CN105040036A - Preparation method of calendering anode for non-ferrous metal eletrodeposition - Google Patents
Preparation method of calendering anode for non-ferrous metal eletrodeposition Download PDFInfo
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Abstract
The invention relates to a preparation technology of a calendering anode for non-ferrous metal eletrodeposition and belongs to the field of non-ferrous metal hydrometallurgy. The technology includes the following steps that firstly, cast lead-base alloy serve as raw materials, and calendering pre-processing is performed on the taken raw materials; and according to the calendering pre-processing, lead allot cast ingots are placed in a resistance furnace and subjected to dispersion annealing and/or deterioration heat treatment; secondly, calendering is performed, and in other words, calendering is performed on the preprocessed alloy through a two-roller or four-roller rolling machine; and thirdly, electric field aging treatment is performed, and in other words, a calendering anode plate is placed in an electric field aging device to be subjected to aging treatment. The calendering anode prepared through the technology has good mechanical performance, corrosion resistance and electrochemical performance and can replace a lead alloy calendering anode prepared through an existing technology; and the calendering anode is applied to a non-ferrous metal eletrodeposition procedure and can reduce cell voltage in the electrolysis process and reduce the cost of the anode, and the service life of the anode can be prolonged.
Description
Technical field
The present invention relates to the preparation method of a kind of non-ferrous metal electrodeposition calendering anode, belong to non-ferrous metal field of hydrometallurgy.
Background technology
In the wet underwater welding process of non-ferrous metal, electrodeposition process is important procedure.Lead-based anode, owing to can form at the condition lower surface of high current density, high sulfuric acid concentration the oxide film that one deck has satisfactory electrical conductivity, is widely used in hydrometallurgy galvanic deposit industry as insoluble anode.But Pb base alloy anode exists following shortcoming: 1) overpotential for oxygen evolution is high, cause a large amount of useless energy consumption.For Metal Zn, the energy consumption of zinc hydrometallurgy electrodeposition operation is about 3200kWh/t-Zn, and adopt lead silver alloy anode, the nearly 1000kWh/t-Zn of useless power consumption, accounts for 30% of electrolytic deposition process energy consumption; 2) need in anode to add noble silver, make anode cost higher; 3) lead based alloy anodes density is large, intensity is low, flexible creep, reduces work-ing life.
In order to overcome the deficiency that lead-based anode exists, both at home and abroad the preparation technology of lead based alloy anodes being improved, adopting the method for calendering to prepare anode.Because calender line can destroy the weave construction of as cast condition lead alloy, obtain the crystal grain of fine uniform, reduce the segregation degree of secondary phase, reduce the defects such as crack hole simultaneously, in zinc galvanic deposit industry, calendering anode replaces casting anode just gradually.Existing calendering anodic process is: lead alloy liquid is poured into a mould, and obtains blank flat after solidifying, and rolling afterwards obtains lead alloy plate, then smooths, shears, obtains production board after soldering polar ear.The weak point of existing technique is: 1) because anode material surface forms the crystalline structure that orientation is consistent, elongate form, number of grain boundaries are few in the rolling direction, cause anode material surface to lack corrosion centers, be difficult to form the excellent PbO of bonding force fast
2oxidation products protective layer.2) positive plate smooth surface is rolled; can not well stick on positive plate face at electrolytic process Anodic mud; majority comes off in the form of sheets; fresh plumbous surface is exposed in the electrolytic solution; well can not protect positive plate; shorten the life-span of positive plate, also cause separating out the leaded height of zinc metal sheet simultaneously, reduce quality product.3) randomness of the structure of the blank flat before calendering is comparatively large, and well regulate and control, the positive plate microstructure of the alloy obtained after making calendering is undesirable, and Pb base alloy mechanical performance may also be caused to worsen.Therefore, prior art has yet to be improved and developed.
Summary of the invention
The object of the invention is the shortcoming existed to overcome above-mentioned prior art, and preparation provides a kind of non-ferrous metal electrodeposition Novel anode with good electro catalytic activity, mechanical property and corrosion resistance nature.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention anode; Comprise the steps:
Step one
With as cast condition lead 2-base alloy for raw material, carry out calendering pre-treatment to got raw material, obtain rolling spare test piece, described calendering preprocessing process comprises at least one in diffusion annealing and rotten thermal treatment;
The temperature of described diffusion annealing is 280 ~ 320 DEG C, is preferably 290-310 DEG C, more preferably 300 DEG C;
Described rotten heat treated temperature is 180 ~ 260 DEG C, preferably 200-240 DEG C, more preferably 220-230 DEG C;
Step 2
Step one gained calendering spare test piece is rolled; Obtain the preform setting size.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention anode; After obtaining preform, directly can use, in order to promote quality further, Aging in electric field process can be carried out to step 2 gained preform, obtaining finished product; During described Aging in electric field process, control temperature is 80 ~ 120 DEG C, preferably 90-110 DEG C, more preferably 100-105 DEG C, and strength of electric field is 1 ~ 8kV/cm, is preferably 3 ~ 6kV/cm, more preferably 4 ~ 5kV/cm.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention 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 of insulation 30 ~ 60min, to be preferably after 40-50min, more preferably 45min with 3 ~ 10 DEG C/min, to be preferably 5-8 DEG C/min, the more preferably speed of 6 DEG C/min and to be cooled to room temperature, leave standstill 1 ~ 2h in room temperature.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention anode; Described in step one, rotten heat-treat condition is: under protective atmosphere, in temperature 180 ~ 260 DEG C, preferably 200-240 DEG C, more preferably 220-230 DEG C, and insulation 30 ~ 45min, preferably 30-40min, more preferably 35min; Room temperature is cooled to the furnace after insulation.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention anode; During to the process of preform Aging in electric field, the period is 40 ~ 90min, is preferably 50-80min, more preferably 60-70min.
The preparation method of a kind of non-ferrous metal electrodeposition calendering of the present invention anode; Comprise the steps:
Steps A
With as cast condition lead 2-base alloy for raw material, carry out calendering pre-treatment to got raw material, obtain rolling spare test piece, described calendering preprocessing process first carries out diffusion annealing process, then carries out rotten thermal treatment;
Described diffusion annealing is: under protective atmosphere, in 280 ~ 320 DEG C, preferably 290-310 DEG C, more preferably 300 DEG C; Be cooled to room temperature with 3 ~ 10 DEG C/min, preferably 5-8 DEG C/min, the more preferably speed of 6 DEG C/min after lower insulation 30 ~ 60min, preferably 40-50min, more preferably 45min, leave standstill 1 ~ 2h in room temperature,
Described rotten thermal treatment is: under protective atmosphere, sample after diffusion annealing process is heated to 180 ~ 260 DEG C, preferably 200-240 DEG C, more preferably 220-230 DEG C, after insulation 30 ~ 45min, preferably 30-40min, more preferably 35min, cools to room temperature with the furnace;
Step B
Step one gained calendering spare test piece is rolled; Obtain the preform setting size;
Step C
Aging in electric field process is carried out to step 2 gained preform, obtains finished product; During described Aging in electric field process, control temperature is 80 ~ 120 DEG C, preferably 90-110 DEG C, more preferably 100-105 DEG C, strength of electric field is 1 ~ 8kV/cm, is preferably 3 ~ 6kV/cm, more preferably 4 ~ 5kV/cm, and the period is 40 ~ 90min, is preferably 50-80min, more preferably 60-70min.
In the present invention, described protective atmosphere is rare gas element, as argon gas and nitrogen.
Principle and advantage
(1) treatment step increasing diffusion annealing in pre-treatment is before calendering passed through, promote the diffusion of alloying element, regulation and control alloying element is at the distribution proportion of crystal boundary/intra-die, reduce grain boundary density, and then reduce the high secondary phase of the activity after rolling in crystal boundary and dendrite boundary region segregation, more preferably alloy mechanical property and corrosion resistance nature can be obtained;
(2) pass through in pre-treatment before calendering, to increase rotten heat treated step, change crystal boundary to form and orientation, improve CSL crystal boundary ratio, destroy complete crystal boundary and dendrite circle network, thus the branch grain boundary width reduced after calendering, suppress intergranular corrosion, thus the corrosion resistance nature of alloy can be improved;
(3) step of the Aging in electric field process after calendering, can refining alloy crystal grain, regulate the distribution of the second phase particles of separating out in calender line, increase the density in room, for electrochemical reaction provides more reaction site, thus improve the chemical property of alloy.
In a word, the present invention under the synergy of each workshop section and processing parameter (especially before calendering first by the diffusion annealing process of suitable parameter, then by the rotten thermal treatment of suitable parameter), achieve beyond thought effect, improve the electro catalytic activity of positive plate, mechanical property and corrosion resistance nature significantly.
Embodiment
Embodiment 1
In the present embodiment, described lead-silver alloys by percentage to the quality; Pb=99.5%; Ag=0.5%;
(1) in resistance furnace, lead-silver alloys is cast according to a conventional method;
(2) lead-silver alloys ingot casting that step (1) obtains is placed in resistance furnace, carry out calendering pre-treatment, processing condition are: under argon atmosphere, at 300 DEG C, be incubated 30min, are cooled to room temperature with the speed of 3 DEG C/min, leave standstill 2h; Be heated to 240 DEG C, insulation 45min, naturally cools to room temperature;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 40min, strength of electric field 2KV/cm at 80 DEG C.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 40 DEG C) application, compared with traditional lead silver alloy anode plate, the physical strength of this alloy anode improves 25% (tensile strength of this embodiment gained finished product is 23.15MPa), bath voltage reduces by 10% (bath voltage of this embodiment gained finished product is 1.64V), and corrosion rate reduces 17%, and (corrosion efficiency of this embodiment gained finished product is 3.32g/m
2h).
Comparative example 1
In this comparative example, the component of lead-silver alloys used and the content of each component are completely consistent with embodiment 1;
Its preparation process is:
(1) in resistance furnace, lead-silver alloys is cast according to a conventional method;
(2) lead-silver alloys ingot casting that step (1) obtains is placed in resistance furnace, carry out calendering pre-treatment, processing condition are: under argon atmosphere, 30min is incubated at 200 DEG C, 240 DEG C are heated to immediately after being cooled to room temperature with the speed of 3 DEG C/min, insulation 45min, naturally cools to room temperature;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field 40min, strength of electric field 2kV/cm under Aging in electric field device room temperature.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 40 DEG C) application, the tensile strength of this alloy anode is 17.60MPa, its bath voltage is 1.83V, and corrosion efficiency is 3.96g/m
2h.
Can be found out by embodiment 1 and comparative example 1, when the parameter of diffusion annealing process and rotten thermal treatment and Aging in electric field process is not in institute of the present invention limited range, the character of its gained finished product is well below the present invention.
Embodiment 2
In the present embodiment, described lead-silver alloys by percentage to the quality; Pb=99.6%; Ag=0.4%;
(1) in resistance furnace, lead-silver alloys is cast according to a conventional method;
(2) the lead 2-base alloy ingot casting that step (1) obtains is placed in resistance furnace, carries out calendering pre-treatment, processing condition are: under argon atmosphere, at 320 DEG C, be incubated 30min, are cooled to room temperature with the speed of 10 DEG C/min, leave standstill 2h;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 60min, strength of electric field 4KV/cm at 100 DEG C.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 30 DEG C) application, compared with traditional lead silver alloy anode plate, the physical strength of this alloy anode improves 40% (tensile strength of this embodiment gained finished product is 26.04MPa), bath voltage reduces by 15% (bath voltage of this embodiment gained finished product is 1.55V), and corrosion rate is basically identical, and (corrosion efficiency of this embodiment gained finished product is 4.02g/m
2h).
Comparative example 2
In this comparative example, the component of lead-silver alloys used and the content of each component are completely consistent with embodiment 2;
Its preparation process is:
(1) in resistance furnace, lead-silver alloys is cast according to a conventional method;
(2) lead-silver alloys ingot casting that step (1) obtains is placed in resistance furnace, carry out calendering pre-treatment, processing condition are: under argon atmosphere, 30min is incubated at 160 DEG C, rolled by two rollers or four-high mill immediately after being cooled to room temperature with the speed of 3 DEG C/min, obtain finished product;
(3) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 40 DEG C) application, the tensile strength of this alloy anode is 17.42MPa, its bath voltage is 1.84V, and corrosion efficiency is 4.24g/m
2h.
Can be found out by embodiment 2 and comparative example 2, when the parameter of diffusion annealing process is not in institute of the present invention limited range and when saving Aging in electric field process, the character of its gained finished product is well below the present invention.
Embodiment 3
In the present embodiment, described lead-Yin-rare earth alloy by percentage to the quality; Pb=99.5%, Ag=0.4%, rare earth=0.1%;
(1) under nitrogen protection atmosphere, molten lead liquid in electromagnetic oven, adds plumbous rare earth mother alloy and argent, obtains lead-Yin-rare earth alloy;
(2) the lead 2-base alloy ingot casting that step (1) obtains is placed in resistance furnace, carries out calendering pre-treatment, processing condition are: under nitrogen protection atmosphere, are incubated 60min at 280 DEG C, are cooled to room temperature with the speed of 10 DEG C/min, leave standstill 1h; Be heated to 260 DEG C, insulation 30min, naturally cools to room temperature;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 60min, strength of electric field 8KV/cm at 100 DEG C.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 30 DEG C) application, compared with traditional lead silver alloy anode plate, the physical strength of this alloy anode improves 30% (tensile strength of this embodiment gained finished product is 23.92MPa), bath voltage reduces by 12% (bath voltage of this embodiment gained finished product is 1.60V), and corrosion rate reduces 36%, and (corrosion efficiency of this embodiment gained finished product is 2.56g/m
2h).
Comparative example 3
In this comparative example, the component of lead-Yin-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, molten lead liquid in electromagnetic oven, adds plumbous rare earth mother alloy and argent, obtains lead-Yin-rare earth alloy;
(2) the lead 2-base alloy ingot casting that step (1) obtains is placed in resistance furnace, carry out calendering pre-treatment, processing condition are: under nitrogen protection atmosphere, 60min is incubated at 360 DEG C, room temperature is cooled to the speed of 15 DEG C/min, leave standstill 1h post-heating to 360 DEG C, insulation 1h, is cooled to room temperature with the speed of 15 DEG C/min;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 30min, strength of electric field 10KV/cm at 150 DEG C.
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 30 DEG C) application, the tensile strength of this alloy anode is 18.40MPa, its bath voltage is 1.77V, and corrosion efficiency is 3.55g/m
2h.
As can be seen from embodiment 3 and comparative example 3: when the parameter such as the speed of diffusion annealing process, cooling, rotten thermal treatment, the temperature of Aging in electric field, the strength of electric field of Aging in electric field exceeds the maximum value of the present invention's restriction, this causes the character of its gained finished product well below the present invention.
Embodiment 4
In the present embodiment, described lead-Yin-rare earth alloy by percentage to the quality; Pb=99.2%, Ag=0.5%, rare earth=0.3%;
(1) under nitrogen protection atmosphere, molten lead liquid in electromagnetic oven, adds plumbous silver-colored mother alloy, and plumbous rare earth mother alloy, obtains lead-Yin-rare earth alloy;
(2) the lead 2-base alloy ingot casting that step (1) obtains is placed in resistance furnace, carries out calendering pre-treatment, processing condition are: under argon atmosphere, at 320 DEG C, be incubated 60min, are cooled to room temperature with the speed of 5 DEG C/min, leave standstill 1h; Be heated to 180 DEG C, insulation 30min, naturally cools to room temperature;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 90min, strength of electric field 6KV/cm at 120 DEG C.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 30 DEG C) application, compared with traditional lead silver alloy anode plate, the physical strength of this alloy anode improves 22% (tensile strength of this embodiment gained finished product is 22.45MPa), bath voltage reduces by 14% (bath voltage of this embodiment gained finished product is 1.57V), and corrosion rate reduces 35%, and (corrosion efficiency of this embodiment gained finished product is 2.60g/m
2h).
Comparative example 4
In this comparative example, the component of lead-Yin-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, molten lead liquid in electromagnetic oven, adds plumbous silver-colored mother alloy, and plumbous rare earth mother alloy, obtains lead-Yin-rare earth alloy;
(2) the lead 2-base alloy ingot casting that step (1) obtains is placed in resistance furnace, carries out calendering pre-treatment, processing condition are: under argon atmosphere, at 250 DEG C, be incubated 20min, are cooled to room temperature with the speed of 1 DEG C/min, leave standstill 0.5h; Be heated to 170 DEG C, insulation 20min, naturally cools to room temperature;
(3) roll: the alloy that step (2) obtains is rolled by two rollers or four-high mill;
(4) Aging in electric field process: the positive plate that step (3) obtains is placed in Aging in electric field device, Aging in electric field 30min, strength of electric field 0.5KV/cm at 50 DEG C.，
(5) (Zn in Zinc electrolysis system
2+50g/L, H
2sO
4160g/L, temperature 30 DEG C) application, the tensile strength of this alloy anode is 18.22MPa, its bath voltage is 1.79V, and corrosion efficiency is 3.96g/m
2h.
As can be seen from embodiment 4 and comparative example 4: when the parameter such as the speed of diffusion annealing process, cooling, rotten thermal treatment, the temperature of Aging in electric field, the strength of electric field of Aging in electric field is less than the minimum value of the present invention's restriction, this causes the character of its gained finished product well below the present invention.
Claims (10)
1. a non-ferrous metal electrodeposition preparation method for calendering anode, is characterized in that comprising the steps:
Step one
With as cast condition lead 2-base alloy for raw material, carry out calendering pre-treatment to got raw material, obtain rolling spare test piece, described calendering preprocessing process comprises at least one in diffusion annealing and rotten thermal treatment;
The temperature of described diffusion annealing is 280 ~ 320 DEG C;
Described rotten heat treated temperature is 180 ~ 260 DEG C;
Step 2
Step one gained calendering spare test piece is rolled; Obtain the preform setting size.
2. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 1, is characterized in that:
Aging in electric field process is carried out to step 2 gained preform, obtains finished product; During described Aging in electric field process, control temperature is 80 ~ 120 DEG C, and strength of electric field is 1 ~ 8kV/cm.
3. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 1; it is characterized in that: diffusion annealing described in step one is: under protective atmosphere, after 280 ~ 320 DEG C of insulation 30 ~ 60min, be cooled to room temperature with the speed of 3 ~ 10 DEG C/min.
4. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 3, is characterized in that; Described diffusion annealing is: under protective atmosphere, after 290-310 DEG C of insulation 40-50min, be cooled to room temperature with the speed of 5-8 DEG C/min.
5. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 1, is characterized in that: described in step one, rotten heat treated condition is: under protective atmosphere, in temperature 180 ~ 260 DEG C; Soaking time 30 ~ 45min; Room temperature is cooled to the furnace after insulation.
6. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 5, is characterized in that: described rotten heat treated condition is: under protective atmosphere, after 200-240 DEG C of insulation 30-40min, cool to room temperature with the furnace.
7. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 2, is characterized in that: during Aging in electric field process, control temperature is 80 ~ 120 DEG C, the period is 40 ~ 90min, control strength of electric field is 1 ~ 8kV/cm.
8. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 7, is characterized in that: during Aging in electric field process, control temperature is 90-110 DEG C, the period is 50-80min, control strength of electric field is 3 ~ 6kV/cm.
9. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 8, is characterized in that: during Aging in electric field process, control temperature is 100-105 DEG C, the period is 60-70min, control strength of electric field is 4 ~ 5kV/cm.
10. the preparation method of a kind of non-ferrous metal electrodeposition calendering anode according to claim 1, is characterized in that comprising the steps:
Steps A
With as cast condition lead 2-base alloy for raw material, carry out calendering pre-treatment to got raw material, obtain rolling spare test piece, described calendering preprocessing process first carries out diffusion annealing process, then carries out rotten thermal treatment;
Described diffusion annealing is: be cooled to room temperature with the speed of 3 ~ 10 DEG C/min be incubated 30 ~ 60min at 280 ~ 320 DEG C after, leaves standstill 1 ~ 2h, obtain the sample after diffusion annealing process in room temperature;
Described rotten thermal treatment is: cool to room temperature with the furnace after the sample after diffusion annealing process being heated to 180 ~ 260 DEG C of insulation 30 ~ 45min;
Step B
Step one gained calendering spare test piece is rolled; Obtain the preform setting size;
Step C
Aging in electric field process is carried out to step 2 gained preform, obtains finished product; During described Aging in electric field process, control temperature is 80 ~ 120 DEG C, and strength of electric field is 1 ~ 8kV/cm, the time is 40 ~ 90min.
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| CN105040036B (en) | 2017-07-28 |
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