An apparatus and method for preparing pure metal by segregation purification

Abstract

An apparatus and method for preparing pure metal by segregation purification, which solves the problems of inconvenient use of the spraying device and high working intensity during the purification process of aluminum at present. It includes a segregation furnace for segregating and purifying aluminum liquid; a crucible as a carrier for the aluminum liquid; a stirring device for stirring and mixing the aluminum liquid in the crucible after the crucible is placed in the segregation furnace; and a spraying device for spraying non-stick aluminum coating on the inner wall of the crucible at the initial stage, and its spraying flow rate can be adjusted according to the change of the inner diameter of the crucible. Compared with the prior art, the present invention has the following advantages: 1) Through the setting of the spraying device, the flow rate is automatically adjusted according to the size of the inner wall of the crucible, so as to achieve uniform spraying; 2) The multiple stirring methods of the stirring device increase the stirring efficiency and improve the efficiency of preparing pure aluminum.

Description

Technical Field

[0001] The present invention relates to the technical field of foundry metallurgy, and in particular to an apparatus and method for preparing pure metal by segregation purification. Background Art

[0002] With the continuous progress and development of science and technology, high-purity aluminum has a wide range of applications in the fields of electronics, aviation, aerospace, and national defense industries, and its usage is increasing year by year. Using the segregation method to purify metals, especially aluminum, is a mature industrial process method. The common segregation process is complex, small in size, low in output, not easy to operate, with low production efficiency, and it is difficult to achieve large-scale mass production and the popularization of the process.

[0003] The application number is 202010381579.6, and the name is a method for segregating and purifying high-purity aluminum. The steps are as follows: the segregation furnace is started and preheated, the inner wall of the crucible is sprayed with non-stick aluminum coating and then preheated, the preheated crucible is placed in the segregation furnace, molten aluminum or refined electrolytic aluminum liquid is poured into the crucible, the cooling water on the outer wall of the crucible is turned on, and when the temperature of the aluminum liquid drops to the set value, the upper cover of the segregation furnace is closed, and the heating device, stirring device, and vacuum pumping device of the segregation furnace are turned on. By the above method, a relatively high purification efficiency and purification quality can be maintained.

[0004] However, the above method has deficiencies. When spraying the non-stick aluminum coating on the inner wall of the crucible, it is carried out by constantly moving the spraying device close to the inner wall of the crucible, which is very troublesome to operate, takes a long time at this time, and has a large working intensity. Summary of the Invention

[0005] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides an apparatus and method for preparing pure metal by segregation purification, effectively solving the problems that the spraying device is inconvenient to use and has a large working intensity during the purification process of aluminum.

[0006] To solve the above problems, an apparatus for segregating and purifying high-purity metal includes a segregation furnace for segregating and purifying aluminum liquid;

[0007] A crucible as a carrier for aluminum liquid;

[0008] A stirring device for stirring and mixing the aluminum liquid in the crucible after the crucible is placed in the segregation furnace;

[0009] A spraying device for spraying non-stick aluminum coating on the inner wall of the crucible in the initial stage, which can adjust the spraying flow rate according to the change of the inner diameter of the crucible.

[0010] Preferably, the spraying device includes a support frame that slides vertically, a spraying liquid pipeline is fixed below the support frame, and a flow control valve is installed on the spraying liquid pipeline;

[0011] A support plate is fixed below the support frame. A sliding plate that slides horizontally is provided on the support plate. A spraying head is fixed to the outermost side of the sliding plate. The spraying head is connected to a spraying liquid pipeline through a hose.

[0012] The sliding plate is connected to the control handle of the valve of the flow control valve. The horizontal sliding of the sliding plate controls the opening size of the valve.

[0013] Preferably, a first connecting rod is hinged to the upper end of the sliding plate. The upper end of the first connecting rod is hinged to a second connecting rod. The other end of the second connecting rod is coaxially fixed to the control handle of the valve.

[0014] Preferably, a horizontal slideway is provided on the support plate. The sliding plate slides along the slideway and the outer end of the sliding plate is placed outside the support plate.

[0015] Preferably, a spring is fixed to the support plate. The other end of the spring is fixedly connected to the sliding plate. The spring always pushes the sliding plate to move away from the support plate.

[0016] Preferably, a guide wheel is rotatably provided at the outermost end of the sliding plate. The guide wheel is in contact with the inner wall of the crucible.

[0017] Preferably, the stirring device includes a furnace cover. A rotating arm that can rotate is provided below the furnace cover. A gear that can rotate is provided at the outermost end of the rotating arm.

[0018] An internal gear ring is fixed to the lower end of the furnace cover. The gear meshes with the internal gear ring.

[0019] A rotating shaft is coaxially fixed to the gear. A multi-faceted shaft is fixed to the lower end of the rotating shaft. A stirring shaft that rotates along with the multi-faceted shaft and can slide vertically is provided on the multi-faceted shaft.

[0020] Preferably, a closed spiral cam groove is provided on the outer circumference of the rotating shaft. A pin shaft that can slide is provided in the cam groove.

[0021] A vertically sliding sleeve is provided below the rotating arm. The pin shaft passes through the cam groove and is fixedly connected to the sleeve.

[0022] The upper end of the stirring shaft is rotatably connected to the sleeve.

[0023] Preferably, a guide shaft is fixed to the lower end of the rotating arm. A guide arm is fixed to the outer end of the sleeve. The lower end of the sleeve slidably passes through the guide arm.

[0024] A method for preparing high-purity metal by segregation purification includes the following steps:

[0025] S1, turn on and preheat the segregation furnace. After spraying the inner wall of the crucible with non-stick aluminum coating by a spraying device, place it in a heating furnace for preheating.

[0026] S2. Open the furnace lid of the segregation furnace, place the preheated crucible into the segregation furnace, pour the molten aluminum or refined electrolytic aluminum liquid into the crucible, turn on the cooling device on the outer wall of the crucible, and monitor the temperature of the aluminum liquid through the temperature measuring device.

[0027] S3. When the temperature of the aluminum liquid drops to the set value, close the upper lid of the segregation furnace, and at the same time turn on the heating device, stirring device and vacuum pumping device of the segregation furnace.

[0028] S4. During the solidification production process of aluminum crystals, control the temperature of the aluminum melt between 660°C and 680°C through the temperature measuring device, perform forced cooling on the purification heat conduction layer through the cooling device, control the temperature gradient of the solid-liquid interface of the aluminum melt in the crucible between 5°C and 20°C, monitor the growth rate in real time, adjust and correct the heating temperature of the segregation furnace and the cooling water flow rate in real time according to the growth rate, and control the crystallization rate at 4 - 8 cm / h and the crystallization time at 2 - 4 hours.

[0029] S5. When the aluminum crystal grows to the set thickness, turn off the heating device, stirring device and vacuum pumping device of the segregation furnace, turn off the cooling device on the outer wall of the crucible, open the furnace lid 10 of the segregation furnace, and remove the crucible.

[0030] S6. Pour out the remaining low-grade aluminum liquid in the crucible to obtain high-purity aluminum ingots.

[0031] S7. After the crucible cools down, remove the aluminum ingot in the crucible, and obtain the finished high-purity aluminum ingot after rinsing, grinding and polishing.

[0032] S8. Melt the finished high-purity aluminum ingot and pour it back into the crucible, then put it into the segregation furnace again, and repeat steps S2 - S7 until high-purity aluminum ingots meeting the purity requirements are obtained.

[0033] The present invention has the following benefits compared with the prior art: 1) Through the setting of the spraying device, the flow rate is automatically adjusted according to the size of the inner wall of the crucible, so as to achieve uniform spraying; 2) The multiple stirring methods of the stirring device increase the stirring efficiency and improve the efficiency of preparing pure aluminum. Description of the Drawings

[0034] Figure 1 It is a process flow schematic diagram of the present invention;

[0035] Figure 2 It is a structural schematic diagram of the spraying device of the present invention;

[0036] Figure 3 It is an axonometric structural schematic diagram of the spraying device of the present invention;

[0037] Figure 4 It is a structural schematic diagram of the stirring device of the present invention;

[0038] Figure 5Schematic axonometric structure diagram of the stirring device of the present invention;

[0039] Among them, Figure 1 1. Support frame; 2. Spraying liquid pipeline; 3. Flow control valve; 4. Support plate; 5. Sliding plate; 6. First connecting rod; 7. Second connecting rod; 8. Spring; 9. Guide wheel; 10. Furnace cover; 11. Rotating arm; 12. Internal gear ring; 13. Gear; 14. Rotating shaft; 15. Multi-faceted shaft; 16. Stirring shaft; 17. Cam groove; 18. Pin shaft; 19. Sleeve; 20. Guide shaft. Detailed implementation manners

[0040] Now, the present invention will be further described in detail with reference to the accompanying drawings. The drawings are simplified schematic diagrams, which only illustrate the basic structure of the present invention in a schematic manner, so they only show the components related to the present invention.

[0041] Please refer to Figure 1 ,

[0042] A method for preparing high-purity metal by segregation purification includes the following steps:

[0043] S1. The segregation furnace is started and preheated. After spraying the inner wall of the crucible with a non-stick aluminum coating using a spraying device, it is placed in the heating furnace for preheating.

[0044] S2. Open the furnace cover 10 of the segregation furnace, put the preheated crucible into the segregation furnace, pour molten aluminum metal or refined electrolytic aluminum liquid into the crucible, turn on the cooling device on the outer wall of the crucible, and monitor the temperature of the aluminum liquid through a temperature measuring device.

[0045] S3. When the temperature of the aluminum liquid drops to the set value, close the upper cover of the segregation furnace, and at the same time turn on the heating device, stirring device and vacuum pumping device of the segregation furnace.

[0046] S4. During the solidification process of aluminum crystals, control the temperature of the aluminum melt between 660 °C and 680 °C through a temperature measuring device, forcibly cool the purification heat conduction layer through a cooling device, control the temperature gradient of the solid-liquid interface of the aluminum melt in the crucible between 5 °C and 20 °C, monitor the growth rate in real time, and adjust and correct the heating temperature of the segregation furnace and the cooling water flow according to the growth rate in real time, and control the crystallization rate at 4 - 8 cm / h and the crystallization time at 2 - 4 hours.

[0047] S5. When the growth of the aluminum crystal reaches the set thickness, turn off the heating device, stirring device and vacuum pumping device of the segregation furnace, turn off the cooling device on the outer wall of the crucible, open the furnace cover 10 of the segregation furnace, and remove the crucible.

[0048] S6. Pour out the remaining low-grade aluminum liquid in the crucible to obtain high-purity aluminum ingots.

[0049] S7. After the crucible is cooled, the aluminum ingot in the crucible is removed, rinsed, polished, and then the finished high-purity aluminum ingot is obtained;

[0050] S8. The finished high-purity aluminum ingot is melted and then poured back into the crucible, and then put into the segregation furnace again. Repeat steps S2 - S7 until a high-purity aluminum ingot meeting the purity requirements is obtained.

[0051] The preparation method in the present invention is almost the same as that in the application No. 202010381579.6. The difference is that we use a spraying device to spray the inner wall of the crucible. We know the shape of the crucible. If an artificial or regular spraying device is used, it will cause the problem of low spraying efficiency. Therefore, we use a self-developed spraying device to spray the inner wall of the crucible to improve the efficiency;

[0052] In addition, we have also improved the stirring device. The stirring device no longer uses a single rotor to rotate for stirring, but adopts a more efficient stirring method.

[0053] In addition, regarding the specific process in this step, we can refer to the content in the application No. 202010381579.6. In this application, we will not elaborate on this content in detail.

[0054] Such as Figures 2 - 5 , a device for preparing high-purity metal by segregation purification, including a segregation furnace for segregating and purifying molten aluminum;

[0055] A crucible, serving as a carrier for molten aluminum;

[0056] A stirring device for stirring and mixing the molten aluminum in the crucible after the crucible is placed in the segregation furnace;

[0057] A spraying device for spraying non-stick aluminum coating on the inner wall of the crucible at the initial stage, and it can adjust the size of the spraying flow rate according to the change of the inner diameter of the crucible.

[0058] In this device, we use a segregation furnace and a crucible in the preparation, which are existing equipment and can be directly used. What we have improved are the stirring device and the spraying device. Through this improvement, we can well improve the preparation of pure aluminum and increase the production efficiency.

[0059] The spraying device includes a support frame 1 that slides vertically. A spraying liquid pipeline 2 is fixed below the support frame 1, and a flow control valve 3 is installed on the spraying liquid pipeline 2;

[0060] A support plate 4 is fixed below the support frame 1. A sliding plate 5 that slides horizontally is provided on the support plate 4. A spraying head is fixed on the outermost side of the sliding plate 5, and the spraying head is connected to the spraying liquid pipeline 2 through a hose;

[0061] The sliding plate 5 is connected to the control handle of the valve of the flow control valve 3, and the horizontal sliding of the sliding plate 5 controls the opening size of the valve.

[0062] In the present invention, due to the special shape of the crucible, we designed this spraying device. The inner wall of the crucible is sprayed by a spray head. The spray head rotates in a circle to spray the inner wall of the crucible. During this process, the whole support frame 1 moves downward. At this time, the inner diameter of the crucible wall decreases, and the sliding plate 5 slides inward accordingly, so as to control the size of the flow control valve 3. In this way, as the inner diameter of the crucible decreases, the spraying flow rate can be reduced, which can well ensure the spraying uniformity and increase the speed.

[0063] The upper end of the sliding plate 5 is hinged with a first connecting rod 6, the upper end of the first connecting rod 6 is hinged with a second connecting rod 7, and the other end of the second connecting rod 7 is coaxially fixed with the control handle of the valve.

[0064] When the sliding plate 5 slides horizontally, it drives the control handle to rotate through the first connecting rod 6 and the second connecting rod 7, so as to control the opening size of the flow control valve 3, thus achieving the purpose of this application.

[0065] Preferably, a horizontal slideway is provided on the support plate 4, and the sliding plate 5 slides along the slideway and the outer end of the sliding plate 5 is placed outside the support plate 4.

[0066] A spring 8 is fixed on the support plate 4, and the other end of the spring 8 is fixedly connected with the sliding plate 5. The spring 8 always pushes the sliding plate 5 to move away from the support plate 4.

[0067] In this device, a plug is fixed at the inner end of the support plate 4, and the plug can prevent the separation between the sliding plate 5 and the support plate 4. In addition, under the elastic drive of the spring 8, the sliding plate 5 is made to close to the inner wall of the crucible.

[0068] A guide wheel 9 is rotatably provided at the outermost end of the sliding plate 5, and the guide wheel 9 is in contact with the inner wall of the crucible.

[0069] In the present invention, the guide wheel 9 is in contact with the inner wall of the crucible, so that when the whole device is rotating, the resistance received by the device can be well reduced.

[0070] The stirring device includes a furnace cover 10, a rotating arm 11 is rotatably provided below the furnace cover 10, and a gear 13 is rotatably provided at the outermost end of the rotating arm 11;

[0071] An internal gear ring 12 is fixed at the lower end of the furnace cover 10, and the gear 13 meshes with the internal gear ring 12;

[0072] The gear 13 is coaxially fixed with a rotating shaft 14, and a multi-faceted shaft 15 is fixed to the lower end of the rotating shaft 14. A stirring shaft 16 that rotates with the multi-faceted shaft 15 and can slide vertically is provided on the multi-faceted shaft 15.

[0073] In this device, when the rotating arm 11 rotates, it will drive the rotation center to rotate in a circle. Additionally, when the gear 13 rotates in a circle, it will also generate a self-rotation, that is, the rotation of the rotating shaft 14. The rotation of the rotating shaft 14 drives the stirring shaft 16 to rotate together. A plurality of stirring blades are provided on the outer circumference of the stirring shaft 16 to stir the molten aluminum. Additionally, during the rotation of the stirring shaft 16, a vertical reciprocating slide will also occur, thereby enhancing the final stirring effect and improving efficiency.

[0074] A closed spiral cam groove 17 is provided on the outer circumference of the rotating shaft 14, and a pin shaft 18 is slidably provided in the cam groove 17;

[0075] A vertically sliding sleeve 19 is provided below the rotating arm 11, and the pin shaft 18 passes through the cam groove 17 and is fixedly connected to the sleeve 19;

[0076] The upper end of the stirring shaft 16 is rotatably connected to the sleeve 19.

[0077] In this device, during the rotation of the cam groove 17, it drives the pin shaft 18 to move vertically up and down, thereby realizing the vertical sliding of the sleeve 19. The sleeve 19 is rotatably connected to the stirring shaft 16, thereby driving the stirring shaft 16 to slide vertically. Moreover, the stirring shaft 16 is slidably connected to the multi-faceted shaft 15. Thus, when the multi-faceted shaft 15 rotates, it drives the stirring shaft 16 to rotate.

[0078] A guide shaft 20 is fixed to the lower end of the rotating arm 11, a guide arm is fixed to the outer end of the sleeve 19, and the lower end of the sleeve 19 slidably passes through the guide arm.

[0079] With the cooperation of the guide shaft 20 and the guide arm, the vertical sliding effect of the sleeve 19 is ensured.

[0080] The embodiments are merely examples given for clear illustration and are not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or alterations can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or alterations derived therefrom are still within the protection scope of this invention.

Claims

1. An apparatus for preparing high-purity metal by segregation purification, characterized in that, It includes a segregation furnace for segregating and purifying molten aluminum; A crucible, serving as a carrier for molten aluminum; A stirring device for stirring and mixing the molten aluminum in the crucible after the crucible is placed in the segregation furnace; A spraying device for spraying non-sticking aluminum coating on the inner wall of the crucible at the initial stage, and it can adjust the spraying flow rate according to the change of the inner diameter of the crucible; The spraying device includes a vertically sliding support frame (1), a spraying liquid pipeline (2) is fixed below the support frame (1), and a flow control valve (3) is installed on the spraying liquid pipeline (2); A support plate (4) is fixed below the support frame (1), a sliding plate (5) that slides horizontally is provided on the support plate (4), and a spraying head is fixed at the outermost side of the sliding plate (5), and the spraying head is connected to the spraying liquid pipeline (2) through a hose; The sliding plate (5) is connected to the control handle of the valve of the flow control valve (3), and the horizontal sliding of the sliding plate (5) controls the opening size of the valve.

2. The device for preparing high-purity metal by segregation purification according to claim 1, wherein, A first connecting rod (6) is hinged at the upper end of the sliding plate (5), a second connecting rod (7) is hinged at the upper end of the first connecting rod (6), and the other end of the second connecting rod (7) is coaxially fixed with the control handle of the valve.

3. The device for preparing high-purity metal by segregation purification according to claim 1, wherein A horizontal slideway is provided on the support plate (4), the sliding plate (5) slides along the slideway and the outer end of the sliding plate (5) is placed outside the support plate (4).

4. The device for preparing high-purity metal by segregation purification according to claim 2, characterized in that, A spring (8) is fixed on the support plate (4), the other end of the spring (8) is fixedly connected to the sliding plate (5), and the spring (8) always pushes the sliding plate (5) to move away from the support plate (4).

5. The device for preparing high-purity metal by segregation purification according to claim 1, characterized in that, A guide wheel (9) is rotatably provided at the outermost end of the sliding plate (5), and the guide wheel (9) is in contact with the inner wall of the crucible.

6. The device for preparing high-purity metal by segregation purification according to claim 1, wherein The stirring device includes a furnace cover (10), a rotating arm (11) that can rotate is provided below the furnace cover (10), and a gear (13) that can rotate is provided at the outermost end of the rotating arm (11); An internal gear ring (12) is fixed at the lower end of the furnace cover (10), and the gear (13) meshes with the internal gear ring (12); A rotating shaft (14) is coaxially fixed to the gear (13), a multi-faceted shaft (15) is fixed at the lower end of the rotating shaft (14), and a stirring shaft (16) that rotates along with the multi-faceted shaft (15) and can slide vertically is provided on the multi-faceted shaft (15).

7. The device for preparing high-purity metal by segregation purification according to claim 6, characterized in that, A closed spiral cam groove (17) is provided on the outer circumference of the rotating shaft (14), and a pin shaft (18) is slidably provided in the cam groove (17); A vertically sliding sleeve (19) is provided below the rotating arm (11), and the pin shaft (18) passes through the cam groove (17) and is fixedly connected to the sleeve (19); The upper end of the stirring shaft (16) is rotatably connected to the sleeve (19).

8. The device for preparing high-purity metal by segregation purification according to claim 7, wherein A guide shaft (20) is fixed at the lower end of the rotating arm (11), a guide arm is fixed at the outer end of the sleeve (19), and the lower end of the sleeve (19) slidably passes through the guide arm.

9. A method for preparing high-purity metal by segregation purification, using the preparation device according to any one of claims 1-8, comprising the following steps: S1, the segregation furnace is started and preheated, and after the inner wall of the crucible is sprayed with non-sticking aluminum coating by the spraying device, it is placed in the heating furnace for preheating; S2. Open the furnace lid of the segregation furnace, place the preheated crucible into the segregation furnace, pour the molten aluminum or refined electrolytic aluminum liquid into the crucible, turn on the cooling device on the outer wall of the crucible, and monitor the temperature of the aluminum liquid through the temperature measuring device; S3. After the temperature of the aluminum liquid drops to the set value, close the upper cover of the segregation furnace, and at the same time turn on the heating device, stirring device and vacuum pumping device of the segregation furnace; S4. During the solidification production process of aluminum crystals, control the temperature of the aluminum melt between 660 °C and 680 °C through the temperature measuring device, conduct forced cooling on the purification heat conduction layer through the cooling device, control the temperature gradient of the solid-liquid interface of the aluminum melt in the crucible between 5 °C and 20 °C, monitor the growth rate in real time, adjust and correct the heating temperature of the segregation furnace and the cooling water flow rate in real time according to the growth rate, and control the crystallization rate at 4 - 8 cm / h and the crystallization time at 2 - 4 hours; S5. When the growth of the aluminum crystal reaches the set thickness, turn off the heating device, stirring device and vacuum pumping device of the segregation furnace, turn off the cooling device on the outer wall of the crucible, open the furnace lid (10) of the segregation furnace, and remove the crucible; S6. Pour out the remaining low-grade aluminum liquid in the crucible to obtain high-purity aluminum ingots; S7. After the crucible cools down, remove the aluminum ingot in the crucible, and obtain the finished high-purity aluminum ingot after rinsing, polishing; S8. Melt the finished high-purity aluminum ingot and pour it back into the crucible again, put it into the segregation furnace again, and repeat steps S2 - S7 until high-purity aluminum ingots meeting the purity requirements are obtained.

Images