into a die to obtain a blank plate;
and 4, extruding or exploding and spraying active particles: rolling the blank plate obtained in the step 3, and then embedding active solid particles through extrusion or explosion spraying to obtain a metal-based ceramic composite anode plate;
step 5, rolling the metal-based ceramic composite anode plate obtained in the step 4 to obtain a preformed product with a set size;
and 6, carrying out electric field aging treatment on the preformed product obtained in the step 5 to obtain a finished product.
The active solid particles in the step 4 are B4C。
In the step 2, the plating solution consists of 85g/L sodium stannate, 10g/L sodium hydroxide, 5g/L sodium acetate and 0g/L additive gelatin.
The process conditions of the step 2 are as follows: current density 2A/dm2(ii) a The temperature is 55 ℃; the electroplating time is 10 min.
And 3, the lead alloy is lead-tin-calcium.
And 6, performing electric field aging treatment, wherein the temperature is controlled to be 60 ℃, the electric field intensity is 9kV/cm, and the time is 90 min.
Step 4 the active particles have a diameter size of 20 μm.
Example 2
The invention adopts the technical scheme that the preparation method of the lead-based anode plate for the non-ferrous metal electrodeposition is implemented according to the following steps:
step 1, lead substrate pretreatment: quenching the lead matrix material for 4 hours at 300 ℃, and then performing surface increasing treatment and oil removal on the surface;
step 2, tinning: tin plating lead on the base material;
step 3, casting a lead alloy layer: placing the substrate processed in the step 2 in a preheated cast steel vertical die, and pouring the molten lead alloy liquid into a die to obtain a blank plate;
and 4, extruding or exploding and spraying active particles: rolling the blank plate obtained in the step 3, and then embedding active solid particles through extrusion or explosion spraying to obtain a metal-based ceramic composite anode plate;
step 5, rolling the metal-based ceramic composite anode plate obtained in the step 4 to obtain a preformed product with a set size;
and 6, carrying out electric field aging treatment on the preformed product obtained in the step 5 to obtain a finished product.
The active solid particles in the step 4 are B4C、Si4N4Particles.
In the step 2, the plating solution consists of 90g/L sodium stannate, 12g/L sodium hydroxide, 8g/L sodium acetate and 0.7g/L additive gelatin.
The process conditions of the step 2 are as follows: current density 2.3A/dm2(ii) a The temperature is 60 ℃; the electroplating time is 30 min.
In the step 3, the lead alloy is the existing lead-silver binary alloy or one of lead-silver-calcium, lead-tin-calcium and lead-antimony-tin binary alloy.
And 6, carrying out electric field aging treatment, wherein the temperature is controlled to be 8 ℃, the electric field intensity is 5kV/cm, and the time is 60 min.
Step 4 the active particles have a diameter size of 700 μm.
Example 3
The invention adopts the technical scheme that the preparation method of the lead-based anode plate for the non-ferrous metal electrodeposition is implemented according to the following steps:
step 1, lead substrate pretreatment: quenching the lead matrix material for 5 hours at 350 ℃, and then performing surface increasing treatment and oil removal on the surface;
step 2, tinning: tin plating lead on the base material;
step 3, casting a lead alloy layer: placing the substrate processed in the step 2 in a preheated cast steel vertical die, and pouring the molten lead alloy liquid into a die to obtain a blank plate;
and 4, extruding or exploding and spraying active particles: rolling the blank plate obtained in the step 3, and then embedding active solid particles through extrusion or explosion spraying to obtain a metal-based ceramic composite anode plate;
step 5, rolling the metal-based ceramic composite anode plate obtained in the step 4 to obtain a preformed product with a set size;
and 6, carrying out electric field aging treatment on the preformed product obtained in the step 5 to obtain a finished product.
In step 4, the active solid particles are WC.
In the step 2, the plating solution consists of 100g/L sodium stannate, 15g/L sodium hydroxide, 15g/L sodium acetate and 1.5g/L additive gelatin.
The process conditions of the step 2 are as follows: current density 3A/dm2(ii) a The temperature is 70 ℃; the electroplating time is 50 min.
The lead alloy in the step 3 is the existing lead-silver binary alloy.
And 6, performing electric field aging treatment, wherein the temperature is controlled to be 100 ℃, the electric field intensity is 9kV/cm, and the time is 40-90 min.
Step 4 the active particles have a diameter size of 1000 μm.
Claims (7)
1. A preparation method of a lead-based anode plate for non-ferrous metal electrodeposition is characterized by comprising the following steps:
step 1, lead substrate pretreatment: quenching the lead matrix material for 3-5 hours at 200-350 ℃, and then performing surface increasing treatment and oil removal on the surface;
step 2, tinning: tin plating lead on the base material;
step 3, casting a lead alloy layer: placing the substrate processed in the step 2 in a preheated cast steel vertical die, and pouring the molten lead alloy liquid into a die to obtain a blank plate;
and 4, extruding or exploding and spraying active particles: rolling the blank plate obtained in the step 3, and then embedding active solid particles through extrusion or explosion spraying to obtain a metal-based ceramic composite anode plate;
step 5, rolling the metal-based ceramic composite anode plate obtained in the step 4 to obtain a preformed product with a set size;
and 6, carrying out electric field aging treatment on the preformed product obtained in the step 5 to obtain a finished product.
2. The method for preparing a lead-based anode plate for non-ferrous metal electrodeposition as claimed in claim 1, wherein the active solid particles in the step 4 are WC, SiC and B4C. Or Si4N4One or more of the particles.
3. The method for preparing the lead-based anode plate for the electrodeposition of nonferrous metals according to claim 1, wherein the plating solution in the step 2 comprises 85-100 g/L of sodium stannate, 10-15 g/L of sodium hydroxide, 5-15 g/L of sodium acetate and 0-1.5 g/L of gelatin as an additive.
4. The method for preparing the lead-based anode plate for the non-ferrous metal electrodeposition as claimed in claim 1, wherein the process conditions in the step 2 are as follows: the current density is 2-3A/dm2(ii) a The temperature is 55-70 ℃; the electroplating time is 10-50 min.
5. The method for preparing the lead-based anode plate for the non-ferrous metal electrodeposition as claimed in claim 1, wherein the lead alloy in the step 3 is one of the existing lead-silver binary alloy or lead-silver-calcium, lead-tin-calcium and lead-antimony-tin binary alloy.
6. The method for preparing a lead-based anode plate for non-ferrous metal electrodeposition according to claim 1, wherein in the step 6, during the electric field aging treatment, the temperature is controlled to be 60-100 ℃, the electric field intensity is 2-9 kV/cm, and the time is 40-90 min.
7. The method for preparing a lead-based anode plate for non-ferrous metal electrodeposition according to claim 1, wherein the diameter of the active particles in the step 4 is 20-1000 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911284805.2A CN110938840A (en) | 2019-12-13 | 2019-12-13 | Preparation method of lead-based anode plate for non-ferrous metal electrodeposition |
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| CN201911284805.2A CN110938840A (en) | 2019-12-13 | 2019-12-13 | Preparation method of lead-based anode plate for non-ferrous metal electrodeposition |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150348A (en) * | 2021-12-08 | 2022-03-08 | 昆明理工恒达科技股份有限公司 | WC particle reinforced low-silver-lead alloy composite anode plate for non-ferrous metal electrodeposition and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212849A (en) * | 2011-04-22 | 2011-10-12 | 昆明理工恒达科技有限公司 | Method for preparing novel anode plate for electrodeposition of non-ferrous metal |
| CN104372267A (en) * | 2014-10-24 | 2015-02-25 | 陈帆 | Method for processing 2A17 aluminum alloy plate |
| CN105040036A (en) * | 2015-06-17 | 2015-11-11 | 中南大学 | Preparation method of calendering anode for non-ferrous metal eletrodeposition |
-
2019
- 2019-12-13 CN CN201911284805.2A patent/CN110938840A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212849A (en) * | 2011-04-22 | 2011-10-12 | 昆明理工恒达科技有限公司 | Method for preparing novel anode plate for electrodeposition of non-ferrous metal |
| CN104372267A (en) * | 2014-10-24 | 2015-02-25 | 陈帆 | Method for processing 2A17 aluminum alloy plate |
| CN105040036A (en) * | 2015-06-17 | 2015-11-11 | 中南大学 | Preparation method of calendering anode for non-ferrous metal eletrodeposition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150348A (en) * | 2021-12-08 | 2022-03-08 | 昆明理工恒达科技股份有限公司 | WC particle reinforced low-silver-lead alloy composite anode plate for non-ferrous metal electrodeposition and preparation method |
| CN114150348B (en) * | 2021-12-08 | 2024-03-12 | 昆明理工恒达科技股份有限公司 | WC particle reinforced low-silver lead alloy composite anode plate for nonferrous metal electrodeposition and preparation method |
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