CN111472005A - Acidic environment-friendly anti-oxidation process for electrolytic copper foil - Google Patents
Acidic environment-friendly anti-oxidation process for electrolytic copper foil Download PDFInfo
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- CN111472005A CN111472005A CN202010342533.3A CN202010342533A CN111472005A CN 111472005 A CN111472005 A CN 111472005A CN 202010342533 A CN202010342533 A CN 202010342533A CN 111472005 A CN111472005 A CN 111472005A
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors
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Abstract
The invention discloses an acidic environment-friendly anti-oxidation process for electrolytic copper foil, which comprises the steps of preparing anti-oxidation liquid from 2-Mercaptobenzoxazole (MBO), glycol, a silane coupling agent, alkanolamine, α -alkenyl sodium sulfonate and water, introducing the electrolytic copper foil into the anti-oxidation liquid, soaking and adsorbing for 5-20s, guiding out the soaked and adsorbed electrolytic copper foil, drying and rolling.
Description
Technical Field
The invention relates to the technical field of electrolytic copper foil production, in particular to a process for carrying out surface anti-oxidation treatment on an electrolytic copper foil.
Background
Along with the improvement of the quality requirement of a lithium electro-copper foil client on a high-end battery product, the lithium electro-copper foil is required to have high-temperature oxidation resistance (the lithium electro-copper foil cannot be oxidized and discolored when being put into an oven to be baked for 15min at 140 ℃), and good wettability. Therefore, the technical problems that after the copper foil is subjected to anti-oxidation treatment, the copper foil has high-temperature oxidation resistance (the lithium-ion copper foil cannot be oxidized and discolored when being placed in an oven to be baked for 15min at 140 ℃) and good wettability (the wettability is not less than 36 dyne) are solved in the surface anti-oxidation treatment stage. When an alkaline anti-oxidation process is used in the electrolytic copper foil preparation process, the scaling phenomenon can be generated on the surfaces of the conductive roller and the submerged roller, so that the defects of concave-convex points, wrinkles and the like of a copper foil product are generated, and the yield of the copper foil is reduced. At present, the traditional surface anti-oxidation process technology of the electrolytic copper foil in China mainly comprises the following steps:
the acid electroplating process of the ternary alloy comprises the following steps: chromic anhydride, zinc sulfate, nickel sulfate and phosphoric acid are used as anti-oxidation electroplating liquid, and a product is cleaned and dried by a large amount of pure water; the zinc and chromium alkaline process comprises the following steps: the copper foil is washed by water, zinc sulfate, chromic anhydride and potassium pyrophosphate are added into a surface treatment tank for electroplating, and then a large amount of water washing and drying are carried out; and molybdate passivation technology: the copper foil is washed by water, mixed and electroplated with sodium molybdate, zinc oxide, sodium phosphate and phytic acid, and then washed by a large amount of water and dried.
The oxidation prevention process needs a large amount of pure water for cleaning (the average water consumption in the industry is about 160 tons/ton of copper foil), and a large amount of Cr can be taken away along with the water for cleaning6+、Zn2+、Ni2+The ions can reach the standard and be discharged by a complex wastewater treatment process, and the industrial solid waste residue after filter pressing needs to be treated by a qualification unit, thereby bringing great environmental protection pressure to copper foil manufacturing enterprisesAnd processing costs.
With the increasing demand for environmental protection, copper foil manufacturers tend to develop new environmental protection processes. From the national conditions, in order to break through the national green technology barrier, strengthen the environmental protection, realize the clean production technology of the domestic electrolytic copper foil industry, develop the novel environment-friendly anti-oxidation technology and popularize and apply, adopt advanced technology and equipment, reduce and replace the use amount of toxic and harmful substances, reduce the production amount of the toxic and harmful substances, and are also urgent and unbearable.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an acid environment-friendly anti-oxidation process for electrolytic copper foil, which is simple in process, can enable the copper foil to be free from washing after anti-oxidation treatment, further reduce the consumption of tap water and the manufacturing cost in the manufacturing process of the copper foil, simultaneously enable the surface of the copper foil after anti-oxidation treatment to be free from electroplating other protective metals, further improve the purity of the copper foil and enable the oxidation resistance of the product to reach the prior art standard.
In order to solve the technical problems, the invention adopts the following technical scheme: an acidic environment-friendly anti-oxidation process for electrolytic copper foil, which is characterized by comprising the following steps: the method comprises the following steps of (1),
firstly, preparing an anti-oxidation liquid, and preparing an aqueous solution from 2-mercaptobenzoxazole MBO, glycol, a silane coupling agent, alkanolamine, α -sodium alkenyl sulfonate and water to obtain the anti-oxidation liquid, wherein the concentration of the 2-mercaptobenzoxazole MBO in the aqueous solution is 0.5-2 g/L, the concentration of the glycol is 1-2.5 ml/L, the concentration of the silane coupling agent is 0.8-3.2 ml/L, and the concentration of the alkanolamine is 1-4 ml/L-sodium alkenyl sulfonate is 3-6 g/l;
secondly, pumping the prepared anti-oxidation liquid into an anti-oxidation treatment tank at a certain liquid supply flow rate through a pump, and introducing the electrolytic copper foil into the anti-oxidation liquid for soaking and adsorption for 5-20s after the liquid amount of the anti-oxidation liquid is sufficient;
and finally, guiding the electrolytic copper foil subjected to anti-oxidation liquefaction soaking and adsorption out of the anti-oxidation treatment tank, drying and rolling.
Preferably, the aqueous solution has a concentration of 2-mercaptobenzoxazole MBO of 1.0 g/L, a concentration of ethylene glycol of 2.0 ml/L, a concentration of silane coupling agent of 3.2 ml/L, a concentration of alkanolamine of 1.0 ml/L and a concentration of sodium α -alkenylsulfonate of 4.0 g/l.
After being led out from the anti-oxidation treatment tank, the electrolytic copper foil after being subjected to anti-oxidation liquefaction soaking and adsorption is firstly extruded to extrude out residual liquid on the surface of the electrolytic copper foil, and then is baked.
The equipment for carrying out anti-oxidation treatment on the electrolytic copper foil further comprises a liquid storage tank, a core type filter and a guide roller, wherein the anti-oxidation liquid is filled in the liquid storage tank, the pump is connected with the liquid storage tank through a pipeline, and the core type filter is arranged between the pump and the anti-oxidation treatment tank so as to filter the anti-oxidation liquid; a valve for controlling the flow of the liquid supply is arranged on the pipeline, and the flow of the liquid supply is controlled to be 0.5-1m through the valve3H; the guide roller is arranged along the anti-oxidation treatment tank to guide the electrolytic copper foil into and out of the anti-oxidation treatment tank.
The guide roller comprises a guide roller, a submerged guide roller and a submerged guide roller, and the guide roller is arranged above the anti-oxidation treatment tank; the submerged guide roller and the submerged guide roller are both arranged in the anti-oxidation treatment tank, the submerged guide roller is positioned on one side close to the submerged guide roller, and the submerged guide roller is positioned opposite to the submerged guide roller and used for guiding out the soaked and adsorbed electrolytic copper foil; the submerged guide roller and the submerged guide roller are in the same horizontal position.
An upper liquid squeezing roller and a lower liquid squeezing roller are arranged above the submerged guide roller, are arranged oppositely up and down and are positioned on the anti-oxidation treatment tank, and the electrolytic copper foil guided out by the submerged guide roller is introduced between the upper liquid squeezing roller and the lower liquid squeezing roller to squeeze out residual liquid.
An overflow groove is arranged beside the anti-oxidation treatment groove to receive anti-oxidation liquid overflowing from the anti-oxidation treatment groove; the overflow groove is connected with the liquid storage tank through a pipeline so as to recycle the overflowing anti-oxidation liquid into the liquid storage tank, thereby forming continuous circulation.
The novel surface acid anti-oxidation treatment process with 2-Mercaptobenzoxazole (MBO), glycol, silane coupling agent, alkanolamine and α -sodium alkenyl sulfonate as main components realizes the aims of performing chromium-free anti-oxidation treatment on the lithium electrolytic copper foil, ensuring that the anti-oxidation performance of the product reaches the prior technical standard, reducing the defects of the copper foil and improving the yield, can ensure that the copper foil does not need to be washed after the anti-oxidation treatment, further can reduce the consumption of tap water and the manufacturing cost in the manufacturing process of the copper foil, and simultaneously can ensure that the surface of the copper foil after the anti-oxidation treatment does not need to be plated with other anti-oxidation metals, thereby further improving the purity of the copper foil.
Drawings
FIG. 1 is a schematic view of an apparatus for oxidation-preventing treatment according to the present invention;
FIG. 2 shows the electrolytic copper foil (smooth surface on the left and rough surface on the right) after the high temperature oxidation resistance test.
In the figure, 1 is a liquid storage tank, 2 is a pump, 3 is a valve, 4 is a core filter, 5 is an anti-oxidation treatment tank, 6 is electrolytic copper foil, 7-1 is a lead-in roller, 7-2 is a submerged lead-in roller, 7-3 is a submerged lead-out roller, 7-4 is an upper squeeze roller, 7-5 is a lower squeeze roller, and 8 is an overflow tank.
Detailed Description
The invention will be further illustrated by the following specific examples in conjunction with the accompanying figure 1:
firstly, anti-oxidation treatment:
firstly, 2-Mercaptobenzoxazole (MBO), glycol, a silane coupling agent, alkanolamine, α -sodium alkenyl sulfonate and water are used for preparing an aqueous solution to obtain the anti-oxidation solution, wherein the concentration of the 2-Mercaptobenzoxazole (MBO) in the aqueous solution is 1.0 g/L, the concentration of the glycol is 2.0 ml/L, the concentration of the silane coupling agent is 3.2 ml/L, the concentration of the alkanolamine is 1.0 ml/L and the concentration of the sodium α -alkenyl sulfonate is 4.0 g/l.
Pouring the prepared anti-oxidation liquid into an anti-oxidation liquid storage tank 1, filtering the anti-oxidation liquid by a pump 2 and a pipeline through a core filter 4, conveying the filtered anti-oxidation liquid into an anti-oxidation treatment tank 5, and controlling the flow of the anti-oxidation liquid by using a valve 3, wherein the liquid supply flow of the anti-oxidation liquid is 0.5-1m3H is used as the reference value. The electrolytic copper foil 6 for the lithium ion battery is guided into the anti-oxidation treatment tank 5 through the guide-in roller 7-1, and the electrolytic copper foil 6 is soaked and adsorbed in the anti-oxidation treatment tank for 5-20s through the submerged guide-in roller 7-2 and the submerged guide-out roller 7-3. Electrolytic copper foil soaked in anti-oxidation liquid and adsorbed6, squeezing out redundant anti-oxidation liquid by using an upper liquid squeezing roller 7-4 and a lower liquid squeezing roller 7-5, baking the extruded electrolytic copper foil 6 and then rolling. The overflowing anti-oxidation liquid is received by the overflow groove 8 and then flows back to the anti-oxidation liquid storage tank 1 through a pipeline, so that continuous circulation is formed.
II, experimental verification:
test tool:
small test 100L/1 set (containing titanium anode, stainless steel cathode)
Number of beakers/measuring cylinders/pipettes
Ultrasonic wave dispersion instrument 1
Test chemicals:
2-Mercaptobenzoxazole (MBO), ethylene glycol, silane coupling agent, alkanolamine, α -sodium alkenylsulfonate
Experimental procedure (surface oxidation resistance treatment test step):
(1)100mm × 100mm, 5 μm double-sided smooth copper foil, and weighing;
(2) preparing about 400ml of anti-oxidation treatment liquid according to a test process scheme in a 500ml beaker;
(3) soaking the copper foil in the anti-oxidation liquid for about 20s, taking out and cleaning, placing in a drying oven, baking at 140 ℃ for 15min, and observing the oxidation condition of the surface of the copper foil.
L16 (4) was used in the surface oxidation prevention test5) And (3) an orthogonal table, wherein the four levels of five factors are inspected, and the optimal surface anti-oxidation treatment parameters are determined and verified by observing the influence of the anti-oxidation liquid on the surface appearance of the 5-micron electrolytic copper foil. The orthogonal test table is shown in table 1.
Table 1 orthogonal test table
Test results and analysis:
(1) high temperature oxidation resistance test
And (3) baking the copper foil sample in an oven at 140 ℃ for 15 minutes under different test scheme conditions, observing the oxidation condition of the smooth surface and the rough surface of the copper foil after baking is finished, and determining the high-temperature oxidation resistance of the smooth surface and the rough surface of the copper foil, wherein the test results are shown in Table 2.
Test results after baking at 2140 ℃ for 15min
Observing the surface oxidation condition of the copper foil sample treated under different scheme conditions, and finding that the surface of the copper foil sample treated under the scheme 7 has no oxidation phenomenon after being baked for 15min at 140 ℃, as shown in figure 2, the surface oxidation phenomenon of the copper foil can meet the requirement of high-temperature oxidation resistance of the copper foil, the surface oxidation phenomenon of the copper foil surface treated under the other scheme conditions is serious compared with the light surface, and the requirement of high-temperature oxidation resistance cannot be met.
(2) Wetting Performance test
A plurality of original foil samples (100 × 100mm) without oxidation-resistant liquid are taken and soaked in prepared different oxidation-resistant liquid for 20s, then the original foil samples are taken out for natural air drying, and the surface wettability of the copper foil samples is tested after air drying.
Comprehensively analyzing the anti-oxidation performance and the wettability tested under different anti-oxidation liquid proportioning conditions, and determining the optimal parameters of the surface treatment anti-oxidation liquid as follows:
the present invention has been described in detail, and it should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Claims (7)
1. An acidic environment-friendly anti-oxidation process for electrolytic copper foil, which is characterized by comprising the following steps: the method comprises the following steps of (1),
firstly, preparing an anti-oxidation liquid, and preparing an aqueous solution from 2-mercaptobenzoxazole MBO, glycol, a silane coupling agent, alkanolamine, α -sodium alkenyl sulfonate and water to obtain the anti-oxidation liquid, wherein the concentration of the 2-mercaptobenzoxazole MBO in the aqueous solution is 0.5-2 g/L, the concentration of the glycol is 1-2.5 ml/L, the concentration of the silane coupling agent is 0.8-3.2 ml/L, and the concentration of the alkanolamine is 1-4 ml/L-sodium alkenyl sulfonate is 3-6 g/l;
secondly, pumping the prepared anti-oxidation liquid into an anti-oxidation treatment tank at a certain liquid supply flow rate through a pump, and introducing the electrolytic copper foil into the anti-oxidation liquid for soaking and adsorption for 5-20s after the liquid amount of the anti-oxidation liquid is sufficient;
and finally, guiding the electrolytic copper foil subjected to anti-oxidation liquefaction soaking and adsorption out of the anti-oxidation treatment tank, drying and rolling.
2. The acidic environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 1, wherein the concentration of 2-mercaptobenzoxazole MBO in the aqueous solution is 1.0 g/L, the concentration of ethylene glycol is 2.0 ml/L, the concentration of silane coupling agent is 3.2 ml/L, the concentration of alkanolamine is 1.0 ml/L and the concentration of sodium α -alkenyl sulfonate is 4.0 g/l.
3. The acid environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 1, characterized in that: after being led out from the anti-oxidation treatment tank, the electrolytic copper foil after being subjected to anti-oxidation liquefaction soaking and adsorption is firstly extruded to extrude out residual liquid on the surface of the electrolytic copper foil, and then is baked.
4. The acid environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 3, characterized in that: the equipment for carrying out anti-oxidation treatment on the electrolytic copper foil further comprises a liquid storage tank, a core type filter and a guide roller, wherein the anti-oxidation liquid is filled in the liquid storage tank, the pump is connected with the liquid storage tank through a pipeline, and the core type filter is arranged between the pump and the anti-oxidation treatment tank so as to filter the anti-oxidation liquid; a valve for controlling the flow of the liquid supply is arranged on the pipeline, and the flow of the liquid supply is controlled to be 0.5-1m through the valve3H; the guide roller is arranged along the anti-oxidation treatment tank to guide the electrolytic copper foil into and out of the anti-oxidation treatment tank.
5. The acid environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 4, characterized in that: the guide roller comprises a guide roller, a submerged guide roller and a submerged guide roller, and the guide roller is arranged above the anti-oxidation treatment tank; the submerged guide roller and the submerged guide roller are both arranged in the anti-oxidation treatment tank, the submerged guide roller is positioned on one side close to the submerged guide roller, and the submerged guide roller is positioned opposite to the submerged guide roller and used for guiding out the soaked and adsorbed electrolytic copper foil; the submerged guide roller and the submerged guide roller are in the same horizontal position.
6. The acid environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 5, characterized in that: an upper liquid squeezing roller and a lower liquid squeezing roller are arranged above the submerged guide roller, are arranged oppositely up and down and are positioned on the anti-oxidation treatment tank, and the electrolytic copper foil guided out by the submerged guide roller is introduced between the upper liquid squeezing roller and the lower liquid squeezing roller to squeeze out residual liquid.
7. The acid environment-friendly type oxidation preventing process for electrolytic copper foil according to claim 4, characterized in that: an overflow groove is arranged beside the anti-oxidation treatment groove to receive anti-oxidation liquid overflowing from the anti-oxidation treatment groove; the overflow groove is connected with the liquid storage tank through a pipeline so as to recycle the overflowing anti-oxidation liquid into the liquid storage tank.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114808045A (en) * | 2022-03-29 | 2022-07-29 | 江西铜博科技有限公司 | High-toughness winding-resistant ultrathin lithium battery copper foil and production process thereof |
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| JPH08311658A (en) * | 1995-05-17 | 1996-11-26 | Nippon Parkerizing Co Ltd | Composition for surface treatment of copper based metallic material |
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| CN105039947A (en) * | 2015-07-07 | 2015-11-11 | 安徽铜冠铜箔有限公司 | Oxidation prevention process used for lithium ion battery copper foil |
| CN105386106A (en) * | 2015-11-25 | 2016-03-09 | 青海电子材料产业发展有限公司 | Lithium electric copper foil anti-oxidization liquid and anti-oxidization treatment technology |
| CN107163844A (en) * | 2017-05-16 | 2017-09-15 | 江南大学 | A kind of antirust agent and preparation method and application |
| CN109161881A (en) * | 2018-09-20 | 2019-01-08 | 惠州联合铜箔电子材料有限公司 | The anti-oxidation liquid of a kind of Chrome-free of electrolytic copper foil and without washing anti-oxidation technique |
-
2020
- 2020-04-27 CN CN202010342533.3A patent/CN111472005B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08311658A (en) * | 1995-05-17 | 1996-11-26 | Nippon Parkerizing Co Ltd | Composition for surface treatment of copper based metallic material |
| CN103194744A (en) * | 2013-04-22 | 2013-07-10 | 江西铜业股份有限公司 | Copper foil surface passivation liquid and treatment method thereof, and treated copper foil |
| CN105039947A (en) * | 2015-07-07 | 2015-11-11 | 安徽铜冠铜箔有限公司 | Oxidation prevention process used for lithium ion battery copper foil |
| CN105386106A (en) * | 2015-11-25 | 2016-03-09 | 青海电子材料产业发展有限公司 | Lithium electric copper foil anti-oxidization liquid and anti-oxidization treatment technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114808045A (en) * | 2022-03-29 | 2022-07-29 | 江西铜博科技有限公司 | High-toughness winding-resistant ultrathin lithium battery copper foil and production process thereof |
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