CN112011799A - Additive for cleaning titanium anode plate of electrolytic cell and cleaning method - Google Patents
Additive for cleaning titanium anode plate of electrolytic cell and cleaning method Download PDFInfo
- Publication number
- CN112011799A CN112011799A CN202010830215.1A CN202010830215A CN112011799A CN 112011799 A CN112011799 A CN 112011799A CN 202010830215 A CN202010830215 A CN 202010830215A CN 112011799 A CN112011799 A CN 112011799A
- Authority
- CN
- China
- Prior art keywords
- anode plate
- titanium anode
- cleaning
- electrolytic cell
- pure water
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000010936 titanium Substances 0.000 title claims abstract description 70
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 70
- 238000004140 cleaning Methods 0.000 title claims abstract description 39
- 239000000654 additive Substances 0.000 title claims abstract description 29
- 230000000996 additive effect Effects 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229950005499 carbon tetrachloride Drugs 0.000 claims abstract description 16
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 239000008139 complexing agent Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 8
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 8
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000009991 scouring Methods 0.000 claims abstract description 6
- 238000005201 scrubbing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 14
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- 239000012629 purifying agent Substances 0.000 claims description 2
- 229960001124 trientine Drugs 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011889 copper foil Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000003213 activating effect Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 4
- 238000010411 cooking Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
Classifications
-
- 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
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention discloses an additive for cleaning a titanium anode plate of an electrolytic cell and a cleaning method, wherein the additive comprises polyethylene glycol, sodium dodecyl sulfate, oxalic acid, a complexing agent A, tetrachloromethane and pure water. The cleaning method comprises the following steps: soaking the titanium anode plate in potassium dihydrogen phosphate and water, washing with pure water, uniformly scrubbing with an additive and scouring pad to make scale and the additive fully react, washing with pure water, activating in sulfuric acid, washing and drying in the air. The invention can effectively clean the scale on the anode plate of the electrolytic cell, so that the produced electrolytic copper foil has small surface density range, and simultaneously can reduce the electrolytic cell pressure, reduce the energy consumption, prolong the service life of the titanium anode and reduce the production cost.
Description
Technical Field
The invention relates to the technical field of cleaning of titanium anode plates of electrolytic cells, in particular to an additive for cleaning the titanium anode plates of the electrolytic cells and a cleaning method.
Background
With the rapid development of electronic products, higher requirements are put forward on the consistency of the electrolytic copper foil, and the titanium anode plate with good consistency can produce the electrolytic copper foil with higher precision. In the production process of the electrolytic copper foil, a compact scaling layer is formed on the surface of the anode to influence the consistency of the titanium anode plate, so that the cell pressure is increased, and the power consumption is increased; and the anode potential distribution is not uniform due to the scaling layer, the crystallization speed, the nucleation quantity and the crystal lattice size of copper ions in the electrodeposition process are directly influenced, and the copper foil produced by electrolysis has non-uniform thickness and poor precision. Therefore, the anode plate needs to be periodically disassembled and the scales on the surface of the anode plate need to be cleaned, so that the production is stably and effectively carried out, and the high-precision electrolytic copper foil is obtained.
In the prior art, common methods for removing anode scale include: mechanical removal method, acid cooking method, alkaline cooking method and the like, wherein the mechanical removal method is simple to operate, but easily damages the surface coating of the anode; the acid and alkaline cooking processes are wasteful and inefficient in scale removal and also cause significant damage to the anode.
An effective solution to the problems in the related art has not been proposed yet.
Disclosure of Invention
Aiming at the technical problems in the related art, the invention provides the additive for cleaning the titanium anode plate of the electrolytic cell and the cleaning method.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
an additive for cleaning a titanium anode plate of an electrolytic cell comprises the following components: the water purifying agent comprises polyethylene glycol, sodium dodecyl sulfate, oxalic acid, a complexing agent A, tetrachloromethane and pure water, wherein the concentrations of the polyethylene glycol, the sodium dodecyl sulfate, the oxalic acid, the complexing agent A and the tetrachloromethane are respectively 50-60 g/L, 80-100 g/L, 100-120 g/L, 150-160 ml/L and 120-150 ml/L.
Further, the molecular weight of the polyethylene glycol is 4000, and the complexing agent A is one of triethylene tetramine and ethylenediamine.
On the other hand, the invention also provides a preparation method of the additive, which comprises the steps of adding oxalic acid into tetrachloromethane, stirring for dissolving, adding pure water, stirring uniformly, sequentially adding polyethylene glycol, sodium dodecyl sulfate and complexing agent A, stirring for dissolving, and then fixing the volume by using the pure water.
On the other hand, the invention also provides a method for cleaning the titanium anode plate of the electrolytic cell, which comprises the following cleaning steps:
s1, soaking the titanium anode plate in potassium dihydrogen phosphate and water solution for 2 hours, and taking out;
s2, washing the surface of the titanium anode plate by pure water;
s3, scrubbing scales on the surface of the titanium anode plate by using the additive and the scouring pad as claimed in any one of claims 1-2, and washing the titanium anode plate clean by using pure water;
and S4, putting the titanium anode plate into sulfuric acid solution for activation for 6 hours, washing the titanium anode plate clean by pure water and airing the titanium anode plate.
Further, in the step S1, the mass concentration of the potassium dihydrogen phosphate solution is 50%.
Further, the temperature of the solution for soaking the titanium anode plate in the step S1 is 80 ℃.
Further, the water pressure of the pure water in the step S2 is 0.05 MPa.
Further, the mass concentration of the sulfuric acid solution in the step S4 is 10%.
The invention has the beneficial effects that: the additive and the cleaning method for cleaning the titanium anode plate of the electrolytic cell can effectively clean scales on the titanium anode plate of the electrolytic cell, the produced electrolytic copper foil has small surface density range, and simultaneously can reduce the pressure of the electrolytic cell, reduce the energy consumption, prolong the service life of the titanium anode and reduce the production cost.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
Example 1
The additive for cleaning the titanium anode plate of the electrolytic tank comprises 50g/L of polyethylene glycol, 80g/L of sodium dodecyl sulfate, 100g/L of oxalic acid, 150mL/L of complexing agent A, 120mL/L of tetrachloromethane and pure water.
The preparation method of the additive comprises the following steps: weighing 100g of oxalic acid, adding the oxalic acid into 120mL of tetrachloromethane, stirring and dissolving the oxalic acid and the tetrachloromethane mutually, adding 500mL of pure water, stirring, sequentially adding 50g of polyethylene glycol, 80g of sodium dodecyl sulfate and 150mL of complexing agent A, using the pure water to fix the volume to 1 liter, and stirring and dissolving.
The cleaning method of the titanium anode plate of the electrolytic cell comprises the following steps:
soaking a titanium anode plate to be cleaned in 50% by mass of potassium dihydrogen phosphate and 80 ℃ water solution for 2 hours, taking out the titanium anode plate after soaking for 2 hours, washing the surface of the titanium anode plate with pure water under the water pressure of 0.05MPa, scrubbing the surface of the titanium anode plate with scouring pad and the cleaning additive to enable scales to fully react with the cleaning additive, washing the titanium anode plate with the pure water, activating the titanium anode plate in 10% by mass of sulfuric acid for 6 hours, washing the titanium anode plate with the pure water, and drying the titanium anode plate in the air.
Example 2
The additive for cleaning the titanium anode plate of the electrolytic tank comprises 55g/L of polyethylene glycol, 90g/L of sodium dodecyl sulfate, 110g/L of oxalic acid, 155mL/L of complexing agent A, 130mL/L of tetrachloromethane and pure water.
The preparation method of the additive comprises the following steps: weighing 110g of oxalic acid, adding the oxalic acid into 130mL of tetrachloromethane, stirring and dissolving the oxalic acid and the tetrachloromethane mutually, adding 500m of water, stirring, sequentially adding 55g of polyethylene glycol, 90g of sodium dodecyl sulfate and 155mL of complexing agent A, using pure water to fix the volume to 1 liter, and stirring and dissolving.
The cleaning method of the titanium anode plate of the electrolytic cell comprises the following steps:
soaking a titanium anode plate to be cleaned in 50% of monopotassium phosphate and 80 ℃ water for 2 hours, taking out the titanium anode plate after continuously soaking, washing the surface of the titanium anode plate with pure water under the water pressure of 0.05MPa, scrubbing the surface of the titanium anode plate with scouring pad and the cleaning additive to enable scales to fully react with the cleaning additive, washing the titanium anode plate with pure water, activating the titanium anode plate in 10% of sulfuric acid for 6 hours, washing the titanium anode plate with pure water, and airing.
Example 3
The additive for cleaning the titanium anode plate of the electrolytic tank comprises 60g/L of polyethylene glycol, 100g/L of sodium dodecyl sulfate, 120g/L of oxalic acid, 160mL/L of complexing agent A, 150mL/L of tetrachloromethane and pure water.
The preparation method of the additive comprises the following steps: weighing 120g of oxalic acid, adding the oxalic acid into 150mL of tetrachloromethane, stirring and dissolving the oxalic acid and the tetrachloromethane mutually, adding 500mL of water, stirring, sequentially adding 60g of polyethylene glycol, 100g of sodium dodecyl sulfate and 160mL of complexing agent A, using pure water to fix the volume to 1 liter, and stirring and dissolving the mixture.
The cleaning method of the titanium anode plate of the electrolytic cell comprises the following steps:
soaking a titanium anode plate to be cleaned in 50% of monopotassium phosphate and 80 ℃ water for 2 hours, taking out the titanium anode plate after continuously soaking, washing the surface of the titanium anode plate with pure water under the water pressure of 0.05MPa, scrubbing the surface of the titanium anode plate with scouring pad and the cleaning additive to enable scales to fully react with the cleaning additive, washing the titanium anode plate with pure water, activating the titanium anode plate in 10% of sulfuric acid for 6 hours, washing the titanium anode plate with pure water, and airing.
The data table of the surface density range difference measured by an electronic scale and the electrolytic bath pressure measured by a universal meter for 6um, 8um and 12um copper foils produced by the titanium anode plates before and after cleaning in the above examples 1, 2 and 3 is as follows:
in conclusion, by means of the technical scheme, the additive for cleaning the titanium anode plate of the electrolytic cell and the cleaning method can effectively clean scales on the titanium anode plate of the electrolytic cell, the produced electrolytic copper foil has small surface density range, and meanwhile, the electrolytic cell pressure can be reduced, the energy consumption can be reduced, the service life of the titanium anode can be prolonged, and the production cost can be reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. An additive for cleaning a titanium anode plate of an electrolytic cell is characterized by comprising the following components: the water purifying agent comprises polyethylene glycol, sodium dodecyl sulfate, oxalic acid, a complexing agent A, tetrachloromethane and pure water, wherein the concentrations of the polyethylene glycol, the sodium dodecyl sulfate, the oxalic acid, the complexing agent A and the tetrachloromethane are respectively 50-60 g/L, 80-100 g/L, 100-120 g/L, 150-160 ml/L and 120-150 ml/L.
2. The additive for cleaning the titanium anode plate of the electrolytic cell as claimed in claim 1, wherein the molecular weight of the polyethylene glycol is 4000, and the complexing agent A is one of triethylene tetramine and ethylene diamine.
3. A method for preparing the additive according to any one of claims 1 to 2, wherein oxalic acid is added to tetrachloromethane, and after being dissolved by stirring, pure water is added, and after being uniformly stirred, polyethylene glycol, sodium dodecyl sulfate and the complexing agent a are sequentially added, and after being dissolved by stirring, the volume is determined by using pure water.
4. The method for cleaning the titanium anode plate of the electrolytic cell is characterized by comprising the following steps of:
s1, soaking the titanium anode plate in potassium dihydrogen phosphate and water solution for 2 hours, and taking out;
s2, washing the surface of the titanium anode plate by pure water;
s3, scrubbing scales on the surface of the titanium anode plate by using the additive and the scouring pad as claimed in any one of claims 1-2, and washing the titanium anode plate clean by using pure water;
and S4, putting the titanium anode plate into sulfuric acid solution for activation for 6 hours, washing the titanium anode plate clean by pure water and airing the titanium anode plate.
5. The method for cleaning the titanium anode plate of the electrolytic cell according to claim 4, wherein the mass concentration of the potassium dihydrogen phosphate solution in the step S1 is 50%.
6. The method for cleaning the titanium anode plate of the electrolytic cell according to claim 4, wherein the temperature of the solution for soaking the titanium anode plate in the step S1 is 80 ℃.
7. The method for cleaning the titanium anode plate of the electrolytic cell according to claim 4, wherein the water pressure of the pure water in the step S2 is 0.05 MPa.
8. The method for cleaning the titanium anode plate of the electrolytic cell according to claim 4, wherein the mass concentration of the sulfuric acid solution in the step S4 is 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010830215.1A CN112011799A (en) | 2020-08-18 | 2020-08-18 | Additive for cleaning titanium anode plate of electrolytic cell and cleaning method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010830215.1A CN112011799A (en) | 2020-08-18 | 2020-08-18 | Additive for cleaning titanium anode plate of electrolytic cell and cleaning method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112011799A true CN112011799A (en) | 2020-12-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010830215.1A Pending CN112011799A (en) | 2020-08-18 | 2020-08-18 | Additive for cleaning titanium anode plate of electrolytic cell and cleaning method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112011799A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114717057A (en) * | 2022-03-18 | 2022-07-08 | 九江德福科技股份有限公司 | Cleaning solution and cleaning method for cleaning collagen adding system |
| CN115305161A (en) * | 2022-07-22 | 2022-11-08 | 福建紫金铜箔科技有限公司 | Electrolytic copper foil anode plate cleaning agent and preparation method thereof |
| CN116254536A (en) * | 2023-02-17 | 2023-06-13 | 九江斯坦德能源工业有限公司 | Cleaning agent and cleaning method for titanium anode plate of foil producing machine |
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| CN116254536A (en) * | 2023-02-17 | 2023-06-13 | 九江斯坦德能源工业有限公司 | Cleaning agent and cleaning method for titanium anode plate of foil producing machine |
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Application publication date: 20201201 |
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