Method and device capable of improving copper dissolving efficiency for electrolytic copper foil

Abstract

The invention discloses a method and device capable of improving the copper dissolving efficiency for electrolytic copper foils, and relates to the technical field of electrolytic copper foil production, and the method comprises the following specific steps: step 1, adding a copper wire into a copper dissolving tank, and then sealing a feeding port; 2, a circulating pump is started, and a dissolving solution is added into the copper dissolving tank; 3, heating equipment is started to heat the copper dissolving tank, and after the dissolved solution is heated to 50-60 DEG C, heating operation is stopped; 4, compressed air is introduced into the copper dissolving tank; 5, SO2 is introduced into the compressed air; 6, after the copper wire is dissolved for 3.5-4.5 h, the Cu < 2 + > concentration of the dissolving solution in the copper dissolving tank reaches 86 g / L, and the production requirement of the next procedure is met; and 7, conveying the qualified copper sulfate solution to the next process for production. According to the method and device capable of improving the copper dissolving efficiency for the electrolytic copper foil, the spraying mode is changed on the tank body part, the spraying head 6 is additionally arranged, the spraying area is increased, and therefore the copper dissolving efficiency is improved.

Description

Technical Field

[0001] The invention relates to the technical field of electrolytic copper foil production, in particular to a method and a device for improving copper dissolving efficiency for electrolytic copper foil. Background Art

[0002] At present, copper dissolution mainly adopts two methods: immersion copper dissolution and spray copper dissolution. Immersion copper dissolution is to cut the raw copper plate into small pieces or melt it into wires and put it into the copper dissolution tank. The sulfuric acid aqueous solution and compressed air enter from the bottom of the tank. After being heated by the shell and tube heat exchanger, they slowly flow from the gap between the copper blocks in a "Y", "Z" and "S" shape from bottom to top. During the flow process, it contacts the surface of the copper block and undergoes a chemical reaction. Spray copper dissolution sprays sulfuric acid onto the copper plate through a nozzle, so that copper reacts with sulfuric acid to form copper sulfate. The advantage of this method is that the surface of the copper plate can be treated more evenly, and the reaction speed and efficiency can be better controlled. Generally, copper foil companies use immersion copper dissolution to treat waste foil. However, since the waste foil is piled together and put into the copper dissolution tank, the surface area of ​​the copper foil in contact with the sulfuric acid liquid is limited, which greatly limits the copper dissolution rate. Therefore, improving the copper dissolution rate is of great significance to the production of copper foil. Summary of the invention

[0003] The purpose of the present invention is to provide an invention for accelerating copper dissolution, so as to solve the technical problem that the surface area of ​​copper foil in contact with sulfuric acid liquid is limited, which limits the rate of copper dissolution. Studies have found that dispersing and spraying the copper solution while introducing air can accelerate the dissolution of copper in sulfuric acid solution, thereby achieving the purpose of increasing the copper dissolution rate.

[0004] To achieve the above objectives, the present invention is implemented by the following technical scheme: A method for improving copper dissolving efficiency for electrolytic copper foil, comprising the following specific steps:

[0005] Step 1: Add the copper wire into the copper dissolving tank and then close the feeding port;

[0006] Step 2: Turn on the circulation pump and add the dissolving liquid into the copper dissolving tank;

[0007] Step 3: Turn on the heating equipment to heat the copper dissolving tank, and stop the heating operation after the dissolving liquid is heated to 50-60°C;

[0008] Step 4: Introduce compressed air into the copper dissolving tank;

[0009] Step 5: Introduce SO2 into the compressed air at a flow rate of 5.0m 3 / h, the inlet pressure is set to 0.25Mpa;

[0010] Step 6: After the copper wire is dissolved for 3.5-4.5 hours, the copper dissolving tank dissolves the Cu 2+When the concentration reaches 86g / L, it meets the production requirements of the next process;

[0011] Step 7: Send the qualified copper sulfate solution to the next process for production.

[0012] Optionally, in step 1, the diameter of the copper wire is set to 1±0.1 mm, the length is set to 600±10 mm, and the size of the copper melting tank is φ2500×4000 mm;

[0013] The added mass of the raw materials is 4.5-5.3 tons, and the stacking thickness of the material layer is 1.5±0.1m.

[0014] Optionally, the dissolving solution in step 2 is composed of a mixture of sulfuric acid, water and copper sulfate solution;

[0015] The sulfuric acid concentration is 85±5g / L, Cu 2+ The concentration is 10±1g / L and the volume of the solution is 14.5m 3 When the concentration of sulfuric acid in the solution is lower than 20g / L, it needs to be replenished again.

[0016] Optionally, the compressed air flow rate in step 4 is 120m 3 / h, the internal pressure is 0.25Mpa.

[0017] A device for improving the copper dissolving efficiency for electrolytic copper foil as claimed in any one of the above claims, comprising a tank body, a top cover is provided on the top of the tank body, a spray pipe and a bottom plate are provided on the top of the tank body, the spray pipe is located above the bottom plate, a support plate connected to the inside of the tank body is provided below the bottom plate, and a plurality of spray heads are provided on the side wall of the spray pipe;

[0018] The tank body is also provided with a circulating liquid mechanism;

[0019] The circulating liquid mechanism includes a recovery pipe located at the bottom end of the tank body, one side of the recovery pipe is connected to one end of a return pipe, the return pipe passes through the bottom end of the tank body, the other end of the return pipe passes through the top cover, and a lifting pump is provided in the middle of the return pipe.

[0020] Optionally, the tank body, the top cover and the spray pipe are coaxially distributed.

[0021] Optionally, the spray pipe and the recovery pipe are both designed to be ring-shaped.

[0022] Optionally, the spray heads are provided in four groups along the spray pipe path, and the angles between the spray pipes in each group are 20°.

[0023] Optionally, the axis of the lowest spray head is parallel to the axis of the tank body.

[0024] The present invention provides a method and device for improving the copper dissolving efficiency of electrolytic copper foil, which has the following features:

[0025] Beneficial effects:

[0026] The method and device for improving copper dissolving efficiency of electrolytic copper foil increases the spraying area by changing the spraying mode and adding a spray head 6 in the tank body, thereby improving the copper dissolving efficiency.

[0027] By installing an O-type tube and a perforated tube at the bottom of a traditional high-efficiency copper dissolving tank, and connecting a spray pump to the O-type tube, the suction force at the holes of the perforated tube can suck the copper scraps impurities in the copper sulfate solution into the pipeline and perform secondary dissolution, thereby effectively reducing the copper scraps impurity content in the copper sulfate solution and improving the purity of the copper sulfate solution.

[0028] The use of low-temperature copper dissolution can reduce the corrosion loss of acidic liquid to the equipment, and reduce the evaporation and loss of sulfuric acid and copper ions caused by high temperature; the spray-type fast and efficient copper dissolution system has a simple structure and is easy to maintain. The copper dissolution speed can be controlled on demand by switching the exhaust system and adjusting the spray flow. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a front view full cross-sectional schematic diagram of the invention;

[0030] Figure 2 It is a partially enlarged schematic diagram of the spray pipe in the invention.

[0031] In the figure: 1. tank body; 2. top cover; 3. spray pipe; 4. bottom plate; 5. support plate; 6. spray head; 7. circulating liquid mechanism; 701. recovery pipe; 702. reflux pipe; 703. lifting pump. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0033] In the description of the present invention, unless otherwise specified, "plurality" means two or more than two; the orientations or positional relationships indicated by the terms "upper", "lower", "left", "right", "inner", "outer", "front end", "rear end", "head", "tail", etc. are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", "third", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0034] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0035] A method for improving copper dissolving efficiency for electrolytic copper foil comprises the following specific steps:

[0036] Step 1: Add the copper wire into the copper dissolving tank, and then close the feeding port. The diameter of the copper wire is set to 1 mm, the length is set to 600 mm, and the size of the copper dissolving tank is φ2500×4000 mm;

[0037] The added mass of raw materials is 5.05 tons, and the thickness of the material layer is 1.53m;

[0038] Step 2: Turn on the circulation pump and add a dissolving solution into the copper dissolving tank, wherein the dissolving solution is a mixture of sulfuric acid, water and copper sulfate solution;

[0039] The sulfuric acid concentration is 86g / L, Cu 2+ The concentration is 9.8g / L and the volume of the solution is 14.5m 3 When the concentration of sulfuric acid in the solution is lower than 20g / L, it needs to be replenished again;

[0040] Step 3: Turn on the heating equipment to heat the copper dissolving tank, and stop the heating operation after the dissolving liquid is heated to 53.8°C;

[0041] Step 4: Introduce compressed air into the copper dissolving tank with a compressed air flow rate of 120m 3 / h, internal pressure is 0.25Mpa;

[0042] Step 5: Introduce SO2 into the compressed air at a flow rate of 5.0m 3 / h, the inlet pressure is set to 0.25Mpa;

[0043] Step 6: After the copper wire is dissolved for 3.8 hours, the copper dissolving tank dissolves the Cu 2+ When the concentration reaches 86g / L, it meets the production requirements of the next process;

[0044] Step 7: Send the qualified copper sulfate solution to the next process for production.

[0045] See also Figure 1, a device for improving copper dissolving efficiency for electrolytic copper foil, comprising a tank body 1, a top cover 2 is provided on the top of the tank body 1, a spray pipe 3 and a bottom plate 4 are provided on the top of the tank body 1, the spray pipe 3 is located above the bottom plate 4, a support plate 5 connected to the inside of the tank body 1 is provided below the bottom plate 4, and a plurality of spray heads 6 are provided on the side wall of the spray pipe 3;

[0046] A circulating liquid mechanism 7 is also provided inside the tank body 1;

[0047] The circulating liquid mechanism 7 includes a recovery pipe 701 located at the bottom end of the tank body 1, one side of the recovery pipe 701 is connected to one end of a return pipe 702, the return pipe 702 passes through the bottom end of the tank body 1, and the other end of the return pipe 702 passes through the top cover 2. A lifting pump 703 is provided in the middle of the return pipe 702.

[0048] In this embodiment, Figure 1 As shown, the tank body 1, the top cover 2 and the spray pipe 3 are coaxially distributed.

[0049] In this embodiment, Figure 1 As shown, the spray pipe 3 and the recovery pipe 701 are both designed in an annular shape.

[0050] In this embodiment, Figure 1 As shown, four groups of spray heads 6 are provided along the spray pipe 3 path, and the angle between each group of spray pipes 3 is 20°.

[0051] In this embodiment, Figure 1 As shown, the axis of the lowest spray head 6 is parallel to the axis of the tank body 1 .

[0052] Designing a circulating liquid pipeline can realize the recycling of spraying, thereby solving the problems of insufficient copper material reaction and poor reaction liquid circulation in existing spray copper dissolving equipment;

[0053] The spray heads 6 at the bottom of the spray pipe 3 are internal spray heads 6, and the axis of each internal spray head 6 passes through the center of the spray pipe 3. The internal spray heads 6 are divided into four categories: the first group of internal spray heads 6 are located at the bottom of the spray pipe 3, biased toward the innermost side, and the angle between the axis direction and the vertical direction is 60°; the second group of spray heads 6 are located at the bottom of the spray pipe 3, biased toward the inner side, and the angle between the axis direction and the vertical direction is 40°; the third group of spray heads 6 are located in the middle of the spray pipe 3, and the angle between the axis direction and the vertical direction is 20°; the fourth group of spray heads 6 are located at the very bottom of the spray pipe 3, and the angle between the axis direction and the vertical direction is 0°.

[0054] The present invention can also add a switch exhaust system and adjust the spray flow rate, thereby controlling the copper dissolving speed on demand. The spray-type fast and efficient copper dissolving system has a simple structure and is easy to maintain.

[0055] When in use, metallic copper is taken as the solid phase and sulfuric acid solution is taken as the liquid phase and put into a copper dissolving tank; compressed air is injected into the copper dissolving tank by starting the air compressor, and the copper material gradually dissolves to form a copper sulfate solution; excess air and acid mist generated in the process are extracted through an exhaust pipe; in addition, the solution is heated by a heat exchanger, and sulfuric acid solution is continuously added, so that the copper sulfate solution enters the second copper dissolving tank from the overflow port of the first copper dissolving tank, and a secondary copper dissolving operation is carried out to eliminate the influence of monovalent copper ions on the quality of copper foil.

[0056] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for improving copper dissolving efficiency for electrolytic copper foil, characterized in that: The specific steps include: Step 1: Add the copper wire into the copper dissolving tank and then close the feeding port; Step 2: Turn on the circulation pump and add the dissolving liquid into the copper dissolving tank; Step 3: Turn on the heating equipment to heat the copper dissolving tank, and stop the heating operation after the dissolving liquid is heated to 50-60°C; Step 4: Introduce compressed air into the copper dissolving tank; Step 5: Introduce SO2 into the compressed air at a flow rate of 5.0m 3 / h, the inlet pressure is set to 0.25Mpa; Step 6: After the copper wire is dissolved for 3.5-4.5 hours, the copper dissolving tank dissolves the Cu 2+ When the concentration reaches 86g / L, it meets the production requirements of the next process; Step 7: Send the qualified copper sulfate solution to the next process for production.

2. A method for improving copper dissolving efficiency for electrolytic copper foil according to claim 1, characterized in that: In the step 1, the diameter of the copper wire is set to 1±0.1 mm, the length is set to 600±10 mm, and the size of the copper melting tank is φ2500×4000 mm; The added mass of the raw materials is 4.5-5.3 tons, and the stacking thickness of the material layer is 1.5±0.1m.

3. The method for improving copper dissolving efficiency for electrolytic copper foil according to claim 1, characterized in that: In the step 2, the dissolving solution is composed of a mixture of sulfuric acid, water and copper sulfate solution; The sulfuric acid concentration is 85±5g / L, Cu 2+ The concentration is 10±1g / L and the volume of the solution is 14.5m 3 When the concentration of sulfuric acid in the solution is lower than 20g / L, it needs to be replenished again.

4. A method for improving copper dissolving efficiency for electrolytic copper foil according to claim 1, characterized in that: The compressed air flow rate in step 4 is 120m 3 / h, the internal pressure is 0.25Mpa.

5. A device for improving copper dissolving efficiency for electrolytic copper foil as claimed in any one of claims 1 to 4, comprising a tank (1), characterized in that: The top of the tank body (1) is provided with a top cover (2), the top of the tank body (1) is provided with a spray pipe (3) and a bottom plate (4), the spray pipe (3) is located above the bottom plate (4), a support plate (5) connected to the inside of the tank body (1) is provided below the bottom plate (4), and a plurality of spray heads (6) are provided on the side wall of the spray pipe (3); A circulating liquid mechanism (7) is also provided inside the tank body (1); The circulating liquid mechanism (7) comprises a recovery pipe (701) located at the bottom end of the tank body (1), one side of the recovery pipe (701) is connected to one end of a return pipe (702), the return pipe (702) passes through the bottom end of the tank body (1), the other end of the return pipe (702) passes through the top cover (2), and a lift pump (703) is provided in the middle of the return pipe (702).

6. A method and device for improving copper dissolving efficiency for electrolytic copper foil according to claim 5, characterized in that: The tank body (1), the top cover (2) and the spray pipe (3) are coaxially distributed.

7. A method and device for improving copper dissolving efficiency for electrolytic copper foil according to claim 5, characterized in that: The spray pipe (3) and the recovery pipe (701) are both designed in an annular shape.

8. A method and device for improving copper dissolving efficiency for electrolytic copper foil according to claim 5, characterized in that: The spray heads (6) are arranged in four groups along the spray pipe (3) path, and the angle between each group of spray pipes (3) is 20°.

9. A method and device for improving copper dissolving efficiency for electrolytic copper foil according to claim 5, characterized in that: The axis of the lowest spray head (6) is parallel to the axis of the tank body (1).

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