Ultramicro metal powder electrochemical preparation device

Abstract

An electrochemical preparation device for ultramicro metal powder relates to the field of metal powder manufacturing and comprises an electrolytic bath, a preparation box, a cooling liquid box and an organic liquid box. A plurality of anode tubes are arranged at the bottom of the electrolytic bath, a cathode tube is rotationally connected in the electrolytic bath, a first branch tube and a second branch tube are arranged on the cathode tube, and a nozzle for spraying organic liquid to the first branch tube or the second branch tube is arranged at the upper part in the electrolytic bath; the organic liquid tank is communicated with the nozzle through an organic liquid pipe; the cooling liquid tank is communicated with the cathode tube through a water tube and is used for providing cooling water into the first branch tube and the second branch tube; and the preparation box is connected with the electrolytic bath through a transmission pipe and is used for receiving and treating a mixture of the metal powder and the organic liquid flowing out of the electrolytic bath. According to the invention, the electrochemical reduction reaction is carried out on the first branch pipe and the second branch pipe of the cathode pipe, and the agglomeration of the metal powder is effectively prevented through the coating effect of the organic liquid, so that the ultramicro metal powder with high purity and uniform granularity is prepared.

Description

Technical Field

[0001] The invention relates to the field of metal powder manufacturing, and in particular to an electrochemical preparation device for ultrafine metal powder. Background Art

[0002] Ultrafine metal powder is a high-tech metal material with extremely small particle size and high specific surface area. They are usually prepared by chemical reaction, mechanical synthesis or physical methods, and can be used in many fields, including electronics, medical, energy and material science. Due to its high specific surface area, ultrafine metal powder can enhance the mechanical properties, thermal conductivity and electrical conductivity of materials. In addition, they can also be used to prepare nanomaterials, coatings and catalysts. The application range of ultrafine metal powder is very wide. For example, in the electronics industry, ultrafine metal powder can be used to prepare high-performance radio frequency devices and integrated circuits; in the medical industry, ultrafine metal powder can be used to prepare biosensors and drug delivery systems; in the energy industry, ultrafine metal powder can be used to develop efficient solar cells and energy storage devices.

[0003] Existing metal powder preparation methods often make it difficult to avoid agglomeration and oxidation of metal powder during preparation and storage, resulting in reduced powder purity and uneven particle size, affecting subsequent processing and application effects. At the same time, the electrochemical reduction reaction is an exothermic process. If the heat cannot be dissipated in time, the temperature in the electrolytic cell will rise, affecting the rate and efficiency of the electrolytic reaction, and may even damage the equipment.

[0004] Therefore, there is an urgent need for an ultrafine metal powder electrochemical preparation device to solve the technical problems existing in the above-mentioned prior art. Summary of the invention

[0005] The purpose of the present invention is to solve the above problems in the prior art and to provide an electrochemical preparation device for ultrafine metal powder to prepare ultrafine metal powder with high purity and uniform particle size.

[0006] In order to achieve the above object, the present invention adopts the following technical scheme:

[0007] An electrochemical preparation device for ultrafine metal powder comprises an electrolytic cell, a preparation box, a cooling liquid tank and an organic liquid tank; a plurality of anode tubes are arranged at the bottom of the electrolytic cell, a cathode tube is rotatably connected inside the electrolytic cell, a first branch tube and a second branch tube are arranged on the cathode tube, and a nozzle for spraying organic liquid to the first branch tube or the second branch tube is arranged at the upper part of the electrolytic cell; the organic liquid tank is connected to the nozzle through the organic liquid pipe; the cooling liquid tank is connected to the cathode tube through a water pipe, and is used to provide cooling water to the first branch tube and the second branch tube; the preparation box is connected to the electrolytic cell through a transmission pipe, and is used to receive and process the mixture of metal powder and organic liquid flowing out of the electrolytic cell.

[0008] The inner walls on both sides of the electrolytic cell are provided with annular guide grooves, and an arc plate for guiding flow is slidably connected to the annular guide grooves, and the arc plate is located below the nozzle.

[0009] The inner wall of the electrolytic cell is also provided with a guide groove, which is located below the arc-shaped plate. A through hole is opened at the guide groove, and the preparation box and the through hole are connected through the transmission pipe.

[0010] A leakage hole is opened at the bottom of the arc-shaped plate, and the nozzle is used to flush the metal powder attached to the first branch pipe and the second branch pipe, and the metal powder flows into the guide groove through the leakage hole.

[0011] The bottom of the electrolytic cell is slidably connected with a bottom plate, the anode tube is fixed on the bottom plate, and a plurality of annular protrusions are arranged on the bottom plate.

[0012] A drainage port connected to the organic liquid tank is also provided on one side of the electrolytic cell, so as to return the excess organic liquid in the electrolytic cell to the organic liquid tank.

[0013] A fine screen is provided in the preparation box, and a drainage pipe connected to the organic liquid tank is provided below the fine screen for returning the organic liquid to the organic liquid tank.

[0014] The included angle between the first branch pipe and the second branch pipe is 100-120°.

[0015] The application of the ultrafine metal powder electrochemical preparation device is used to prepare ultrafine metal powder.

[0016] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0017] 1. The present invention is provided with a first branch pipe and a second branch pipe, and when in use, the electrochemical reduction reaction is carried out on the first branch pipe and the second branch pipe of the cathode tube, and the metal powder is effectively prevented from agglomerating by the coating effect of the organic liquid, thereby preparing ultrafine metal powder with high purity and uniform particle size. In addition, during the preparation process, the organic liquid not only serves as a flushing medium, but also as a protective layer for the metal powder, effectively preventing the metal powder from agglomerating and oxidizing during the preparation and storage process, thereby improving the stability of the metal powder.

[0018] 2. The present invention allows cooling water to be introduced into the first branch pipe and the second branch pipe, thereby effectively absorbing and taking away the heat generated during the reaction, maintaining the temperature in the electrolytic cell stable, and ensuring that the electrolysis reaction is carried out within a suitable temperature range.

[0019] 3. The present invention is provided with a drainage pipe and a conduit, and when in use, the organic liquid used for flushing and the excess organic liquid in the electrolytic cell flow back to the organic liquid tank through the drainage pipe and the conduit, thereby realizing the recycling of the organic liquid, which not only reduces production costs but also reduces pollution to the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the overall structure of the device for electrochemical preparation of ultrafine metal powder;

[0021] Figure 2 It is a rear view schematic diagram of the overall structure of the ultrafine metal powder electrochemical preparation device;

[0022] Figure 3 Schematic diagram of the internal structure of the electrolytic cell;

[0023] Figure 4 Another perspective schematic diagram of the internal structure of the electrolytic cell;

[0024] Figure 5 It is a schematic diagram of the structure of the cathode tube;

[0025] Figure 6 It is a schematic diagram of the cross-sectional structure of the preparation box;

[0026] Figure 7 is a schematic diagram of the cross-sectional structure of the guide rail;

[0027] Figure 8 Schematic diagram of the state of the electrolyte in the electrolytic cell.

[0028] Figure numerals: 1, electrolytic cell; 2, preparation box; 3, coolant tank; 4, organic liquid tank; 5, feed port; 6, water pipe; 7, boost valve; 8, organic liquid pipe; 9, transmission pipe; 10, conduit; 11, guide rail; 12, nozzle; 13, infusion pipe; 14, annular guide groove; 15, arc plate; 16, guide groove; 17, through hole; 18, cathode tube; 19, first branch pipe; 20, second branch pipe; 21, bottom plate; 22, anode tube; 23, drainage port; 24, bearing; 25, protrusion; 26, fine screen; 27, drainage pipe; 28, mounting block; 29, through groove; 30, groove. DETAILED DESCRIPTION

[0029] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer and more understandable, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments.

[0030] It should be explained here that ultrafine powder generally refers to an aggregate composed of tiny solid particles with a particle size less than 100nm, which belongs to the transition area between microscopic particles and macroscopic objects and has a series of special physical and chemical properties. At present, there are many methods for preparing ultrafine powders, and the application and potential application fields are gradually broadened, but the ultrafine powders prepared by most methods have the problem of easy agglomeration and surface oxidation of powder particles, which brings great inconvenience to the subsequent collection, storage, transportation and application process. Therefore, it is of practical significance to find a preparation method that is easy to promote in industrial production. The preparation device provided by the present invention adopts a new electrolysis method, which can prepare ultrafine metal powders with high purity, uniform particle size and surface coating.

[0031] Example 1

[0032] like Figures 1 to 4 As shown, the electrochemical preparation device of ultrafine metal powder in this embodiment includes: a control unit, an electrolytic cell 1, a preparation tank 2, a cooling liquid tank 3 and an organic liquid tank 4;

[0033] The top of the electrolytic cell 1 is provided with a feed port 5, the bottom of the electrolytic cell 1 is provided with a plurality of anode tubes 22, the inside of the electrolytic cell 1 is rotatably connected with a cathode tube 18, the cathode tube 18 includes a first branch tube 19 and a second branch tube 20 of the same specification, and the angle between the first branch tube 19 and the second branch tube 20 is 100-120°;

[0034] The inner walls on both sides of the electrolytic cell 1 are provided with annular guide grooves 14, and arc plates 15 for guiding flow are slidably connected to the annular guide grooves 14. The inner walls on both sides of the electrolytic cell 1 are also provided with guide rails 11, and nozzles 12 are slidably connected to the guide rails 11.

[0035] The inner wall of the electrolytic cell 1 is also provided with a guide groove 16, and a through hole 17 is opened at the guide groove 16. The preparation box 2 and the through hole 17 are connected through a transmission pipe 9;

[0036] The coolant tank 3 is provided with a water pipe 6 connected to the cathode tube 18, the organic liquid tank 4 is provided with an organic liquid pipe 8 connected to the nozzle 12, the organic liquid tank 4 is connected to the electrolytic cell 1 through a conduit 10, and the organic liquid tank 4 is connected to the preparation tank 2 through a drainage pipe 27.

[0037] It needs to be further explained here that the electrochemical reduction reaction is an exothermic process, and a large amount of heat will be generated during the reaction. If the heat cannot be dissipated in time, the electrolyte temperature will rise, thereby affecting the rate and efficiency of the electrolytic reaction, and may even cause the temperature in the electrolytic cell to be too high and damage the equipment. Therefore, the present invention can effectively absorb and take away the heat generated during the reaction by passing cooling water into the first branch pipe 19 and the second branch pipe 20, maintain the temperature stability in the electrolytic cell 1, and ensure that the electrolytic reaction is carried out within a suitable temperature range.

[0038] In this embodiment, all structures of the entire device that are in contact with the electrolyte are made of high temperature resistant and corrosion resistant materials.

[0039] See also Figure 1 In this embodiment, a booster valve 7 is provided on the organic liquid pipe 8 for adjusting the pressure of the organic liquid sprayed from the nozzle 12. Figure 5 One end of the first branch pipe 19 and the second branch pipe 20 are both provided with a protrusion 25, and a bearing 24 is provided at the connection between the first branch pipe 19, the second branch pipe 20 and the cathode tube 18. The inner ring of the bearing 24 is welded to the protrusion 25, and the outer ring is welded to the cathode tube 18. The first branch pipe 19 and the second branch pipe 20 are both rotatably connected to the cathode tube 18 through the bearing 24.

[0040] See also Figure 6 The preparation box 2 is provided with mounting blocks 28 inside, and a vibrating fine screen 26 is clamped between the mounting blocks 28 . The connection between the drainage pipe 27 and the preparation box 2 is located below the fine screen 26 .

[0041] See also Figure 4 and Figure 8 A drainage port 23 connected to the conduit 10 is provided on one side of the electrolytic cell 1, and the excess organic liquid in the electrolytic cell 1 flows into the organic liquid tank 4 through the drainage port 23 and the conduit 10. The function of the guide groove 16 is to receive the organic liquid containing metal powder flowing down from the arc plate 15.

[0042] Specifically, the bottom of the electrolytic cell 1 is slidably connected to a bottom plate 21, an anode tube 22 is fixed on the bottom plate 21, and a plurality of annular protrusions are provided on the bottom plate 21, wherein the annular protrusions help to optimize the current distribution in the electrolytic cell, so that the current passes through the anode tube and the electrolyte more evenly, thereby improving the efficiency and uniformity of the electrolytic reaction; during the electrolysis process, bubbles may be generated, and the annular protrusions help to change the movement trajectory of the bubbles, thereby preventing the bubbles from accumulating near the bottom plate, thereby affecting the electrolytic reaction.

[0043] See also Figure 7 A groove 30 is provided at the bottom of the guide rail 11, and the nozzle 12 can slide in the groove 30. A liquid infusion tube 13 is provided between the guide rails 11 located on the inner walls of both sides of the electrolytic cell 1, and a through groove 29 connected to the liquid infusion tube 13 and the nozzle 12 is provided in the guide rail 11. Specifically, the organic liquid tube 8 is responsible for transporting the organic liquid from the organic liquid tank 4 to the nozzle 12, and the through groove 29 in the guide rail 11 ensures that the organic liquid in the liquid infusion tube 13 can flow smoothly to the nozzle 12. The sliding of the nozzle can be achieved by selecting mature existing technologies such as electric, pneumatic, and screw, which will not be repeated here.

[0044] In this embodiment, a leak hole is opened at the bottom of the arc plate 15, and the metal powder attached to the cathode tube 18 is washed down by the nozzle 12, and flows into the guide groove 16 through the leak hole. The control unit is used to control the pressure of the organic liquid sprayed by the nozzle 12, the temperature of the coolant in the coolant tank 3, and the rotation angle and speed of the cathode tube 18, the first branch pipe 19 and the second branch pipe 20 in real time.

[0045] Specifically, a pressure sensor is installed on the organic liquid pipe 8 to monitor the pressure of the organic liquid sprayed from the nozzle 12 in real time. The control unit has a built-in control algorithm to compare the preset organic liquid pressure range and target value with the actual pressure value fed back by the sensor.

[0046] When the actual pressure value deviates from the preset range, the control unit adjusts the pressure in the organic liquid pipe 8 by adjusting the opening of the boost valve 7, thereby accurately controlling the pressure of the organic liquid sprayed from the nozzle 12. The control unit continuously monitors and adjusts in real time to ensure that the organic liquid pressure remains within the optimal range to meet the needs of flushing metal powder.

[0047] A temperature sensor is installed in the coolant tank 3 to monitor the temperature of the coolant in real time. The control unit is connected to the water pump, radiator and other components of the cooling system. The preset coolant temperature range and target value are compared with the actual temperature value fed back by the temperature sensor.

[0048] When the actual temperature exceeds the preset range, the control unit dynamically adjusts the coolant circulation speed and heat dissipation effect by adjusting the speed of the water pump and the heat dissipation efficiency of the radiator to maintain the stability of the coolant temperature. To prevent the coolant temperature from being too high and causing damage to the equipment, the control unit can be equipped with over-temperature alarm and automatic shutdown protection functions.

[0049] Rotary encoders are installed on the rotating shafts of the cathode tube 18, the first branch tube 19 and the second branch tube 20 to monitor their rotation angles and speeds in real time. The control unit is connected to the motor that drives the cathode tube, the first branch tube and the second branch tube to rotate, and precise control of the rotation angle and speed is achieved by controlling the speed and direction of the motor.

[0050] According to the needs of the electrochemical reduction reaction and the requirements of the preparation process, the rotation angles and speed programs of the cathode tube, the first branch tube and the second branch tube are preset.

[0051] The control unit compares the feedback signal of the rotary encoder with the preset program and realizes closed-loop control by adjusting the control signal of the motor to ensure that the rotation angle and speed of the cathode tube, the first branch tube and the second branch tube are accurate.

[0052] The control unit is preset with a rotation program of the arc plate 15, which is coordinated with the rotation program of the cathode tube 18. When the cathode tube 18 starts to rotate, the control unit starts the rotation program of the arc plate 15, ensuring that the two operate synchronously according to a predetermined timing and angle.

[0053] The present embodiment provides a method for using an ultrafine metal powder electrochemical preparation device, which is applied to the ultrafine metal powder electrochemical preparation device described above, and comprises the following steps:

[0054] The raw materials and the organic liquid are sequentially poured into the electrolytic cell 1 from the feed port 5, and the organic liquid is suspended above the raw materials. The first branch pipe 19 and the second branch pipe 20 in the electrolytic cell 1 are always rotated under the action of the cathode tube 18, and the angle of a single rotation is not greater than the angle formed between the first branch pipe 19 and the second branch pipe 20. When one of the first branch pipe 19 or the second branch pipe 20 is perpendicular to the bottom plate 21, the arc plate 15 rotates to the bottom of the other one, and at the same time, the nozzle 12 sprays the organic liquid to wash off the attached metal powder, and collects it in the preparation box 2, and then obtains the ultrafine metal powder after screening and drying.

[0055] Furthermore, during the flushing process, the organic liquid flowing into the electrolytic cell 1 flows into the organic liquid tank 4 through the drainage port 23 , and the organic liquid flowing into the preparation tank 2 flows into the organic liquid tank 4 through the drainage pipe 27 .

[0056] It is further explained here that the control unit starts the rotation program of the cathode tube 18, the cathode tube 18 starts to rotate, and drives the first branch tube 19 and the second branch tube 20 to perform intermittent electrolysis reaction and organic liquid coating. The position of the cathode tube 18 and the arc plate 15 can be monitored in real time by the rotary encoder, and the feedback signal is sent to the control unit.

[0057] When the control unit detects that one of the first branch pipe 19 or the second branch pipe 20 is perpendicular to the bottom plate 21, the arc plate 15 is started to rotate to the bottom of the other branch pipe according to a preset program or a control instruction of the electric actuator.

[0058] The nozzle 12 sprays the organic liquid to wash down the metal powder attached to the branch pipe. The washed down metal powder and organic liquid mixture flows into the guide groove 16 through the leakage hole at the bottom of the arc plate 15 and is collected into the preparation box 2 through the transmission pipe 9.

[0059] Example 2

[0060] The raw materials used in this example are: CuSO4, H2SO4; organic liquid: toluene, oleic acid; which are added into the electrolytic cell in sequence to prepare ultrafine Cu powder.

[0061] During the experiment, CuSO4 solution was prepared with distilled water and injected into the electrolytic cell. At the same time, a certain amount of H2SO4 was added to maintain the pH value of the mixed solution at 4. Then a certain amount of 3% by volume of toluene and 3% by volume of oleic acid were added (here 3% refers to the volume percentage of toluene or oleic acid in the mixed solution in the electrolytic cell). The prepared organic liquid floats on the electrolyte (that is, the mixed solution of CuSO4 solution and H2SO4) due to its lower density, thus forming two layers of liquid surface inside the electrolytic cell.

[0062] like Figure 8 As shown, A is the organic liquid, and B is the mixed solution of CuSO4 liquid and H2SO4. It can be seen from the figure that the upper surface of the organic liquid and the lowest end of the drainage port are on the same horizontal line.

[0063] The electrolyte is electrolyzed using a JWY-30-2A DC regulated power supply, and an insoluble anode made of Pb-Sn alloy is used in the electrolysis process. The cathode tube in the electrolytic cell is constantly rotating at a speed of 5r / min, and cooling water is passed through it.

[0064] Under the rotation of the cathode tube, the first branch and the second branch are always kept one in the electrolyte and the other outside the electrolyte. When the first branch or the second branch is in the electrolyte, the electrolyte undergoes an electrochemical reduction reaction, and the metal is precipitated on the first branch or the second branch. When one of the branches rotates to the organic liquid layer, the metal precipitation stops because the organic liquid is non-conductive, and the precipitated metal is coated on the branch surface by the organic liquid. When the branch rotates to the electrolyte again, metal is precipitated again, but the precipitated metal cannot be connected to the metal remaining on the branch surface last time due to the barrier of the organic film. Therefore, when the process is repeated, a mixture of precipitated metal powder and organic liquid is obtained.

[0065] The nozzle is facing the branch pipe leaving the electrolyte, and the metal powder precipitated on the branch pipe is washed away by spraying organic liquid. The spraying speed of the organic liquid is 5m / s, and it flows into the preparation box through the guide groove and the transmission pipe. A small part of the organic liquid will flow back to the electrolytic cell. For details, see Figure 8 When the organic liquid contacts the first branch pipe, splashing may occur. Since the first branch pipe is inclined, some organic liquid may flow to the lower end of the first branch pipe and fall into the electrolytic cell. Since a drainage port is provided on one side of the electrolytic cell, the excess organic liquid will flow into the organic liquid tank from the drainage port, thereby always keeping the total mass of the organic liquid in the electrolytic cell unchanged.

[0066] After the metal powder mixture entering the preparation box is vibrated and centrifuged, the organic liquid can be recycled through the drainage pipe, and the remaining powder particles can be vacuum dried to obtain the required ultrafine Cu powder.

[0067] The morphology, composition and particle size of the powder were observed and analyzed using transmission electron microscopy, small-angle X-ray scattering, etc. The antioxidant property of the powder was determined by weighing, and the specific surface area of ​​the powder was determined by BET gas adsorption method.

[0068] The ultrafine Cu powder prepared by the device in this embodiment has uniform particle size and an average particle size of 60 nm through transmission electron microscopy and X-ray diffraction analysis.

[0069] The specific surface area of ​​the powder was measured by BET gas adsorption method and was 18 m 2 / g, since the powder particles are spherical, the corresponding average particle size can be converted from the specific surface area measurement value to be 51nm, which further explains that the obtained powder has good dispersibility.

[0070] After the ultrafine Cu powder was exposed to air for 100 days, its weight did not change significantly, which further indicated that the ultrafine Cu powder had good oxidation resistance.

[0071] The reason why the obtained ultrafine Cu powder has high dispersibility and excellent antioxidant properties is that the surface of the powder particles is covered with an organic coating layer, which effectively prevents the agglomeration of the powder particles and gives the powder the ability to resist oxidation in the air, which is extremely beneficial to the stability of the ultrafine powder during storage, transportation and use.

[0072] In addition, due to the characteristics of the electrolysis method itself and the simple operation process of the preparation device, the particle size can be controlled by adjusting the electrolysis process parameters. In addition to preparing ultrafine Cu powder, the preparation device can also be used to prepare powders of various metals and alloys such as Ni, Fe, Ag, Sn, Pb, Cr, Mn, Cu-Zn, Cu-Ni, Ni-Mo, Fe-Cr, etc.

[0073] The principle of the present invention is as follows:

[0074] 1. When the present invention is used, the metal salt solution and the organic liquid required for preparing the metal powder are simultaneously added into the electrolytic cell through the feed port 5 at the top of the electrolytic cell 1. Since the density of the organic liquid is relatively small, it will naturally suspend above the metal salt solution, thereby forming an obvious liquid surface stratification in the electrolytic cell.

[0075] 2. The electrolytic cell is provided with a plurality of anode tubes 22 and a rotating cathode tube 18, as well as a first branch tube 19 and a second branch tube 20 connected to the cathode tube. The two branches rotate continuously during the electrolysis process to ensure that the reaction proceeds evenly. When the first branch tube or the second branch tube is immersed in the metal salt solution, due to the electrolysis, the metal ions undergo a reduction reaction on the cathode, precipitate metal atoms and gradually aggregate into powder attached to the surface of the branch tube. When the branch tube rotates to the organic liquid layer, the metal precipitation reaction stops because the organic liquid is not conductive. At this time, the precipitated metal powder is coated with the organic liquid to form a protective film to prevent agglomeration and oxidation between the powders. As the branch tube continues to rotate, when the branch tube with metal powder attached enters the metal salt solution again, new metal powder will continue to precipitate, but due to the barrier of the organic film, the newly precipitated powder will not agglomerate with the previous powder. When the metal powder in the first branch tube or the second branch tube accumulates to a certain extent, the nozzles 12 on both sides of the electrolytic cell will spray organic liquid, and the metal powder attached to the branch tube will be flushed down by the flushing effect of the organic liquid. The washed metal powder and organic liquid mixture flows into the guide groove 16 through the leakage hole at the bottom of the arc plate 15, and enters the preparation box 2 through the through hole 17 and the transmission pipe 9.

[0076] 3. A vibrating fine screen 26 is provided inside the preparation box 2 to screen the metal powder and organic liquid mixture flushed in. The organic liquid flows back to the organic liquid tank 4 through the drainage pipe 27 to achieve recycling. The remaining metal powder is screened and dried to finally obtain ultrafine metal powder with uniform particle size and high purity.

[0077] 4. During the entire preparation process, the control unit performs real-time monitoring and adjustment. The control unit can control the organic liquid pressure sprayed from the nozzle, the coolant temperature in the coolant tank, and the rotation angle and speed of the cathode tube, the first branch pipe and the second branch pipe in real time to ensure the stability and efficiency of the preparation process.

[0078] Through the above, the device of the present invention realizes the electrochemical preparation of ultrafine metal powder, has the advantages of high purity, uniform particle size, prevention of agglomeration and oxidation, and is suitable for the preparation of various metal and alloy powders.

Claims

1. An electrochemical preparation device for ultrafine metal powder, characterized in that: It comprises an electrolytic cell, a preparation box, a cooling liquid tank and an organic liquid tank; a plurality of anode tubes are arranged at the bottom of the electrolytic cell, a cathode tube is rotatably connected inside the electrolytic cell, a first branch tube and a second branch tube are arranged on the cathode tube, and a nozzle for spraying organic liquid to the first branch tube or the second branch tube is arranged at the upper part of the electrolytic cell; the organic liquid tank is connected with the nozzle through the organic liquid pipe; the cooling liquid tank is connected with the cathode tube through the water pipe, and is used for providing cooling water to the first branch tube and the second branch tube; the preparation box is connected with the electrolytic cell through a transmission pipe, and is used for receiving and processing the mixture of metal powder and organic liquid flowing out of the electrolytic cell.

2. The device for electrochemical preparation of ultrafine metal powder according to claim 1, characterized in that: The inner walls on both sides of the electrolytic cell are provided with annular guide grooves, and an arc plate for guiding flow is slidably connected to the annular guide grooves, and the arc plate is located below the nozzle.

3. The electrochemical preparation device for ultrafine metal powder according to claim 2, characterized in that: The inner wall of the electrolytic cell is also provided with a guide groove, which is located below the arc-shaped plate. A through hole is opened at the guide groove, and the preparation box and the through hole are connected through the transmission pipe.

4. The device for electrochemical preparation of ultrafine metal powder according to claim 3, characterized in that: A leakage hole is opened at the bottom of the arc-shaped plate, and the nozzle is used to flush the metal powder attached to the first branch pipe and the second branch pipe, and the metal powder flows into the guide groove through the leakage hole.

5. The device for electrochemical preparation of ultrafine metal powder according to claim 1, characterized in that: The bottom of the electrolytic cell is slidably connected with a bottom plate, the anode tube is fixed on the bottom plate, and a plurality of annular protrusions are arranged on the bottom plate.

6. The device for electrochemical preparation of ultrafine metal powder according to claim 1, characterized in that: A drainage port connected to the organic liquid tank is also provided on one side of the electrolytic cell, so as to return the excess organic liquid in the electrolytic cell to the organic liquid tank.

7. The device for electrochemical preparation of ultrafine metal powder according to claim 1, characterized in that: A fine screen is provided in the preparation box, and a drainage pipe connected to the organic liquid tank is provided below the fine screen for returning the organic liquid to the organic liquid tank.

8. The device for electrochemical preparation of ultrafine metal powder according to claim 1, characterized in that: The included angle between the first branch pipe and the second branch pipe is 100-120°.

9. Application of the device for electrochemical preparation of ultrafine metal powder according to any one of claims 1 to 8, characterized in that: Used to prepare ultrafine metal powder.

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