CN105040036B - A kind of preparation method of non-ferrous metal electrodeposition calendering anode - Google Patents
A kind of preparation method of non-ferrous metal electrodeposition calendering anode Download PDFInfo
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- CN105040036B CN105040036B CN201510336296.9A CN201510336296A CN105040036B CN 105040036 B CN105040036 B CN 105040036B CN 201510336296 A CN201510336296 A CN 201510336296A CN 105040036 B CN105040036 B CN 105040036B
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Abstract
The present invention relates to a kind of technology of preparing of non-ferrous metal electrodeposition with calendering anode, belong to non-ferrous metal field of hydrometallurgy.The present invention comprises the following steps：(1) using as cast condition lead-containing alloy as raw material, calendering pretreatment is carried out to taken raw material；Metal ingot casting, i.e., be placed in resistance furnace by the calendering pretreatment, is diffused annealing and/or rotten heat treatment；(2) roll, alloy is rolled by two rollers or four-high mill after will pre-processing；(3) Aging in electric field is handled, and will be rolled positive plate and is placed in Aging in electric field device and carries out Ageing Treatment.There is preferable mechanical property, decay resistance and chemical property using calendering anode produced by the present invention, the metal calendering anode of original technique can be replaced；Applied to non-ferrous metal electrodeposition process, tank voltage, reduction anode cost and the service life for extending anode of electrolytic process can be reduced.
Description
Technical field
The present invention relates to a kind of preparation method of non-ferrous metal electrodeposition with calendering anode, belong to non-ferrous metal hydrometallurgy neck
Domain.
Background technology
During the wet underwater welding of non-ferrous metal, electrodeposition process is important procedure.Lead-based anode is due to can be in height
Surface forms one layer of oxide film with satisfactory electrical conductivity under conditions of current density, high sulfuric acid concentration, by as not
Molten anode is widely used in hydrometallurgy electro-deposition industry.However, Pb based alloy anodes have the following disadvantages：1) overpotential for oxygen evolution
Height, causes a large amount of useless energy consumptions.By taking metal Zn as an example, the energy consumption of zinc hydrometallurgy electrodeposition process is about 3200kWh/t-Zn, is used
Lead silver alloy anode, the useless nearly 1000kWh/t-Zn of power consumption, accounts for the 30% of electrolytic deposition process energy consumption；Your 2) need that gold added in anode
Category silver so that anode cost is higher；3) lead based alloy anodes density is big, low intensity, flexible creep, reduce service life.
In order to overcome the shortcomings of that lead-based anode is present, the preparation technology to lead based alloy anodes is improved both at home and abroad,
Anode is prepared using the method for calendering.Because calender line can destroy the institutional framework of as cast condition metal, fine uniform is obtained
Crystal grain, reduce the segregation degree of secondary phase, while reducing the defect such as crack hole, in zinc electro-deposition industry, roll anode
Just gradually replace casting anode.It is existing calendering anodic process be：Metal liquid is poured into a mould, and blank flat is obtained after solidification, it
Rolling lead alloy plate, then obtains production board after smoothing, shearing, soldering polar ear afterwards.Existing process is disadvantageous in that：
1) because anode material surface forms the few crystal structure of consistent orientation, elongate form, number of grain boundaries in the rolling direction, cause
Anode material surface lacks corrosion centers, it is difficult to quick to form the excellent PbO of adhesion2Oxidation product protective layer.2) sun is rolled
Polar board surface is smooth, can not be sticked to well in anode plate face in electrolytic process Anodic mud, and majority comes off in the form of sheets so that
Fresh lead surface exposure is in the electrolytic solution, it is impossible to protects positive plate well, the life-span of positive plate is shortened, while also result in analysis
Go out the leaded height of zinc metal sheet, reduce product quality.3) structure of the blank flat before calendering is random larger, does not carry out well
Regulation and control, make the positive plate microstructure of the alloy obtained after calendering undesirable, it is possible to also result in the deterioration of Pb based alloys mechanical performance.Cause
This, prior art has yet to be improved and developed.
The content of the invention
Present invention aims in order to overcome the shortcoming that above-mentioned prior art is present, prepare to provide a kind of with preferably electricity
The non-ferrous metal electrodeposition Novel anode of catalytic activity, mechanical performance and decay resistance.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；Comprise the steps：
Step one
Using as cast condition lead-containing alloy as raw material, calendering pretreatment is carried out to taken raw material, obtains rolling spare test piece, the pressure
Prolonging preprocessing process includes at least one of diffusion annealing and rotten heat treatment；
The temperature of the diffusion annealing is 280~320 DEG C, is preferably 290-310 DEG C, is more preferably 300 DEG C；
The temperature of the rotten heat treatment is 180~260 DEG C, is preferably 200-240 DEG C, is more preferably 220-230
℃；
Step 2
Calendering spare test piece obtained by step one is rolled；The preform being sized.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；Obtain after preform, can be used directly, be
Further lifting quality, can carry out Aging in electric field processing to preform obtained by step 2, obtain finished product；The Aging in electric field
During processing, control temperature for 80~120 DEG C, be preferably 90-110 DEG C, more preferably 100-105 DEG C, electric-field intensity be 1~
8kV/cm, preferably 3~6kV/cm, more preferably 4~5kV/cm.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；Diffusion annealing described in step one is：
Under protective atmosphere, in 280~320 DEG C, preferably 290-310 DEG C, more preferably 300 DEG C are incubated 30~60min, are preferably
With 3~10 DEG C/min, preferably 5-8 DEG C/min, more preferably 6 DEG C/min after 40-50min, more preferably 45min
Speed be cooled to room temperature, be stored at room temperature 1~2h.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；Go bad heat treatment condition described in step one
For：Under protective atmosphere, in 180~260 DEG C of temperature, preferably 200-240 DEG C, more preferably 220-230 DEG C, insulation 30
~45min, preferably 30-40min, more preferably 35min；Cool to room temperature after insulation with the furnace.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；When handling preform Aging in electric field, control
Time processed is 40~90min, is preferably 50-80min, is more preferably 60-70min.
A kind of preparation method of present invention non-ferrous metal electrodeposition calendering anode；Comprise the steps：
Step A
Using as cast condition lead-containing alloy as raw material, calendering pretreatment is carried out to taken raw material, obtains rolling spare test piece, the pressure
It is first progress diffusion annealing processing to prolong preprocessing process, then carries out rotten heat treatment；
The diffusion annealing is：Under protective atmosphere, in 280~320 DEG C, be preferably 290-310 DEG C, more preferably
300℃；30~60min of lower insulation, be preferably 40-50min, more preferably after 45min with 3~10 DEG C/min,
Preferably 5-8 DEG C/min, more preferably 6 DEG C/min speed be cooled to room temperature, be stored at room temperature 1~2h,
It is described it is rotten heat treatment be：Under protective atmosphere, the sample after diffusion annealing is handled be heated to 180~260 DEG C,
Preferably 200-240 DEG C, more preferably 220-230 DEG C, insulation 30~45min, be preferably 30-40min, further preferably
To cool to room temperature with the furnace after 35min；
Step B
Calendering spare test piece obtained by step one is rolled；The preform being sized；
Step C
Aging in electric field processing is carried out to preform obtained by step 2, finished product is obtained；During the Aging in electric field processing, control temperature
Spend for 80~120 DEG C, preferably 90-110 DEG C, more preferably 100-105 DEG C, electric-field intensity is 1~8kV/cm, is preferably
3~6kV/cm, more preferably 4~5kV/cm, control time are 40~90min, are preferably 50-80min, further preferably
For 60-70min.
In the present invention, the protective atmosphere is inert gas, such as argon gas and nitrogen.
Principle and advantage
(1) by increasing the process step of diffusion annealing in pre-processing before calendering, the diffusion of alloying element, regulation and control are promoted
Alloying element reduces grain boundary density in the distribution proportion of crystal boundary/intra-die, and then reduces active high secondary after calendering
In crystal boundary and branch grain boundary area segregation, more preferably alloy mechanical property and decay resistance are resulted in；
(2) by increasing rotten heat treatment in pre-processing before calendering the step of, change crystal boundary and constitute and be orientated, improve
CSL crystal boundary ratios, destroy complete crystal boundary and dendrite circle network, so as to reduce the branch grain boundary width after calendering, suppress intergranular
Corrosion, so as to improve the decay resistance of alloy；
(3) Aging in electric field after rolling is the step of handle, can refining alloy crystal grain, separate out in regulation calender line
The distribution of second phase particles, increases the density in room, more reaction sites is provided for electrochemical reaction, so as to improve the electricity of alloy
Chemical property.
In a word, the present invention (is especially first passed through suitable before calendering under the synergy of each workshop section and technological parameter
When parameter diffusion annealing handle, then by the rotten heat treatment of suitable parameter), achieve unexpected effect, significantly
The electro catalytic activity for improving positive plate, mechanical performance and decay resistance.
Embodiment
Embodiment 1
In the present embodiment, the lead-silver alloy is by percentage to the quality；Pb=99.5%；Ag=0.5%；
(1) lead-silver alloy is cast in resistance furnace according to a conventional method；
(2) lead for obtaining step (1)-silver alloy ingot casting is placed in resistance furnace, carries out calendering pretreatment, process conditions
For：Under argon atmosphere, 30min is incubated at 300 DEG C, room temperature is cooled to 3 DEG C/min speed, 2h is stood；Heating
To 240 DEG C, 45min is incubated, room temperature is naturally cooled to；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 80 DEG C during electric field
Imitate 40min, electric-field intensity 2KV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 40 DEG C of temperature) application, with traditional pb-ag alloy
Positive plate is compared, and (tensile strength of finished product is obtained by the embodiment for the mechanical strength raising 25% of the alloy anode
23.15MPa), tank voltage reduction by 10% (tank voltage of finished product obtained by the embodiment is 1.64V), rate of corrosion reduces by 17% (reality
The corrosion efficiency for applying finished product obtained by example is 3.32g/m2·h)。
Comparative example 1
In this comparative example, the component of lead-silver alloy used and the content of each component are completely consistent with embodiment 1；
Its preparation process is：
(1) lead-silver alloy is cast in resistance furnace according to a conventional method；
(2) lead for obtaining step (1)-silver alloy ingot casting is placed in resistance furnace, carries out calendering pretreatment, process conditions
For：Under argon atmosphere, 30min is incubated at 200 DEG C, be cooled to 3 DEG C/min speed after room temperature be immediately heated to
240 DEG C, 45min is incubated, room temperature is naturally cooled to；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device Aging in electric field at room temperature
40min, electric-field intensity 2kV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 40 DEG C of temperature) application, the tension of the alloy anode
Intensity is that 17.60MPa, its tank voltage are 1.83V, and corrosion efficiency is 3.96g/m2·h。
By embodiment 1 and comparative example 1 as can be seen that when diffusion annealing is handled and gone bad at heat treatment and Aging in electric field
When the parameter of reason is not in the range of the present invention is limited, the property of its gained finished product is well below the present invention.
Embodiment 2
In the present embodiment, the lead-silver alloy is by percentage to the quality；Pb=99.6%；Ag=0.4%；
(1) lead-silver alloy is cast in resistance furnace according to a conventional method；
(2) the lead-containing alloy ingot casting for obtaining step (1) is placed in resistance furnace, carries out calendering pretreatment, and process conditions are：
Under argon atmosphere, 30min is incubated at 320 DEG C, room temperature is cooled to 10 DEG C/min speed, 2h is stood；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 100 DEG C during electric field
Imitate 60min, electric-field intensity 4KV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 30 DEG C of temperature) application, with traditional pb-ag alloy
Positive plate is compared, and (tensile strength of finished product is obtained by the embodiment for the mechanical strength raising 40% of the alloy anode
26.04MPa), tank voltage reduction by 15% (tank voltage of finished product obtained by the embodiment is 1.55V), the basically identical (reality of rate of corrosion
The corrosion efficiency for applying finished product obtained by example is 4.02g/m2·h)。
Comparative example 2
In this comparative example, the component of lead-silver alloy used and the content of each component are completely consistent with embodiment 2；
Its preparation process is：
(1) lead-silver alloy is cast in resistance furnace according to a conventional method；
(2) lead for obtaining step (1)-silver alloy ingot casting is placed in resistance furnace, carries out calendering pretreatment, process conditions
For：Under argon atmosphere, 30min is incubated at 160 DEG C, is cooled to 3 DEG C/min speed after room temperature immediately by two
Roller or four-high mill are rolled, and obtain finished product；
(3) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 40 DEG C of temperature) application, the tension of the alloy anode
Intensity is that 17.42MPa, its tank voltage are 1.84V, and corrosion efficiency is 4.24g/m2·h。
By embodiment 2 and comparative example 2 as can be seen that when the parameter that diffusion annealing is handled does not limit scope in the present invention
It is interior and save Aging in electric field processing when, its gained finished product property well below the present invention.
Embodiment 3
In the present embodiment, the lead-silver-rare earth alloy is by percentage to the quality；Pb=99.5%, Ag=0.4%, rare earth
=0.1%；
(1) under nitrogen protection atmosphere, the molten lead liquid in electromagnetic oven adds lead rare earth foundry alloy and argent, obtained
Lead-silver-rare earth alloy；
(2) the lead-containing alloy ingot casting for obtaining step (1) is placed in resistance furnace, carries out calendering pretreatment, and process conditions are：
Under nitrogen protection atmosphere, 60min is incubated at 280 DEG C, room temperature is cooled to 10 DEG C/min speed, 1h is stood；It is heated to 260
DEG C, 30min is incubated, room temperature is naturally cooled to；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 100 DEG C during electric field
Imitate 60min, electric-field intensity 8KV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 30 DEG C of temperature) application, with traditional pb-ag alloy
Positive plate is compared, and (tensile strength of finished product is obtained by the embodiment for the mechanical strength raising 30% of the alloy anode
23.92MPa), tank voltage reduction by 12% (tank voltage of finished product obtained by the embodiment is 1.60V), rate of corrosion reduces by 36% (reality
The corrosion efficiency for applying finished product obtained by example is 2.56g/m2·h)。
Comparative example 3
In this comparative example, the component of lead-silver-rare earth alloy used and the content of each component are completely consistent with embodiment 3；
Its preparation process is：
(1) under nitrogen protection atmosphere, the molten lead liquid in electromagnetic oven adds lead rare earth foundry alloy and argent, obtained
Lead-silver-rare earth alloy；
(2) the lead-containing alloy ingot casting for obtaining step (1) is placed in resistance furnace, carries out calendering pretreatment, and process conditions are：
Under nitrogen protection atmosphere, 60min is incubated at 360 DEG C, room temperature is cooled to 15 DEG C/min speed, is heated to after standing 1h
360 DEG C, 1h is incubated, room temperature is cooled to 15 DEG C/min speed；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 150 DEG C during electric field
Imitate 30min, electric-field intensity 10KV/cm.
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 30 DEG C of temperature) application, the tension of the alloy anode
Intensity is that 18.40MPa, its tank voltage are 1.77V, and corrosion efficiency is 3.55g/m2·h。
It can be seen that from embodiment 3 and comparative example 3：When diffusion annealing processing, the speed of cooling, rotten heat treatment, electric field
The maximum that the parameters such as the temperature of timeliness, the electric-field intensity of Aging in electric field are limited beyond the present invention, this causes its gained finished product
Property is well below the present invention.
Embodiment 4
In the present embodiment, the lead-silver-rare earth alloy is by percentage to the quality；Pb=99.2%, Ag=0.5%, rare earth
=0.3%；
(1) under nitrogen protection atmosphere, the molten lead liquid in electromagnetic oven adds the silver-colored foundry alloy of lead, and lead rare earth foundry alloy is obtained
To lead-silver-rare earth alloy；
(2) the lead-containing alloy ingot casting for obtaining step (1) is placed in resistance furnace, carries out calendering pretreatment, and process conditions are：
Under argon atmosphere, 60min is incubated at 320 DEG C, room temperature is cooled to 5 DEG C/min speed, 1h is stood；It is heated to
180 DEG C, 30min is incubated, room temperature is naturally cooled to；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 120 DEG C during electric field
Imitate 90min, electric-field intensity 6KV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 30 DEG C of temperature) application, with traditional pb-ag alloy
Positive plate is compared, and (tensile strength of finished product is obtained by the embodiment for the mechanical strength raising 22% of the alloy anode
22.45MPa), tank voltage reduction by 14% (tank voltage of finished product obtained by the embodiment is 1.57V), rate of corrosion reduces by 35% (reality
The corrosion efficiency for applying finished product obtained by example is 2.60g/m2·h)。
Comparative example 4
In this comparative example, the component of lead-silver-rare earth alloy used and the content of each component are completely consistent with embodiment 4；
Its preparation process is：
(1) under nitrogen protection atmosphere, the molten lead liquid in electromagnetic oven adds the silver-colored foundry alloy of lead, and lead rare earth foundry alloy is obtained
To lead-silver-rare earth alloy；
(2) the lead-containing alloy ingot casting for obtaining step (1) is placed in resistance furnace, carries out calendering pretreatment, and process conditions are：
Under argon atmosphere, 20min is incubated at 250 DEG C, room temperature is cooled to 1 DEG C/min speed, 0.5h is stood；It is heated to
170 DEG C, 20min is incubated, room temperature is naturally cooled to；
(3) roll：The alloy that step (2) is obtained is rolled by two rollers or four-high mill；
(4) Aging in electric field is handled：The positive plate that step (3) is obtained is placed in Aging in electric field device, at 50 DEG C during electric field
Imitate 30min, electric-field intensity 0.5KV/cm.,
(5) (the Zn in Zinc electrolysis system2+50g/L, H2SO4160g/L, 30 DEG C of temperature) application, the tension of the alloy anode
Intensity is that 18.22MPa, its tank voltage are 1.79V, and corrosion efficiency is 3.96g/m2·h。
It can be seen that from embodiment 4 and comparative example 4：When diffusion annealing processing, the speed of cooling, rotten heat treatment, electric field
The parameters such as the temperature of timeliness, the electric-field intensity of Aging in electric field are less than the minimum value that the present invention is limited, and this causes its gained finished product
Property is well below the present invention.
Claims (10)
1. a kind of non-ferrous metal electrodeposition preparation method of calendering anode, it is characterised in that comprise the steps：
Step one
Using as cast condition lead-containing alloy as raw material, calendering pretreatment is carried out to taken raw material, obtains rolling spare test piece, the calendering is pre-
Processing procedure includes at least one of diffusion annealing and rotten heat treatment；
The temperature of the diffusion annealing is 280 ~ 320 DEG C；
The temperature of the rotten heat treatment is 180 ~ 260 DEG C；
Step 2
Calendering spare test piece obtained by step one is rolled；The preform being sized.
2. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 1, it is characterised in that：
Aging in electric field processing is carried out to preform obtained by step 2, finished product is obtained；During Aging in electric field processing, the temperature is controlled to be
80~120 DEG C, electric-field intensity is 1 ~ 8kV/cm.
3. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 1, it is characterised in that；Step
Diffusion annealing described in one is：Under protective atmosphere, it is incubated in 280 ~ 320 DEG C cold with 3 ~ 10 DEG C/min speed after 30 ~ 60min
But to room temperature.
4. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 3, it is characterised in that；It is described
Diffusion annealing is：Under protective atmosphere, it is incubated in 290-310 DEG C after 40-50min and room temperature is cooled to 5-8 DEG C/min speed.
5. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 1, it is characterised in that；Step
The condition of rotten heat treatment is described in one：Under protective atmosphere, in 180 ~ 260 DEG C of temperature；30 ~ 45min of soaking time；Insulation
After cool to room temperature with the furnace.
6. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 5, it is characterised in that；It is described
The condition of rotten heat treatment is：Under protective atmosphere, room temperature is cooled to the furnace after being incubated 30-40min in 200-240 DEG C.
7. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 2, it is characterised in that：Electric field
During Ageing Treatment, to control temperature be 80~120 DEG C, control time is 40~90min, controls electric-field intensity to be 1 ~ 8kV/cm.
8. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 7, it is characterised in that：Electric field
During Ageing Treatment, to control temperature be 90-110 DEG C, control time is 50-80min, controls electric-field intensity to be 3 ~ 6kV/cm.
9. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 8, it is characterised in that：Electric field
During Ageing Treatment, to control temperature be 100-105 DEG C, control time is 60-70min, controls electric-field intensity to be 4 ~ 5kV/cm.
10. a kind of preparation method of non-ferrous metal electrodeposition calendering anode according to claim 1, it is characterised in that including
Following step：
Step A
Using as cast condition lead-containing alloy as raw material, calendering pretreatment is carried out to taken raw material, obtains rolling spare test piece, the calendering is pre-
Processing procedure is first progress diffusion annealing processing, then carries out rotten heat treatment；
The diffusion annealing is：Room temperature is cooled to 3 ~ 10 DEG C/min speed after being incubated 30 ~ 60min at 280 ~ 320 DEG C,
1 ~ 2h is stored at room temperature, the sample after diffusion annealing processing is obtained；
It is described it is rotten heat treatment be：Sample after diffusion annealing is handled is heated to after 180 ~ 260 DEG C of 30 ~ 45min of insulation with stove
It is cooled to room temperature；
Step B
Calendering spare test piece obtained by step A is rolled；The preform being sized；
Step C
Aging in electric field processing is carried out to preform obtained by step B, finished product is obtained；During Aging in electric field processing, the temperature is controlled to be
80~120 DEG C, electric-field intensity be 1 ~ 8kV/cm, time be 40~90min.
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| CN111005040A (en) * | 2019-12-13 | 2020-04-14 | 陕西易莱德新材料科技有限公司 | Preparation method of aluminum-based anode plate for non-ferrous metal electrodeposition |
| CN110938840A (en) * | 2019-12-13 | 2020-03-31 | 陕西易莱德新材料科技有限公司 | Preparation method of lead-based anode plate for non-ferrous metal electrodeposition |
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