High-purity copper continuous electrolytic refining equipment
By setting up a rotating electrolytic wall and independent electrolytic interval in the electrolytic cell, the problems of large investment in existing equipment, long process time and difficulty in removing impurities are solved, and efficient and continuous high-purity copper production is achieved, ensuring high-purity electrolytic copper output.
Patent Information
- Application Number
- CN202411978076.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-11
AI Technical Summary
The existing equipment for producing high-purity electrolytic copper with electrolytic methods has problems such as large equipment investment, long process time and difficulty in control. The multiple electrolytic technology is complicated and it is difficult to effectively remove impurities, resulting in the purity of high-purity copper produced by it being difficult to reach 99.999% or above.
A high-purity copper continuous electrolytic refining device is adopted. By setting a rotating electrolytic wall, anode plate and cathode plate parallel to each other in the electrolytic cell, a plurality of independent electrolytic intervals are formed, each interval is equipped with a separate DC power supply, and the electrolytic intervals are separated by the interlaced and rotating metal rod and the elastic glue rod to achieve continuous electrolysis and efficient impurity removal.
The continuous electrolytic production of high-purity copper has been achieved, which significantly improves the production efficiency of high-purity copper. It can ensure that the purity of electrolytic copper output reaches 99.99% and above when the raw material purity is 99.99%, and the electrolytic process is optimized, reducing energy consumption and raw material waste, and reducing production costs.
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Figure CN119800455A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of equipment for producing metals by electrolysis, and specifically relates to a high-purity copper continuous electrolytic refining equipment for preparing high-purity electrolytic copper by realizing multiple continuous electrolytic refining through a single tank body. Background Art
[0002] High-purity oxygen-free copper, as an extremely pure copper material, ensures its unique physical properties. High-purity oxygen-free copper not only has good electrical and thermal conductivity, and can play a key role in high-speed electronic transmission and efficient heat energy conduction, but also has excellent ductility and processing performance. High-purity oxygen-free copper also exhibits excellent corrosion resistance, low-temperature stability and weather resistance, and can maintain stable performance in various harsh environments. These unique advantages make high-purity oxygen-free copper widely used in high-tech fields such as electronic chips, semiconductor industry, liquid crystal display, electrical, chemical, automobile, aerospace and new energy.
[0003] Electrolytic copper is produced by electrolysis, with crude copper (copper containing impurities) as the anode, stainless steel or titanium plate as the cathode, and copper sulfate or copper nitrate solution and corresponding acid as the electrolyte. During the electrolysis process, the crude copper at the anode will gradually dissolve, and the copper ions (Cu 2+ ) will enter the electrolyte, while impurity metals that are more active than copper will enter the electrolyte in the form of metal cations, and some inactive metals will be deposited at the bottom of the electrolytic cell in solid form to form anode mud. 2+ ) will get electrons, be reduced to metallic copper, and be deposited on the cathode. In this way, the crude copper can be purified by electrolysis to obtain pure copper. Some trace impurities, such as silver and other impurities, are partially dissolved in the solution and then enter the cathode copper through electrolysis. The impurities in the cathode copper are high. As time goes by, the content of silver in the electrolyte continues to increase, causing the impurities in the cathode copper to continue to increase. Some impurities are mainly mechanically mixed into the cathode copper, and some impurities are also mixed in the gaps between the grains. In order to obtain high-purity copper, multiple electrolysis technology is often used at present, that is, after electrolyzing a cell body, the cathode copper of this cell body is placed as the anode in the second cell body. If you want to get a higher level of cathode copper, the cathode copper of the second electrolysis is used as the anode and electrolyzed again in the third cell body. This is more complicated, the equipment investment is large, the process time is long, and the control is more difficult. The present invention aims to provide a new type of high-purity copper continuous electrolytic refining equipment to solve these problems. Summary of the invention
[0004] In view of the problems existing in the background technology, the present invention provides a high-purity copper continuous electrolytic refining equipment, the technical scheme includes: an anode plate, a cathode plate, an electrolytic cell, a rotating electrolytic wall and a DC power supply, wherein the rotating electrolytic wall, the anode plate and the cathode plate are arranged parallel to each other along the width direction of the electrolytic cell, and the anode plate and the cathode plate are arranged at both ends of the length direction of the electrolytic cell respectively; at least one rotating electrolytic wall is arranged in the area between the anode plate and the cathode plate in the electrolytic cell, each of the rotating electrolytic walls divides the electrolytic cell into two electrolytic intervals in the length direction, and each of the electrolytic intervals is filled with electrolyte;
[0005] The rotating electrolytic wall comprises: a rotating mechanism, a torque transmission mechanism, a rod mounting frame, an electrical connection member, a metal rod and an elastic rubber rod, the two ends of the rod mounting frame are fixed to the tank wall of the fixed electrolytic tank, the upper ends of the metal rod and the elastic rubber rod are rotatably connected to the rod mounting frame, the lower ends of the metal rod and the elastic rubber rod are rotatably connected to the tank bottom of the electrolytic tank in a sealed manner, and the upper ends of the metal rod and the elastic rubber rod are connected to the rotating mechanism through the torque transmission mechanism;
[0006] Each electrolysis zone is provided with a separate DC power supply, the metal rod is connected to the DC power supply through an electrical connection member, and the anode plate and the cathode plate are connected to the DC power supply of the electrolysis zone to which they belong.
[0007] The interior of the electrolytic cell is a rectangular parallelepiped space.
[0008] The metal rods and elastic rubber rods with the same outer diameter are arranged alternately along the width direction of the electrolytic cell, the elastic rubber rods are pressed tightly against the structures in contact with both sides, and the metal rods, the elastic rubber rods and the bottom of the electrolytic cell are also sealed;
[0009] The structure in contact at both sides is a metal rod or a side wall of an electrolytic cell.
[0010] The outer diameters of the metal rod and the elastic rubber rod are 20 to 30 mm.
[0011] The metal rod is a copper rod or a titanium rod.
[0012] The cathode plate is a stainless steel plate or a titanium plate.
[0013] The distance between the anode plate and the rotating electrolysis wall is 70mm-100mm, and the distance between the cathode plate and the rotating electrolysis wall is 70mm-100mm.
[0014] When the number of the rotating electrolysis walls exceeds one, the distance between adjacent rotating electrolysis walls 200 is 70-90 mm.
[0015] The current density in each electrolysis zone is the voltage divided by the contact area between the electrolyte and the cathode metal, where the cathode metal is the cathode plate connected to the negative pole of the DC power supply at both ends of the electrolysis zone, or the metal rod of the rotating electrolysis wall.
[0016] The current density in the electrolysis space is controlled to be 100-200A / m 2 .
[0017] The beneficial effects of the present invention are:
[0018] 1. The present invention separates the electrolysis intervals by staggered and simultaneously rotating elastic rubber rods and metal rods, thereby achieving continuity and high efficiency of the electrolysis operation and significantly improving the production efficiency of high-purity copper.
[0019] 2. The present invention deeply removes impurities by sequentially arranging relatively independent electrolysis zones, and ensures that the purity of the output electrolytic copper reaches 99.999% or above when the purity of the raw materials is 99.99%; and the purity of the product can be increased by continuously increasing the separation tank bodies (rotating electrolysis walls and electrolysis zones).
[0020] 3. The present invention optimizes the electrolysis process, reduces energy consumption, waste of raw materials and equipment downtime, and effectively reduces the overall production cost. At the same time, the equipment is reasonably designed and easy to maintain. It is suitable for all electrolytically purified metals, such as gold, silver, nickel, etc., thereby further compressing the initial investment and later operating costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a top view schematic diagram of Example 1 of a high-purity copper continuous electrolytic refining equipment of the present invention.
[0022] Figure 2 It is a front view schematic diagram of embodiment 1 of the present invention.
[0023] Figure 3 It is a top view schematic diagram of embodiment 2 of the present invention.
[0024] Among them, 100-electrolytic cell, 200-rotating electrolytic wall, 300-electrolytic interval, 1-driving motor, 2-elastic rubber rod, 3-electrical connection component, 4-cathode plate, 5-metal rod, 6-control power supply, 7-anode plate, 8-rod mounting frame, 9-torque transmission mechanism. DETAILED DESCRIPTION
[0025] The present invention is further described in detail below in conjunction with the accompanying drawings.
[0026] like Figure 1 and Figure 2The embodiment 1 of the present invention shown in the figure comprises: an anode plate 7, a cathode plate 4, an electrolytic cell 100, a rotating electrolytic wall 200 and a DC power supply 6, wherein the interior of the electrolytic cell 100 is a rectangular parallelepiped, and the rotating electrolytic wall 200, the anode plate 7 and the cathode plate 4 are arranged parallel to each other along the width direction of the electrolytic cell 100, and the anode plate 7 and the cathode plate 4 are arranged at both ends of the length direction of the electrolytic cell 100 respectively; at least one rotating electrolytic wall 200 is arranged in the area between the anode plate 7 and the cathode plate 4 in the electrolytic cell, and each of the rotating electrolytic walls 200 divides the electrolytic cell 100 into two electrolytic sections 300 in the length direction, and each of the electrolytic sections 300 is filled with the same or different electrolytes according to the process, and each electrolytic section 300 is provided with a separate DC power supply 6, and the anode plate 7 and the cathode plate 4 are connected to the DC power supply 6 of the electrolytic section to which they belong;
[0027] The rotating electrolysis wall 200 comprises: a rotating mechanism 1, a torque transmission mechanism 9, a rod mounting frame 8, an electrical connection component 3, a metal rod 5 and an elastic rubber rod 2, both ends of the rod mounting frame 8 are fixed to the tank wall of the fixed electrolytic tank 100, the upper ends of the metal rod 5 and the elastic rubber rod 2 are rotatably connected to the rod mounting frame 8, the lower ends of the metal rod 5 and the elastic rubber rod 2 are rotatably connected to the tank bottom of the electrolytic tank 100, the upper ends of the metal rod 5 and the elastic rubber rod 2 are connected to the rotating mechanism 1 through the torque transmission mechanism 9 so as to rotate simultaneously under the drive of the rotating mechanism 1; the metal rod 5 is connected to the DC power supply 6 through the electrical connection component 3;
[0028] The metal rod 5 and the elastic rubber rod 2 with the same outer diameter are arranged alternately along the width direction of the electrolytic cell 100, and the elastic rubber rod 2 and the structures on both sides (the metal rod 5 or the side wall of the electrolytic cell 100) are kept tightly pressed. At the same time, the metal rod 5 and the elastic rubber rod 2 are also kept sealed (pressed) with the bottom of the electrolytic cell 100, thereby ensuring that the electrolytes in different electrolytic intervals 300 are not mixed, thereby effectively isolating the anode mud; the combination of the metal rod and the elastic rubber rod can maintain the separation of the electrolytic intervals during rotation, and at the same time allow the side with precipitated copper to transfer from one electrolytic interval to another; the current density in each electrolytic interval is the contact area between the electrolyte and the cathode metal, wherein the cathode metal is the cathode plate 4 connected to the negative pole of the DC power supply 6 at both ends of the electrolytic interval, or the metal rod of the rotating electrolytic wall 200.
[0029] In this embodiment, the electrical connection member 3 is a copper rod fixed to the rod mounting frame 8, and the metal rod 5 is connected to the DC power supply 6 by means of a brush.
[0030] The torque transmission mechanism 9 is a transmission mechanism such as a gear transmission, a chain transmission or a belt transmission. In this embodiment, a gear transmission is specifically selected.
[0031] The metal rod 5 is one of a copper rod and a titanium rod. In this embodiment, the copper rod is selected.
[0032] The cathode plate 4 is one of a stainless steel plate and a titanium plate. In this embodiment, a titanium plate is selected.
[0033] In this embodiment, two rotating electrolysis walls 200 are provided; the distance between the anode plate 7 and the rotating electrolysis wall 200 is 70 mm-100 mm, the distance between the cathode plate 4 and the rotating electrolysis wall 200 is 70 mm-100 mm, and the distance between adjacent rotating electrolysis walls is 70-90 mm; at the same time, the current density in the electrolysis space 300 is controlled at 100-200 A / m 2 each rotating electrolytic wall 200, the outer diameter of the metal rod 5 and the elastic rubber rod 2 is 20 to 30 mm.
[0034] When working,
[0035] Step 1: First, inject the pre-prepared electrolyte mother solution (the initial electrolyte is a mixed solution containing 35g / L sulfuric acid and 50g / L copper sulfate) into each electrolysis interval, and the liquid level is maintained at 2\3 to 3\4 of the electrolytic cell; the copper sulfate is high-purity copper sulfate.
[0036] Step 2: Start all output power supplies 8 and drive motor 1 to start electrolysis;
[0037] At this time, in the first electrolysis interval, the DC power supply 6 is set to a current density of 200A / m 2 The rotation speed of the first row of rotating electrolytic walls 200 is set to 10 revolutions per minute; its purpose is to remove impurities in copper; the elastic rubber rod 2 and the metal rod 5 (pure copper rod) are driven by the driving motor 1 through the gear chain to rotate, and the side with the precipitated copper is transferred to the next electrolytic interval;
[0038] At the same time, in the second electrolysis interval, set the DC power supply 6 electrolysis parameter current density to 200A / m 2 , the rotation speed of the second rotating electrolysis wall 200 is set to 15 revolutions per minute; further electrolysis is performed;
[0039] At the same time, in the third electrolysis interval, set the DC power supply 6 electrolysis parameter current density to 200A / m 2 , further electrolysis is performed to remove copper attached to the cathode plate 4;
[0040] Step 3: When the copper deposited on the cathode plate of the last area reaches the required thickness, the electrolysis process is stopped and the DC power supply is turned off.
[0041] Step 4: Finally, carefully peel off the precipitated copper from the cathode plate to avoid damaging its surface.
[0042] Step 5: Perform preliminary rinsing to remove electrolyte and impurities attached to the surface: Use deionized water for thorough cleaning to ensure the purity of the precipitated copper surface. Perform pickling on the cleaned copper plate, using a 1% nitric acid solution to clean the surface oxides and residues. Pay attention to controlling the pickling time and temperature to avoid excessive corrosion. After pickling, rinse with running ultrapure water for more than three times to remove residual acid on the surface; the last step is to use alcohol ultrasonic rinse and dry the package.
[0043] Step 6: Test the produced electrolytic copper. Please see Table 1 below for the test results of key impurity indicators. It can be seen from the test results that when the purity of the raw materials is 99.99%, the purity of the produced electrolytic copper reaches 99.9999%.
[0044] Table 1 Test results of key impurity indicators of electrolytic copper in Example 1
[0045]
[0046] In the above step 2 in Example 1, as the electrolysis time increases, the resistance in the solution changes (such as the influence of anode mud), resulting in an increase in current. As the electrolysis time increases, the rotation rate can be adjusted accordingly; but it is necessary to ensure that in each of two adjacent electrolysis intervals 300, the current density of the electrolysis interval 300 close to the cathode plate 4 is not less than the current density of the electrolysis interval 300 close to the anode plate 7.
[0047] like Figure 3 The embodiment 2 of the present invention shown in the figure is different from the embodiment 1 in that a rotating electrolysis wall 200 is provided between the anode plate 7 and the cathode plate 4;
[0048] In this embodiment, the distance between the anode plate 7 and the rotating electrolysis wall 200 is also 70mm-100mm, the distance between the cathode plate 4 and the rotating electrolysis wall 200 is also 70mm-100mm, and the current density in the electrolysis space 300 is controlled at 100-200A / m 2 in the rotating electrolysis wall 200, the outer diameter of the metal rod 5 and the elastic rubber rod 2 is 20 to 30 mm.
[0049] The process during operation is the same as in Example 1, except that there are only two electrolysis intervals in step 2.
[0050] In step 6, the electrolytic copper produced is tested. The test results of key impurity indicators are shown in Table 2 below. It can be seen from the test results that when the purity of the raw materials is 99.99%, the purity of the electrolytic copper produced reaches 99.999%.
[0051] Table 2 Test results of key impurity indicators of electrolytic copper in Example 2
[0052]
Claims
1. A high-purity copper continuous electrolytic refining equipment, characterized in that: include: An anode plate (7), a cathode plate (4), an electrolytic cell (100), a rotating electrolytic wall (200) and a direct current power source (6), wherein the rotating electrolytic wall (200), the anode plate (7) and the cathode plate (4) are arranged parallel to each other along the width direction of the electrolytic cell (100), and the anode plate (7) and the cathode plate (4) are arranged at two ends of the length direction of the electrolytic cell (100) respectively; at least one rotating electrolytic wall (200) is arranged in the area between the anode plate (7) and the cathode plate (4) in the electrolytic cell, and each of the rotating electrolytic walls (200) divides the electrolytic cell (100) into two electrolytic sections (300) in the length direction, and each of the electrolytic sections (300) is filled with electrolyte; The rotating electrolysis wall (200) comprises: a rotating mechanism (1), a torque transmission mechanism (9), a rod mounting frame (8), an electrical connection member (3), a metal rod (5) and an elastic rubber rod (2); both ends of the rod mounting frame (8) are fixed to the tank wall of the fixed electrolytic tank (100); the upper ends of the metal rod (5) and the elastic rubber rod (2) are rotationally connected to the rod mounting frame (8); the lower ends of the metal rod (5) and the elastic rubber rod (2) are sealingly rotationally connected to the tank bottom of the electrolytic tank (100); and the upper ends of the metal rod (5) and the elastic rubber rod (2) are connected to the rotating mechanism (1) via the torque transmission mechanism (9); Each electrolysis zone (300) is provided with a separate DC power supply (6), the metal rod (5) is connected to the DC power supply (6) via an electrical connection member (3), and the anode plate (7) and the cathode plate (4) are connected to the DC power supply (6) of the corresponding electrolysis zone.
2. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The interior of the electrolytic cell (100) is a rectangular parallelepiped space.
3. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The metal rods (5) and the elastic rubber rods (2) having the same outer diameter are arranged alternately along the width direction of the electrolytic cell (100), the elastic rubber rods (2) and the structures in contact with both sides are kept tightly pressed, and the metal rods (5) and the elastic rubber rods (2) are also kept sealed from the bottom of the electrolytic cell (100); The structure in contact on both sides is a metal rod (5) or a side wall of the electrolytic cell (100).
4. A high-purity copper continuous electrolytic refining equipment according to claim 1 or 3, characterized in that: The outer diameters of the metal rod (5) and the elastic rubber rod (2) are 20 to 30 mm.
5. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The metal rod (5) is a high-purity copper rod or a titanium rod.
6. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The cathode plate (4) is a stainless steel plate or a titanium plate.
7. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The distance between the anode plate (7) and the rotating electrolysis wall (200) is 70 mm-100 mm, and the distance between the cathode plate (4) and the rotating electrolysis wall (200) is 70 mm-100 mm.
8. A high-purity copper continuous electrolytic refining equipment according to claim 1 or 7, characterized in that: When the number of the rotating electrolysis walls (200) exceeds one, the distance between adjacent rotating electrolysis walls 200 is 70-90 mm.
9. The high-purity copper continuous electrolytic refining equipment according to claim 1, characterized in that: The current density in each electrolysis zone is the contact area between the electrolyte and the cathode metal, wherein the cathode metal is a cathode plate (4) connected to the negative pole of a DC power supply (6) at both ends of the electrolysis zone, or a metal rod of a rotating electrolysis wall (200).
10. A high-purity copper continuous electrolytic refining equipment according to claim 1 or 9, characterized in that: The current density in the electrolysis space (300) is controlled to be 100-200A / m 2 .