Combined continuous electrolysis device

Abstract

According to the combined continuous electrolysis device provided by the utility model, the side hole is formed in the side surface of the cathode plate, so that electrolyte in an electrolytic bath can enter the upper cavity of the cathode frame, and the deposition hole is formed in the bottom of the upper cavity of the anode frame, so that an anode mud settling area is formed at the lower part of the combined electrode frame formed by alternate arrangement; and anode mud generated by electrolysis enters the anode mud settling area through the deposition holes and further enters the purification device outside the cell through the first pipeline for isolated collection, the anode mud and impurity elements are prevented from polluting the electrolyte, the electrolyte subjected to precision filtration and chemical purification returns to the electrolytic cell again, and continuous electrolysis is achieved.

Description

Technical Field

[0001] The utility model belongs to the technical field of wet electrolysis and purification of metals, and in particular relates to a combined continuous electrolysis device. Background Art

[0002] With the rapid development of VLSI, the size of semiconductor chips has been reduced to the nanometer level. The RC delay and electromigration of metal interconnects have become the main factors affecting chip performance. Traditional aluminum and aluminum alloy interconnects can no longer meet the requirements of VLSI process. Compared with aluminum, copper has higher electromigration resistance and higher conductivity, especially ultra-high purity copper (purity ≥ 6N), which is of great significance for reducing the resistance of chip interconnects and improving their computing speed.

[0003] In order to obtain the above-mentioned high-purity copper, the current method generally uses wet electrolysis to purify high-purity electrolytic copper, and then uses fire smelting to form ingots. Among them, wet purification is particularly important. The purity of electrolytic copper directly determines whether the copper ingot meets the purity requirements of the semiconductor industry.

[0004] As one of the important elements of electrolysis, the electrolytic device is an important factor affecting whether high-purity copper can be produced. At present, the device commonly used in the industry to prepare electrolytic copper is a rectangular tank. As the electrolysis proceeds, the anode mud and impurity elements produced by the anode accumulate and diffuse into the electrolyte of the entire tank, causing contamination of the electrolyte and affecting the purity of the electrolytic copper.

[0005] CN202865358U discloses a high current density circulating flow anode diaphragm electrolysis device, which increases the migration speed of metal cations by increasing the cathode liquid circulation flow rate. On the one hand, the device is provided with an anode mud settling chamber, but has no external discharge design. As the anode mud precipitates, the purity of the solution in the anode gradually decreases, affecting the purity of the product. On the other hand, in order to achieve the purpose of rapid circulation of the cathode solution, the device must install liquid spraying and liquid return pipes on both sides of each cathode frame, which increases the workload of cleaning and assembling the device, and increases the labor intensity and work complexity of the workers.

[0006] CN103409771A discloses a continuous and stable production process device and process for electrolytic nickel or electrolytic cobalt. The device connects the cathode frame and the anode frame together with a screw, and sets a permeable membrane between the cathode frame and the anode frame to form a closed structure. The disadvantage of the device is that no anode mud settling chamber is set, and the anode mud cannot be effectively separated from the electrolyte. The device adopts a relatively primitive solution circulation method of high and low level tanks. When the liquid level height in the high level tank changes, the solution circulation speed also changes accordingly. No pump is used to control the circulation speed, and when the circulation speed needs to be changed due to process changes, it is not easy to adjust.

[0007] In summary, in order to prevent the anode slime and impurity elements from contaminating the electrolyte and ensure the high purity of the electrolytically obtained metal, it is necessary to develop a new type of combined continuous electrolysis device. Summary of the Invention

[0008] Aiming at the deficiencies of the existing technology, the present utility model provides a combined continuous electrolysis device. By opening side holes on the side of the cathode plate, the electrolyte in the electrolytic cell can enter the upper cavity of the cathode frame. By opening deposition holes at the bottom of the upper cavity of the anode frame, an anode slime settling area is formed at the lower part of the combined electrode frames arranged alternately. The electrolytically generated anode slime enters the anode slime settling area through the deposition holes and further enters the off-tank purification device through the first pipeline for isolated collection, preventing the anode slime and impurity elements from contaminating the electrolyte. The electrolyte that has been precisely filtered and chemically purified then returns to the electrolytic cell again to achieve continuous electrolysis.

[0009] To achieve this purpose, the present utility model adopts the following technical solutions:

[0010] The present utility model provides a combined continuous electrolysis device, which is characterized by comprising: an electrolytic cell, a cathode frame, an anode frame, two end sealing plates, and an off-tank purification device; the number of the cathode frames is N, and N is a positive integer ≥ 1; the number of the anode frames is N + 1;

[0011] Among them, the cathode frame is in a "day" shape, so that the cathode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the cathode frame is open for inserting a cathode plate; two side holes are opened on two sides of the upper cavity of the cathode frame;

[0012] Corresponding to the cathode frame, the anode frame is in a "day" shape, so that the anode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the anode frame is open for inserting an anode plate; deposition holes are opened at the bottom of the upper cavity of the anode frame;

[0013] Inside the electrolytic cell, the cathode frame and the anode frame are arranged alternately to form a combined electrode frame; for adjacent cathode frame and anode frame, a filter element is arranged at the position corresponding to the upper cavity; for adjacent cathode frame and anode frame, the cavities at the positions corresponding to the lower cavity are connected as a whole, so that an anode slime settling area is formed at the lower part of the combined electrode frame;

[0014] The end sealing plates are respectively arranged at both ends of the combined electrode frame; corresponding to the bottom of the anode slime settling area, an extraction port is opened at the lower part of one of the end sealing plates, and the extraction port is connected to the inlet of the off-tank purification device through a first pipeline, and the outlet of the off-tank purification device is connected to the upper inlet of the electrolytic cell to realize the circulating flow of the electrolyte.

[0015] For the combined continuous electrolysis device of the present utility model, by opening side holes on the side surface of the cathode plate, the electrolyte in the electrolytic cell can enter the upper cavity of the cathode frame. By opening deposition holes at the bottom of the upper cavity of the anode frame, an anode mud settling area is formed at the lower part of the combined electrode frames arranged alternately. The anode mud generated by electrolysis enters the anode mud settling area through the deposition holes, and further enters the off-tank purification device through the first pipeline for isolated collection, preventing the anode mud and impurity elements from contaminating the electrolyte. The electrolyte that has undergone precision filtration and chemical purification then returns to the electrolytic cell again to achieve continuous electrolysis.

[0016] It should be noted that as is well known to those skilled in the art, both ends of the combined continuous electrolysis device need to be anode frames. Therefore, the number of cathode frames is N, and the number of anode frames is N + 1, which will not be elaborated here; N is a positive integer greater than or equal to 1, such as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12, 14, or 15, etc.

[0017] As a preferred technical solution of the present utility model, at least three side holes are evenly opened on each of the two side surfaces of the upper cavity of the cathode frame.

[0018] As a preferred technical solution of the present utility model, buffer gauze meshes are arranged on the side holes.

[0019] It should be noted that for the cathode frame of the present utility model, by increasing the number of side holes, the impact force of the electrolyte entering the upper cavity of the cathode frame from the side holes during the circulation process can be reduced, avoiding the scouring of the electrolyte on the cathode plate and avoiding the influence on the quality of the deposited metal on the cathode plate. Further, by arranging buffer gauze meshes on the side holes, the scouring of the electrolyte on the cathode plate can be further avoided, and the influence on the quality of the deposited metal on the cathode plate can be further avoided.

[0020] As a preferred technical solution of the present utility model, corresponding to the six edge points of the upper cavity and the lower cavity, assembly holes are respectively opened at the edges of the cathode frame, the anode frame, and the end sealing plate, and are tightly connected by screws and nuts.

[0021] As a preferred technical solution of the present utility model, assembly holes are respectively opened at the middle bottoms of the cathode frame, the anode frame, and the end sealing plate, and are tightly connected by screws and nuts.

[0022] As a preferred technical solution of the present utility model, "day-shaped" sealing ring accommodating grooves are respectively opened on each of the two side surfaces of the cathode frame and the anode frame;

[0023] A "day-shaped" sealing ring accommodating groove is opened on the side surface of the end sealing plate close to the combined electrode frame.

[0024] As a preferred technical solution of the present utility model, a liquid pump is arranged on the first pipeline.

[0025] As a preferred technical solution of the utility model, the first pipeline penetrates into the anode mud sedimentation area to form an internal production section, and the internal production section is evenly provided with production holes.

[0026] As a preferred technical solution of the present utility model, a liquid return pump is arranged on the second pipeline.

[0027] As a preferred technical solution of the utility model, the filter element includes filter cloth and / or ion membrane.

[0028] The combined continuous electrolysis device described in the utility model can be prepared with acid- and alkali-resistant materials such as PP plates or engineering plastics, and the specific size can be customized according to actual use requirements. The cell body of the electrolytic cell is composed of anode and cathode frames and two end sealing plates fastened by threaded rods and nuts. Filter cloth or ion membrane and other materials are installed between the cathode and cathode frames, and two upper and lower chambers are formed after being combined. The cathode frame and the anode frame are both processed and made from a whole piece of material, and the upper and lower cavities are formed by digging through the upper and lower cavities, and the holes opened are at different positions.

[0029] Compared with the prior art, the beneficial effects of the utility model are:

[0030] The utility model provides a combined continuous electrolysis device. By opening side holes on the side of the cathode plate, the electrolyte in the electrolytic cell can enter the upper cavity of the cathode frame. By opening sedimentation holes on the bottom of the upper cavity of the anode frame, the lower part of the combined pole frame formed by alternating arrangement forms an anode mud sedimentation area. The anode mud generated by electrolysis enters the anode mud sedimentation area through the sedimentation holes, and further enters the external purification device through a first pipeline for isolated collection, so as to prevent the anode mud and impurity elements from contaminating the electrolyte. The electrolyte that has been precisely filtered and chemically purified returns to the electrolytic cell again, so as to realize continuous electrolysis. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is an overall cross-sectional view of the combined continuous electrolysis device of the utility model;

[0032] Figure 2 It is an exploded view of the combined pole frame in the combined continuous electrolysis device of the utility model;

[0033] Figure 3 It is a schematic diagram of the overall structure of the cathode frame or the anode frame of the utility model;

[0034] Among them, 1. electrolytic cell; 2. cathode frame; 3. anode frame; 4. end sealing plate; 5. out-of-tank purification device; 6. combined electrode frame; 7. filter element; 8. anode mud settling area; 9. assembly hole; 10. sealing ring accommodating groove; 11. liquid extraction pump; 12. liquid return pump. Detailed implementation manners

[0035] To make the technical solutions, objectives, and advantages of the present utility model clearer, the present utility model will be further described in detail below through specific implementation examples in conjunction with the drawings. It should be understood that the specific implementation manners described herein are only used to illustrate and explain the present utility model and are not used to limit the present utility model.

[0036] In the description of the present utility model, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present utility model. In addition, the terms "first", "second", and "third" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0037] In the description of the present utility model, it should be noted that unless otherwise clearly specified and limited, the terms "installation", "connection", 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 directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. In the fields of electricity and communication, it can be a wired connection or a wireless connection. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific situations.

[0038] The present utility model provides a combined continuous electrolysis device, as Figure 1 、 Figure 2 shown in Figure 3 , including: electrolytic cell 1, cathode frame 2, anode frame 3, two end sealing plates 4, and out-of-tank purification device 5; the number of the cathode frames 2 is N, and N is a positive integer greater than or equal to 1; the number of the anode frames 3 is N + 1;

[0039] Among them, the cathode frame 2 is in a "day" shape, so that the cathode frame 2 is divided into an upper cavity and a lower cavity; the top of the upper cavity of the cathode frame 2 is open for inserting a cathode plate; side holes are opened on two sides of the upper cavity of the cathode frame 2;

[0040] Corresponding to the cathode frame 2, the anode frame 3 is in a "day" shape, such that the anode frame 3 is divided into an upper cavity and a lower cavity; the top of the upper cavity of the anode frame 3 is open for inserting an anode plate; deposition holes are formed at the bottom of the upper cavity of the anode frame 3.

[0041] Inside the electrolytic cell 1, the cathode frame 2 and the anode frame 3 are arranged alternately to form a combined electrode frame 6; for the positions corresponding to the upper cavities of the adjacent cathode frame 2 and anode frame 3, filter elements 7 are provided; for the positions corresponding to the lower cavities of the adjacent cathode frame 2 and anode frame 3, the cavities are integrated, such that an anode mud settling area 8 is formed at the lower part of the combined electrode frame 6.

[0042] At both ends of the combined electrode frame 6, end sealing plates 4 are respectively provided; corresponding to the bottom of the anode mud settling area 8, an extraction port is formed at the lower part of one of the end sealing plates 4, the extraction port is connected to the inlet of the off-tank purification device 5 through a first pipeline, and the outlet of the off-tank purification device 5 is connected to the upper inlet of the electrolytic cell 1 to realize the circulating flow of the electrolyte ( Figure 1 the arrows in the figure represent the flow direction of the electrolyte).

[0043] Wherein, at least three side holes are respectively and evenly formed on two side surfaces of the upper cavity of the cathode frame 2; buffer gauze is arranged on the side holes.

[0044] Corresponding to six edge points of the upper cavity and the lower cavity, assembly holes 9 are respectively formed at the edges of the cathode frame 2, the anode frame 3 and the end sealing plate 4, and are tightly connected by screws and nuts; assembly holes 9 are respectively formed at the middle bottoms of the cathode frame 2, the anode frame 3 and the end sealing plate 4, and are tightly connected by screws and nuts.

[0045] Sealing ring accommodation grooves 10 in a "day" shape are respectively formed on two side surfaces of the cathode frame 2 and the anode frame 3; a sealing ring accommodation groove in a "day" shape is formed on the side surface of the end sealing plate 4 close to the combined electrode frame 6.

[0046] A liquid extraction pump 11 is arranged on the first pipeline; the first pipeline extends into the anode mud settling area 8 to form an internal extraction section, and extraction holes are evenly formed on the internal extraction section; a liquid return pump 12 is arranged on the second pipeline.

[0047] Embodiment 1

[0048] This embodiment provides a combined continuous electrolysis device, including: an electrolytic cell, a cathode frame, an anode frame, two end sealing plates, and an off-tank purification device; the number of the cathode frames is 8, and the number of the anode frames is 9.

[0049] Among them, the cathode frame is in the shape of a Chinese character 'Ri' (日), such that the cathode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the cathode frame is open for inserting a cathode plate; two side holes are provided on two sides of the upper cavity of the cathode frame;

[0050] Corresponding to the cathode frame, the anode frame is in the shape of a Chinese character 'Ri' (日), such that the anode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the anode frame is open for inserting an anode plate; a deposition hole is provided at the bottom of the upper cavity of the anode frame;

[0051] Inside the electrolytic cell, the cathode frame and the anode frame are arranged alternately to form a combined electrode frame; for the adjacent cathode frame and anode frame, at the position corresponding to the upper cavity, a filter element is provided; for the adjacent cathode frame and anode frame, at the position corresponding to the lower cavity, the cavities are connected as a whole, such that an anode mud settling area is formed at the lower part of the combined electrode frame;

[0052] End cover plates are respectively provided at both ends of the combined electrode frame; corresponding to the bottom of the anode mud settling area, a sampling outlet is provided at the lower part of one of the end cover plates, and the sampling outlet is connected to the inlet of the out-of-tank purification device through a first pipeline, and the outlet of the out-of-tank purification device is connected to the upper inlet of the electrolytic cell to realize the circulating flow of the electrolyte.

[0053] Among them, three side holes are respectively and evenly provided on two sides of the upper cavity of the cathode frame;

[0054] Corresponding to six edge points of the upper cavity and the lower cavity, assembly holes are respectively provided at the edges of the cathode frame, the anode frame and the end cover plate, and are tightly connected by screws and nuts; assembly holes are respectively provided at the middle bottoms of the cathode frame, the anode frame and the end cover plate, and are tightly connected by screws and nuts;

[0055] Sealing ring accommodating grooves in the shape of a Chinese character 'Ri' (日) are respectively provided on two sides of the cathode frame and the anode frame; a sealing ring accommodating groove in the shape of a Chinese character 'Ri' (日) is provided on the side of the end cover plate close to the combined electrode frame;

[0056] A liquid extraction pump is provided on the first pipeline; the first pipeline extends into the anode mud settling area to form an internal sampling section, and sampling holes are evenly provided on the internal sampling section; a liquid return pump is provided on the second pipeline;

[0057] The filter element includes an ion membrane.

[0058] The combined continuous electrolysis device of the utility model sets the cathode frame and the anode frame in the electrolytic cell, and uses the screw and nut to fasten and connect the anode and cathode frames together to form three areas: the cathode area, the anode area and the anode mud sedimentation chamber. The cathode frame is provided with a cathode plate socket on the upper part, and the openings on both sides make the area in the electrolytic cell except the anode area and the sedimentation area form the cathode area, the bottom is sealed and isolated from the sedimentation area, and a filter cloth or an ion membrane is provided between the cathode frame and the anode frame. The anode frame is provided with an anode plate socket on the upper part, and the side is not opened to isolate it from the cathode area. The bottom opening is connected to the sedimentation area so that the anode mud can sink into the sedimentation area. A pipeline is provided in the sedimentation area, and the solution is extracted by a liquid pump, and after precise filtration and chemical purification, it is pumped into the electrolytic cell by a liquid return pump. The return liquid enters the electrolytic cell instead of directly entering the cathode frame, so as to avoid the return liquid scouring the cathode plate and causing product quality problems. The liquid level difference between the cathode area and the anode area is adjusted to 3-10mm by adjusting the liquid pump and the liquid return pump.

[0059] The combined continuous electrolysis device described in Example 1 of the utility model is prepared by using PP plate, the outer dimensions of the cathode frame and the anode frame are both 460*300*50mm, the upper cavity dimension is 200*300mm, the lower cavity dimension is 200*100mm, the anode and cathode holes for inserting the anode and cathode plates have dimensions of 200*30mm, and the assembly hole diameter is 8mm; the above-mentioned trough body is assembled with the pump and the filter device, the copper electrolyte is introduced, and the anode and cathode plates are placed; the power is turned on for electrolysis; the obtained electrolytic copper is tested for purity reaching the 6N standard.

[0060] In summary, the utility model provides a combined continuous electrolysis device, by opening side holes on the side of the cathode plate, the electrolyte in the electrolytic cell can enter the upper cavity of the cathode frame, and by opening sedimentation holes at the bottom of the upper cavity of the anode frame, an anode mud sedimentation area is formed at the lower part of the combined pole frame formed by alternating arrangement, and the anode mud generated by electrolysis enters the anode mud sedimentation area through the sedimentation holes, and further enters the off-cell purification device through the first pipeline for isolated collection, so as to prevent the anode mud and impurity elements from contaminating the electrolyte, and the electrolyte that has been precisely filtered and chemically purified is returned to the electrolytic cell again to realize continuous electrolysis.

[0061] The above description is only a specific implementation method of the present utility model, but the protection scope of the present utility model is not limited thereto. Technicians in the relevant technical field should understand that any changes or substitutions that can be easily thought of by technicians in the relevant technical field within the technical scope disclosed in the present utility model fall within the protection scope and disclosure scope of the present utility model.

Claims

1. A combined continuous electrolysis device, characterized in that: Comprising: An electrolytic cell, a cathode frame, an anode frame, two end seals, and an out-of-tank purification device; the number of the cathode frames is N, where N is a positive integer greater than or equal to 1; the number of the anode frames is N + 1; Among them, the cathode frame is in a "day" shape, so that the cathode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the cathode frame is open for inserting a cathode plate; two side holes are opened on two sides of the upper cavity of the cathode frame; Corresponding to the cathode frame, the anode frame is in a "day" shape, so that the anode frame is divided into an upper cavity and a lower cavity; the top of the upper cavity of the anode frame is open for inserting an anode plate; a deposition hole is opened at the bottom of the upper cavity of the anode frame; Inside the electrolytic cell, the cathode frames and the anode frames are arranged alternately to form a combined electrode frame; for adjacent cathode frames and anode frames, at the position corresponding to the upper cavity, a filter element is provided; for adjacent cathode frames and anode frames, at the position corresponding to the lower cavity, the cavities are connected as a whole, so that an anode mud settling area is formed at the lower part of the combined electrode frame; The end seals are respectively arranged at both ends of the combined electrode frame; corresponding to the bottom of the anode mud settling area, a sampling port is opened at the lower part of one of the end seals, the sampling port is connected to the inlet of the out-of-tank purification device through a first pipeline, and the outlet of the out-of-tank purification device is connected to the upper inlet of the electrolytic cell to realize the circulating flow of the electrolyte.

2. The combined continuous electrolysis device according to claim 1, characterized in that: At least three side holes are evenly opened on two sides of the upper cavity of the cathode frame respectively.

3. The combined continuous electrolysis device according to claim 2, characterized in that: A buffer screen is arranged on the side holes.

4. The combined continuous electrolysis device according to claim 1, characterized in that: Corresponding to six edge points of the upper cavity and the lower cavity, assembly holes are respectively opened at the edges of the cathode frame, the anode frame and the end seal, and are tightly connected by screws and nuts.

5. The combined continuous electrolysis device according to claim 4, characterized in that: Assembly holes are respectively opened at the middle bottoms of the cathode frame, the anode frame and the end seal, and are tightly connected by screws and nuts.

6. The combined continuous electrolysis device according to claim 1, characterized in that: Seal ring accommodating grooves in a "day" shape are respectively opened on two sides of the cathode frame and the anode frame. A seal ring accommodating groove in a "day" shape is opened on the side of the end seal close to the combined electrode frame.

7. The combined continuous electrolysis device according to claim 1, characterized in that: A liquid extraction pump is arranged on the first pipeline.

8. The combined continuous electrolysis device according to claim 7, characterized in that: The first pipeline extends into the anode mud settling area to form an internal sampling section, and sampling holes are evenly opened on the internal sampling section.

9. The combined continuous electrolysis device according to claim 1, characterized in that: The filter element includes filter cloth and / or ion membrane.

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