CN109112605A - A kind of electrolytic copper foil titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid and regeneration method - Google Patents
A kind of electrolytic copper foil titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid and regeneration method Download PDFInfo
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- CN109112605A CN109112605A CN201810984004.6A CN201810984004A CN109112605A CN 109112605 A CN109112605 A CN 109112605A CN 201810984004 A CN201810984004 A CN 201810984004A CN 109112605 A CN109112605 A CN 109112605A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
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Abstract
The present invention provides a kind of manufacture electrolytic copper foil titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid and regeneration method, which is made of the aqueous solution of the halide of choline, ammonium chloride and polyvinylpyrrolidone-K30.The concentration of the halide of choline is 100-600g/L, and the concentration of ammonium chloride is 20-120g/L, and the concentration of surfactant polyvinylpyrrolidone-K30 is 0.01-0.5g/L.It after titanium-based iridium-tantalum pentoxide coated anode plate is washed with deionized water, is placed in regenerated liquid, under conditions of 30-60 DEG C, is impregnated 20-60 minutes under conditions of ultrasonic activation.Operation of the present invention is simple, regenerated titanium-based iridium-tantalum pentoxide coated anode plate can be restored to original surface state, regenerated titanium-based iridium-tantalum pentoxide coated anode plate fully meets the demand of production Copper Foil in Li-ion Battery, can also meet the needs of production printed wiring board-use copper-clad.
Description
Technical field
The invention belongs to Cu foil anode process fields, are related to a kind of electrolytic copper foil titanium-based iridium-tantalum pentoxide coated anode
Regeneration techniques, in particular to the regenerated liquid and regeneration treating method of a kind of titanium-based iridium-tantalum pentoxide coated anode plate.
Background technique
In electrolytic copper foil production technology, electrolyte is made of copper sulphate, sulfuric acid and additive, and the concentration of sulfuric acid
It is very big, corrosion is easily brought to electrolytic anode.Simultaneously because the current density applied in electrolytic process is very big, on anode
Precipitated oxygen, so analysis oxygen type titanium-based iridium-tantalum that the anode of usually electrolytic copper foil is excellent using corrosion resistance and electrocatalysis characteristic
Oxide coating anode (Ti/IrO2+Ta2O5).In electrolytic process, anode surface is slowly covered by one layer of fine and close layer of scale,
Cause the adverse effects such as the copper foil uniformity that tank voltage increases, power consumption increases and electrolysis is precipitated is inadequate, product qualification rate reduces.Its
The ingredient of fouling is considered the impurity element such as Pb in mainly electrolyte2+、Sr2+、Ca2+And Ba2+Equal sulfate are on anode
Deposition, one of the most common is PbSO4.The presence of layer of scale makes anode conductivity poor, and tank voltage is raised simultaneously as knot
Dirty layer is unevenly distributed anode potential, and the copper foil uniformity that electrolysis production comes out is inadequate, and product qualification rate reduces.In addition,
The zone conducts current covered by fouling is bad, causes the current density relative increase in uncovered region, and anode potential enhancing is accelerated
The passivation failure of the zone-coating.Therefore, in copper foil production technology, regular dismounting anode is needed, removes the fouling on its surface,
Production could be made to stablize, be effectively performed.
Removing the common method of anode fouling has acid wash and alkali wash etc..Acid wash and alkali wash are handled at high temperature
The usage amount of layer of scale, severe operational environment, bronsted lowry acids and bases bronsted lowry is big, easily causes environmental pollution, fouling removal efficiency is low, while strong acid
Or highly basic can also corrode iridium-tantalum pentoxide coating, do a lot of damage to anode.Titanium-based iridium-tantalum pentoxide coating of the invention
Anode regenerated liquid can effectively and quickly remove layer of scale and destroy Titanium base and its surface covering.
Summary of the invention
It is excellent to titanium-based iridium-tantalum pentoxide coated anode regeneration effect the object of the present invention is to provide a kind of simple and easy
Regeneration treatment liquid titanium-based iridium-tantalum pentoxide coated anode surface knot can be effectively removed by the processing of the regenerated liquid
Dirt regenerates titanium-based iridium-tantalum pentoxide coated anode.
In order to achieve the above objectives, regenerated liquid of the invention is the halide, ammonium chloride and polyvinylpyrrolidine by choline
Chemical pretreatment solution composed by ketone-K30 can make to chemically react between layer of scale, to remove fouling.For in regenerated liquid
Choline chloride, choline bromide or choline iodide etc. can be selected in the halide of choline, selects choline chloride more to close from cost consideration
It is suitable.The concentration of choline chloride is too low, does not have the effect of removal fouling, if concentration is excessively high, not only increases the cost of regenerated liquid, together
When due to the viscosity of regenerated liquid it is excessive, to it is subsequent washing affect, concentration range can be controlled in 100-600g/L.For
In regenerated liquid for the concentration of ammonium chloride, the concentration of ammonium chloride is excessive, be easy to cause to titanium-based iridium-tantalum pentoxide coated anode oxygen
The corrosion of compound coating, concentration is too low, then does not have the effect of removal fouling, and the concentration range of ammonium chloride is 20- in regenerated liquid
120g/L.The optimum range of surfactant polyvinylpyrrolidone-K30 concentration in regenerated liquid is 0.01-0.5g/L, poly- second
The concentration of alkene pyrrolidone-K30 is too low, and regenerated liquid, which acts on titanium-based iridium-tantalum pentoxide coated anode moistened surface, to be declined, and goes
Except the ability of fouling dies down, on the contrary excessive concentration, it is easy to form residual on titanium-based iridium-tantalum pentoxide coated anode plate, it is difficult to
Cleaning.
Titanium-based iridium of the invention-tantalum pentoxide coated anode regeneration method is, by titanium-based iridium-tantalum pentoxide coated anode
It after plate is washed with deionized, is placed in regenerated liquid, under conditions of 30-60 DEG C, is impregnated under conditions of ultrasonic activation
20-60 minutes.For the present invention compared with the current common method of removing anode fouling, tool is easy to operate, and can quickly remove knot
Dirty layer, and Titanium base and its surface covering are not destroyed.Regenerated titanium-based iridium-tantalum pentoxide coated anode plate can be restored to original
Surface state can meet the needs of Copper Foil in Li-ion Battery, can also meet the needs of printed wiring board-use copper-clad.
Specific embodiment
Further illustrate regenerated liquid of the invention to the regeneration of titanium-based iridium-tantalum pentoxide coated anode below by embodiment
Method.In order to effectively illustrate the effect after titanium-based iridium-tantalum pentoxide coated anode regeneration, swept from 0.3V with the speed of 5mV/s
To 2.0V, platinum plate electrode is to electrode, and Ag/AgCl electrode is reference electrode, titanium-based iridium-tantalum pentoxide coating of size 2x 6cm
For working electrode, by measuring in 1mol/LH2SO4Oxygen evolution potential in solution is evaluated.After measured, new titanium-based iridium-tantalum
The oxygen evolution potential of oxide coating electrode is 1.22V, has been used by titanium-based iridium-tantalum pentoxide coated electrode analysis oxygen of surface scale
Current potential is about 1.42V or so.
Embodiment 1
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added, obtains regenerated liquid.The concentration of choline chloride is 100g/L, ammonium chloride in regenerated liquid
Concentration be 20g/L, the concentration of polyvinylpyrrolidone-K30 is 0.01g/L.By used titanium-based iridium-tantalum pentoxide coating
It after anode plate is cleaned with deionized water, is placed in regenerated liquid, is impregnated after sixty minutes under conditions of 60 DEG C of ultrasonic activations, i.e.,
It can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity are carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for position.
Embodiment 2
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added, obtains regenerated liquid.The concentration of choline chloride is 300g/L, ammonium chloride in regenerated liquid
Concentration be 40g/L, the concentration of polyvinylpyrrolidone-K30 is 0.05g/L.By used titanium-based iridium-tantalum pentoxide coating
It after anode plate is cleaned with deionized water, is placed in regenerated liquid, after being impregnated 45 minutes under conditions of 50 DEG C of ultrasonic activations, i.e.,
It can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity are carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for position.
Embodiment 3
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added, obtains regenerated liquid.The concentration of choline chloride is 500g/L, ammonium chloride in regenerated liquid
Concentration be 60g/L, the concentration of polyvinylpyrrolidone-K30 is 0.1g/L.By used titanium-based iridium-tantalum pentoxide coating
It after anode plate is cleaned with deionized water, is placed in regenerated liquid, after being impregnated 30 minutes under conditions of 45 DEG C of ultrasonic activations, i.e.,
It can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity are carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for position.
Embodiment 4
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added, obtains regenerated liquid.The concentration of choline chloride is 600g/L, ammonium chloride in regenerated liquid
Concentration be 100g/L, the concentration of polyvinylpyrrolidone-K30 is 0.3g/L.By used titanium-based iridium-tantalum pentoxide coating
It after anode plate is cleaned with deionized water, is placed in regenerated liquid, after being impregnated 30 minutes under conditions of 30 DEG C of ultrasonic activations, i.e.,
It can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity are carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for position.
Embodiment 5
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added, obtains regenerated liquid.The concentration of choline chloride is 600g/L, ammonium chloride in regenerated liquid
Concentration be 120g/L, the concentration of polyvinylpyrrolidone-K30 is 0.5g/L.By used titanium-based iridium-tantalum pentoxide coating
It after anode plate is cleaned with deionized water, is placed in regenerated liquid, is impregnated after twenty minutes under conditions of 45 DEG C of ultrasonic activations, i.e.,
It can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity are carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for position.
Comparative example 1
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added.The concentration of choline chloride is 50g/L, and the concentration of ammonium chloride is 50g/L, poly- second
The concentration of alkene pyrrolidone-K30 is 0.5g/L.Used titanium-based iridium-tantalum pentoxide coated anode plate deionized water is clear
It after washing, is placed in regenerated liquid, is impregnated after sixty minutes under conditions of 60 DEG C of ultrasonic activations, that is, can reach to titanium-based iridium-tantalum
Oxide coating anode carries out regenerated purpose, and the results are shown in Table 1 for titanium-based iridium-tantalum pentoxide coated anode oxygen evolution potential.
Comparative example 2
Choline chloride is slowly dissolve into deionized water, is slowly added to the aqueous solution of ammonium chloride under agitation, then
The aqueous solution of polyvinylpyrrolidone-K30 is added.The concentration of choline chloride is 100g/L, and the concentration of ammonium chloride is 10g/L, is gathered
The concentration of vinylpyrrolidone-K30 is 0.5g/L.By used titanium-based iridium-tantalum pentoxide coated anode plate deionized water
It after cleaning, is placed in regenerated liquid, impregnates after sixty minutes, that is, can reach to titanium-based iridium-under conditions of 60 DEG C of ultrasonic activations
Tantalum pentoxide coated anode carries out regenerated purpose, and titanium-based iridium-tantalum pentoxide coated anode oxygen evolution potential result is listed in table 1
In.
Comparative example 3
Choline chloride is slowly dissolve into deionized water, the aqueous solution of ammonium chloride is slowly added under agitation, obtains
Regenerated liquid.The concentration of choline chloride is 200g/L in regenerated liquid, and the concentration of ammonium chloride is 50g/L.By used titanium-based iridium-tantalum
It after oxide coating anode plate is cleaned with deionized water, is placed in regenerated liquid, is impregnated under conditions of 60 DEG C of ultrasonic activations
After sixty minutes, that is, it can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coating carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for the oxygen evolution potential of anode.
Comparative example 4
Choline chloride is slowly dissolve into deionized water, is slowly added to polyvinylpyrrolidone-K30 under agitation
Aqueous solution, obtain regenerated liquid.The concentration of choline chloride is 200g/L in regenerated liquid, and the concentration of polyvinylpyrrolidone-K30 is
0.1g/L.After used titanium-based iridium-tantalum pentoxide coated anode plate is cleaned with deionized water, it is placed in regenerated liquid,
It is impregnated after sixty minutes under conditions of 60 DEG C of ultrasonic activations, that is, can reach and titanium-based iridium-tantalum pentoxide coated anode is regenerated
Purpose, the results are shown in Table 1 for titanium-based iridium-tantalum pentoxide coated anode oxygen evolution potential.
Comparative example 5
The aqueous solution of ammonium chloride and the aqueous solution of polyvinylpyrrolidone-K30 are mixed, regenerated liquid is obtained.Chlorine in regenerated liquid
The concentration for changing ammonium is 100g/L, and the concentration of polyvinylpyrrolidone-K30 is 0.1g/L.By used titanium-based iridium-tantalum pentoxide
It after coated anode plate is cleaned with deionized water, is placed in regenerated liquid, is impregnated 60 minutes under conditions of 60 DEG C of ultrasonic activations
Afterwards, that is, it can reach and regenerated purpose, titanium-based iridium-tantalum pentoxide coated anode carried out to titanium-based iridium-tantalum pentoxide coated anode
The results are shown in Table 1 for oxygen evolution potential.
Titanium-based iridium-tantalum pentoxide coated anode the oxygen evolution potential of 1 regenerated liquid of table before and after the processing
| Example | Oxygen evolution potential V before regeneration treatment | Oxygen evolution potential V before regeneration treatment |
| Embodiment 1 | 1.42 | 1.23 |
| Embodiment 2 | 1.40 | 1.24 |
| Embodiment 3 | 1.41 | 1.21 |
| Embodiment 4 | 1.43 | 1.24 |
| Embodiment 5 | 1.42 | 1.22 |
| Comparative example 1 | 1.42 | 1.39 |
| Comparative example 2 | 1.42 | 1.38 |
| Comparative example 3 | 1.41 | 1.29 |
| Comparative example 4 | 1.43 | 1.39 |
| Comparative example 5 | 1.42 | 1.35 |
By the result in table 1 it is found that being obtained based on regenerated liquid treated titanium-based iridium-tantalum pentoxide coated anode
Analysis oxygen electricity and new titanium-based iridium-tantalum pentoxide coated anode analysis oxygen electricity be it is very close, can prove through the invention again
It is horizontal that raw liquid processing titanium-based iridium-tantalum pentoxide coated anode can be restored to new titanium-based iridium-tantalum pentoxide coated anode.
Claims (5)
1. a kind of electrolytic copper foil titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid, which is characterized in that at the regeneration
Reason liquid is made of the aqueous solution of the halide of choline, ammonium chloride and surfactant polyvinylpyrrolidone-K30.
2. according to the titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid of electrolytic copper foil described in claim l, feature exists
In: choline chloride, choline bromide or choline iodide can be selected in the halide of choline in the regeneration treatment liquid；The halide of choline
Concentration be 100-600g/L.
3. according to the titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid of electrolytic copper foil described in claim l, feature exists
In: the concentration of ammonium chloride is 20-120g/L in the regeneration treatment liquid.
4. according to the titanium-based iridium-tantalum pentoxide coated anode regeneration treatment liquid of electrolytic copper foil described in claim l, feature exists
In: the concentration of surfactant polyvinylpyrrolidone-K30 is 0.01-0.5g/L in the regeneration treatment liquid.
5. it is a kind of according to the titanium-based iridium-tantalum pentoxide coated anode regeneration of any one of the claim l-4 electrolytic copper foil at
Manage the regeneration method of liquid, it is characterised in that: after cleaning titanium-based iridium-tantalum pentoxide coated anode plate with deionized water, be placed on
In regenerated liquid, under conditions of 30-60 DEG C, impregnated 20-60 minutes under conditions of ultrasonic activation.
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