A method and device for purifying antimony metal

Abstract

The present invention relates to a purification method and device for metallic antimony applied to the field of metallic antimony purification, including a chlorination cylinder with a feed inlet and a gas supply pipe at the top. One side of the chlorination cylinder is connected to a rectification cylinder through a screw feeder. The side of the rectification cylinder far from the chlorination cylinder is connected to a reduction reaction cylinder through a gas guide pipe. The side of the reduction reaction cylinder facing away from the rectification cylinder is connected to a vacuum distillation cylinder through a feed pipe. By means of the cooperation of the first stirring rod, the second stirring rod and the inserted rod, it can move up and down on the surface of the rotating rod, so as to adapt to the change of the stirring depth requirement of the space in the chlorination cylinder when the upper plug plate moves up and down, and perform flexible stirring operations. In addition, through the cooperation of the rotating motor, the pulling rope and the lower plug plate, it can assist the upper plug plate to realize the switching of the sealing state during the up and down movement, so as to adjust the pressure in different spaces in the chlorination cylinder during the up and down movement, and comprehensively improve the reaction efficiency of the chlorination reaction in the chlorination cylinder.

Description

Technical Field

[0001] The present invention relates to a purification method and device, in particular to a purification method and device for metallic antimony applied to the field of metallic antimony purification. Background Art

[0002] High-purity antimony is mainly used in the production of semiconductor compounds such as indium antimonide, gallium antimonide, and aluminum antimonide. Due to the similarity of properties, arsenic, lead, and bismuth are impurities that are difficult to remove during the production of high-purity antimony, resulting in an excessive impurity content in the antimony products prepared by traditional processes.

[0003] The specification of Chinese Patent Application CN118345253A discloses a method for preparing high-purity antimony, including: introducing chlorine gas into refined antimony for chlorination reaction to obtain antimony trichloride; performing rectification purification on the antimony trichloride to obtain high-purity antimony trichloride; and performing a gas-phase reduction reaction on the high-purity antimony trichloride and hydrogen gas to obtain high-purity antimony. The antimony products obtained by using the preparation method of the embodiments of this invention have high purity, and its production process is short, the process is simple and convenient, stable and reliable, and the production cost is low. In addition, the specification of Chinese Patent Application CN118726766A discloses a purification method and device for metallic antimony, which can avoid the problem that the materials above the material receiving plate slide back into the inside of the return material port again, resulting in a decrease in the efficiency of re-conveying unqualified materials.

[0004] In the existing antimony purification methods, during the chlorination process, a single stirring and mixing is used to enhance the uniform mixing of antimony ore and chlorine gas. However, in the actual chlorination process, the single stirring and mixing results in a relatively single stirring surface, and the generation efficiency of antimony trichloride is affected. Summary of the Invention

[0005] Aiming at the above-mentioned existing technology, the technical problem to be solved by the present invention is how to improve the generation efficiency of antimony trichloride during the chlorination process when purifying metallic antimony.

[0006] To solve the above problems, the present invention provides a purification device for metallic antimony, including a chlorination cylinder with a feed inlet and a gas supply pipe at the top. One side of the chlorination cylinder is connected to a rectification cylinder through a screw feeder. The side of the rectification cylinder far from the chlorination cylinder is connected to a reduction reaction cylinder through a gas guide pipe. The side of the reduction reaction cylinder facing away from the rectification cylinder is connected to a vacuum distillation cylinder through a feed pipe.

[0007] A driving motor is installed at the center of the top of the chlorination cylinder. The output end of the driving motor is connected to a rotating rod. A lead screw area is provided on the surface of the rotating rod, and a moving sleeve is threadedly sleeved on the surface of the lead screw area. An upper plug plate is fixedly installed on the surface of the moving sleeve, and a lower plug plate is rotatably sleeved on the surface of the moving sleeve through a self-resetting rotating shaft. A plurality of round holes are provided in both the upper plug plate and the lower plug plate. A rotating motor is installed on the surface of the moving sleeve. The output end of the rotating motor is connected to a pulling rope, and the tail end of the pulling rope is connected to the bottom surface of the lower plug plate;

[0008] A plurality of first stirring rods are installed on the surface of the rotating rod and are distributed above and below the lead screw area. A plurality of chutes are provided on the surface of the rotating rod and are arranged at intervals with the first stirring rods. A wedge-shaped slider is slidably connected inside the chute. A plugging rod is connected to the surface of the wedge-shaped slider, and a plurality of second stirring rods arranged vertically are fixedly installed on the surface of the plugging rod.

[0009] In the above-mentioned purification device for antimony metal, by using the cooperation of the first stirring rod, the second stirring rod and the plugging rod, it can move up and down on the surface of the rotating rod, so as to adapt to the change in the stirring depth requirement of the space inside the chlorination cylinder when the upper plug plate moves up and down, and perform flexible stirring operations.

[0010] As a further improvement of the present application, annular grooves are provided on the surfaces of the upper plug plate and the lower plug plate facing away from each other. A plurality of rotating hoops are rotatably clamped inside the annular grooves, and the ends of the annular grooves are connected to the rotating hoops. When the moving sleeve moves to the end position of the lead screw area, the wedge-shaped slider moves to the end of the chute.

[0011] As a further improvement of the present application, the distance between the bottom end of the lower chute and the bottom end of the rotating rod does not exceed one-fifth of the length value of the rotating rod itself, and a filter screen is rotatably connected to the surface of the rotating rod through a bushing and is located below the lowermost chute. A plurality of filter holes are provided inside the filter screen.

[0012] As a further improvement of the present application, heating layers are installed inside the vacuum distillation cylinder, the reduction reaction cylinder and the rectification cylinder. The inside of the vacuum distillation cylinder is divided into two independent cavities arranged vertically by a heat insulation plate, and the two independent cavities are connected by a diversion pipe with an internal check valve. The heating layer is arranged in the lower independent cavity. A refrigerator is installed on the back of the vacuum distillation cylinder, and the input end of the refrigerator is connected to the upper independent cavity through a hose.

[0013] As a further improvement of the present application, in the initial state, the centers of the round holes inside the lower plug plate and the round holes inside the upper plug plate are on the same axis, and the length of the pulling rope is less than half of the circumference of the moving sleeve.

[0014] As a further improvement of the present application, a one-way valve is installed inside the air supply pipe, and the lower plugging rod is located outside the rotating motor. The diameter of the round hole is larger than the diameter of the filter hole inside the filter screen.

[0015] As a further improvement of the present application, an electronic valve is installed inside the air supply pipe, and a displacement sensor is installed inside the upper plug plate. The displacement sensor is signal-connected to the electronic valve and the rotating motor. When the upper plug plate moves upward, the electronic valve opens; when the upper plug plate moves downward, the rotating motor shuts down for 2 - 3 s and then restarts.

[0016] As another improvement of the present application, a method for purifying antimony metal includes the following working steps:

[0017] S1. Put the crude antimony ore into the chlorination cylinder through the feed inlet, and use the cooperation of the upper plug plate, the lower plug plate, the first stirring rod and the second stirring rod to perform dynamic extrusion and stirring treatment on the chlorine gas and the crude antimony ore intermittently introduced into the chlorination cylinder for multiple times to generate antimony trichloride. Then, send the antimony trichloride into the rectification cylinder through the screw feeder;

[0018] S2. Use the heating layer in the rectification cylinder to perform heating treatment to purify the antimony trichloride in S1 to generate gaseous antimony trichloride, and transfer it unidirectionally to the reduction reaction cylinder through the gas guide pipe;

[0019] S3. The gaseous antimony trichloride is mixed with hydrogen in the reduction reaction cylinder for dynamic reduction treatment, and the temperature in the reduction reaction cylinder is controlled at 550 - 600 °C to generate granular antimony products;

[0020] S4. Put the generated granular antimony products into the vacuum distillation cylinder for distillation treatment, and control the heating temperature in the vacuum distillation cylinder at 800 - 900 °C to separate lead and bismuth impurities. After condensing the obtained steam, high-purity antimony products are obtained.

[0021] In summary, by using the cooperation of the first stirring rod, the second stirring rod and the insertion rod, it can move up and down on the surface of the rotating rod to adapt to the change in the stirring depth requirement of the space in the chlorination cylinder when the upper plug plate moves up and down, and perform flexible stirring operations. In addition, through the cooperation of the rotating motor, the pulling rope and the lower plug plate, it can assist the upper plug plate to switch the sealing state during the up and down movement, so as to adjust the pressure in different spaces in the chlorination cylinder during the up and down movement, making the pressure in the two spaces in a dynamically increasing and decreasing state, and comprehensively improving the reaction efficiency of the chlorination reaction in the chlorination cylinder. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 For the first embodiment of the present application Schematic diagram of the overall structure Figure;

[0023] Figure 2 For the first embodiment of the present application Internal structure of the chlorination cylinder Figure;

[0024] Figure 3Installation diagram of the rotating rod, lead screw area and chute for the first embodiment of this application;

[0025] Figure 4 For the first embodiment of this application Installation of the first stirring rod and the wedge-shaped slider Figure;

[0026] Figure 5 For the first embodiment of this application Installation of the rotating motor and the pulling rope Figure;

[0027] Figure 6 For the first embodiment of this application Schematic diagram of the installation of the annular groove Figure;

[0028] Figure 7 Sealing state diagram of the upper plug and lower plug for the first embodiment of this application;

[0029] Figure 8 Schematic diagram of the state of the upper plug descending to adjust the space inside the chlorination cylinder for the first embodiment of this application;

[0030] Figure 9 Schematic diagram of the method flow for the second embodiment of this application.

[0031] Explanation of the reference numerals in the figure:

[0032] 1. Chlorination cylinder; 2. Screw feeder; 3. Rectification cylinder; 4. Reduction reaction cylinder; 5. Vacuum distillation cylinder; 6. Driving motor; 7. Filter screen; 8. Rotating rod; 81. Lead screw area; 82. Chute; 83. Wedge-shaped slider; 9. First stirring rod; 10. Second stirring rod; 11. Lower plug; 12. Upper plug; 13. Rotating motor; 14. Pulling rope; 15. Annular groove. Specific implementation manners

[0033] The following will describe in detail the two embodiments of this application with reference to the accompanying drawings.

[0034] The first embodiment:

[0035] Figure 1 Shows a purification device for metallic antimony, including a chlorination cylinder 1 with a feed inlet and a gas supply pipe at the top. One side of the chlorination cylinder 1 is connected to a rectification cylinder 3 through a screw feeder 2. The side of the rectification cylinder 3 away from the chlorination cylinder 1 is connected to a reduction reaction cylinder 4 through a gas guide pipe. The side of the reduction reaction cylinder 4 facing away from the rectification cylinder 3 is connected to a vacuum distillation cylinder 5 through a feed pipe;

[0036] Figure 2-5It is shown that a driving motor 6 is installed at the center position of the top of the chlorine cylinder 1. The output end of the driving motor 6 is connected to a rotating rod 8. A lead screw area 81 is provided on the surface of the rotating rod 8, and a moving sleeve is threadedly sleeved on the surface of the lead screw area 81. An upper plug plate 12 is fixedly installed on the surface of the moving sleeve, and a lower plug plate 11 is rotatably sleeved on the surface of the moving sleeve through a self-resetting rotating shaft. A plurality of round holes are provided in both the upper plug plate 12 and the lower plug plate 11. A rotating motor 13 is installed on the surface of the moving sleeve. The output end of the rotating motor 13 is connected to a pulling rope 14, and the tail end of the pulling rope 14 is connected to the bottom surface of the lower plug plate 11;

[0037] A plurality of first stirring rods 9 are installed on the surface of the rotating rod 8 and are distributed above and below the lead screw area 81. A plurality of chutes 82 are provided on the surface of the rotating rod 8 at intervals with the first stirring rods 9. A wedge-shaped slider 83 is slidably connected inside the chute 82. A plugging rod is connected to the surface of the wedge-shaped slider 83, and a plurality of second stirring rods 10 arranged up and down are fixedly installed on the surface of the plugging rod.

[0038] Figure 6 It is shown that annular grooves 15 are provided on the surfaces of the upper plug plate 12 and the lower plug plate 11 facing away from each other. A plurality of rotating hoops are rotatably clamped inside the annular grooves 15, and the ends of the annular grooves 15 are connected to the rotating hoops. When the moving sleeve moves to the end position of the lead screw area 81, the wedge-shaped slider 83 moves to the end of the chute 82.

[0039] The distance between the bottom end of the lower chute 82 and the bottom end of the rotating rod 8 does not exceed one-fifth of the length value of the rotating rod 8 itself. The surface of the rotating rod 8 is rotatably connected to a filter screen 7 located below the lowermost chute 82 through a bushing. A plurality of filter holes are provided inside the filter screen 7.

[0040] Specifically, the design of the filter screen 7 is used to filter and screen the generated antimony trichloride to the lower part of the filter screen 7, and then it is transferred to the rectifying cylinder 3 through the screw feeder 2 for subsequent distillation treatment.

[0041] Heating layers are installed inside the vacuum distillation cylinder 5, the reduction reaction cylinder 4, and the rectifying cylinder 3. The inside of the vacuum distillation cylinder 5 is divided into two independent cavities arranged up and down by a heat insulation plate, and the two independent cavities are connected by a diversion pipe with a built-in check valve. Among them, the heating layer is arranged in the lower independent cavity. A refrigerator is installed on the back of the vacuum distillation cylinder 5, and the input end of the refrigerator is connected to the upper independent cavity through a hose.

[0042] Specifically, the vacuum distillation cylinder 5 can further purify the materials generated in the reduction reaction cylinder 4 by using the different internal distillation temperatures.

[0043] In the initial state, the centers of the round holes in the lower plug plate 11 and the round holes in the upper plug plate 12 are on the same axis, and the length of the pulling rope 14 is less than half of the circumference of the moving sleeve.

[0044] A one-way valve is installed inside the air supply pipe, and the lower plugging rod is located outside the rotating motor 13. The diameter of the round hole is larger than the diameter of the filtering holes in the filter screen 7.

[0045] Specifically, due to the design of the one-way valve, when the upper plugging plate 12 and the lower plugging plate 11 in the plugged state move upward, the gas in the space above the upper plugging plate 12 in the chlorination cylinder 1 will not be discharged through the air supply pipe (at this time, the feeding port is in a closed state due to no longer feeding), thereby ensuring that as the upper plugging plate 12 and the lower plugging plate 11 in the plugged state move upward, the pressure in the upper space can increase smoothly, so as to promote the forward progress of the chlorination reaction.

[0046] Specifically, in this embodiment, considering that chlorine and hydrogen chloride gases are corrosive, each component is treated with anti-corrosion to enhance the service life of this purification device.

[0047] When carrying out the purification treatment of antimony metal, the crude antimony ore is put into the chlorination cylinder 1 through the feeding port, and then chlorine gas is introduced into the chlorination cylinder 1. At normal temperature, the crude antimony ore and chlorine gas react in the chlorination cylinder 1 to generate antimony trichloride, and a stirring structure (which is a prior art and will not be elaborated too much) is used to promote the full progress of the chlorination process in the chlorination cylinder 1.

[0048] After the chlorination reaction is completed, the generated antimony trichloride is transferred into the rectification cylinder 3 by the screw feeder 2 for distillation treatment. The antimony trichloride becomes gaseous and is transferred into the reduction reaction cylinder 4 through the air guide pipe. Hydrogen gas is conveyed into the reduction reaction cylinder 4 through the conduit, and the temperature in the reduction reaction cylinder 4 is controlled within the range of 550 - 600 °C for reduction treatment, thereby generating granular antimony metal (there may be other impurities in the antimony metal).

[0049] The antimony metal (which may carry other impurities) obtained after reduction enters the vacuum distillation cylinder 5 for vacuum distillation treatment, and the possible lead and bismuth impurities are separated.

[0050] During the chlorination process, first keep the overlapping state of the round holes in the upper plugging plate 12 and the lower plugging plate 11, so that the crude antimony ore and chlorine gas entering the chlorination cylinder 1 through the feeding port and the air supply pipe can pass through the round holes and enter the lower part of the lower plugging plate 11, and fall above the filter screen 7. Then start the rotating motor 13 to drive the pulling rope 14 to wind up a short distance, thereby driving the connected lower plugging plate 11 to rotate slightly, so that the round holes in the upper plugging plate 12 and the lower plugging plate 11 are in a misaligned state (as Figure 7As shown, the upper plug plate 12 and the lower plug plate 11 form a closed structure to isolate the space inside the chlorination cylinder 1. As the driving motor 6 rotates, it drives the moving sleeve to move up and down on the surface of the lead screw area 81. Thus, through the connection between the annular groove 15 and the rotating hoop, the insertion rod and the wedge-shaped slider 83 are driven to move up and down synchronously. During this process, since the wedge-shaped slider 83 is in sliding contact with the chute 82, when the rotating rod 8 rotates, the wedge-shaped slider 83 can be driven to rotate. At this time, the second stirring rod 10 on the surface of the insertion rod can rotate synchronously when it undergoes a vertical displacement (since the rotating hoop is connected to the insertion rod, and the rotating hoop and the annular groove 15 are rotationally clamped, the second stirring rod 10 will not affect the upper plug plate 12 when it rotates synchronously with the rotating rod 8).

[0051] Taking the descent of the upper plug plate 12 as an example, the volume of the space between the top wall of the chlorination cylinder 1 and the top of the upper plug plate 12 increases. As the upper plug plate 12 descends, the insertion rod descends, which will drive the second stirring rod 10 that was originally almost at the same height as and arranged staggeredly with the upper first stirring rod 9 to descend, and stir the mixture (crude antimony ore, chlorine, and the generated antimony trichloride) in the enlarged space (because the volume has increased and the stirring depth of the original upper first stirring rod 9 is limited, the descending second stirring rod 10 can be used for supplementary stirring to achieve the mixing process). Moreover, as the upper plug plate 12 descends, the volume of the space below the lower plug plate 11 will be reduced, and thus the pressure in the lower space will increase, which can promote the forward progress of the chlorination reaction below (and at this time, the second stirring rod 10 below is almost at the same height as the first stirring rod 9 below but in a staggered arrangement state, which can also play a role in stirring the mixture in the lower space). Furthermore, the efficiency of the chlorination reaction in the upper and lower two spaces can be improved to varying degrees (as Figure 8 shown).

[0052] The second implementation method:

[0053] Figure 9 Disclosed is a method for purifying metallic antimony, including the following working steps:

[0054] S1. Put the crude antimony ore into the chlorination cylinder 1 through the feed inlet, and use the cooperation of the upper plug plate 12, the lower plug plate 11, the first stirring rod 9, and the second stirring rod 10 to perform dynamic extrusion and stirring treatment on the chlorine and the crude antimony ore that are intermittently introduced into the chlorination cylinder 1 multiple times to generate antimony trichloride, and then send the antimony trichloride into the rectification cylinder 3 through the screw feeder 2;

[0055] S2. Use the heating layer in the rectification cylinder 3 to perform heating treatment to purify the antimony trichloride in S1 to generate gaseous antimony trichloride, and transfer it unidirectionally to the reduction reaction cylinder 4 through the gas guide pipe;

[0056] S3. Gaseous antimony trichloride is mixed with hydrogen in the reduction reaction cylinder 4 for a dynamic reduction treatment. The temperature inside the reduction reaction cylinder 4 is controlled at 550 - 600 degrees Celsius to produce granular antimony products.

[0057] S4. The generated granular antimony products are put into the vacuum distillation cylinder 5 for distillation treatment. The heating temperature inside the vacuum distillation cylinder 5 is controlled at 800 - 900 degrees Celsius to separate lead and bismuth impurities. After the obtained steam is condensed, high-purity antimony products are obtained.

[0058] An electronic valve is installed inside the air supply pipe, and a displacement sensor is installed inside the upper plug plate 12. The displacement sensor is signal-connected to the electronic valve and the rotating motor 13. When the upper plug plate 12 moves upward, the electronic valve opens. When the upper plug plate 12 moves downward, the rotating motor 13 closes and restarts after 2 - 3 seconds.

[0059] Specifically, when carrying out the purification treatment of metallic antimony, during the dynamic extrusion and stirring process according to the first embodiment, when the upper plug plate 12 moves upward (the rotating motor 13 starts to drive the inner round holes of the upper plug plate 12 and the lower plug plate 11 to be misaligned), the volume of the space above the upper plug plate 12 decreases and the pressure increases. At this time, chlorine gas is introduced into the air supply pipe, which will further strengthen the pressure in the upper space and increase the amount of reactants, further promoting the forward progress of the chlorination reaction. After that, the upper plug plate 12 needs to move downward. At this time, the rotating motor 13 is turned off, and under the action of the self-resetting rotating shaft, the round holes in the upper plug plate 12 and the lower plug plate 11 return to the overlapping state. At this time, the antimony trichloride and chlorine gas generated by the reaction in the upper space can be transferred to the lower space, supplementing the reactants in the lower space, and enabling the generated antimony trichloride to pass through the filter screen 7 to reach below the filter screen 7. Then the rotating motor 13 restarts (at this time the electronic valve is closed) to make the upper plug plate 12 and the lower plug plate 11 return to the sealed state, and the extrusion treatment of the lower space is carried out.

[0060] In summary, by using the cooperation of the first stirring rod 9, the second stirring rod 10 and the insertion rod, the present application can move up and down on the surface of the rotating rod 8 to adapt to the change in the stirring depth requirement of the space inside the chlorination cylinder 1 when the upper plug plate 12 moves up and down, and perform flexible stirring operations. In addition, through the cooperation of the rotating motor 13, the pulling rope 14 and the lower plug plate 11, it can assist the upper plug plate 12 to switch the sealed state during the up and down movement, so as to adjust the pressure in different spaces inside the chlorination cylinder 1 during the up and down movement, making the pressure in the two spaces in a dynamically increasing and decreasing state, and comprehensively improving the reaction efficiency of the chlorination reaction inside the chlorination cylinder 1.

[0061] Combined with the current actual requirements, the above-mentioned implementation manner adopted by the present application does not limit the protection scope thereto. Within the scope of knowledge possessed by those skilled in the art, various changes made without departing from the concept of the present application still fall within the protection scope of the present invention.

Claims

1. A purification device for metallic antimony, comprising a chlorination cylinder (1) with a feed inlet and a gas supply pipe at the top, characterized in that: One side of the chlorination cylinder (1) is connected to a rectification cylinder (3) through a screw feeder (2). One side of the rectification cylinder (3) far from the chlorination cylinder (1) is connected to a reduction reaction cylinder (4) through a gas guide pipe. One side of the reduction reaction cylinder (4) facing away from the rectification cylinder (3) is connected to a vacuum distillation cylinder (5) through a feed pipe; A driving motor (6) is installed at the center of the top of the chlorination cylinder (1). The output end of the driving motor (6) is connected to a rotating rod (8). A lead screw area (81) is provided on the surface of the rotating rod (8). A moving sleeve is threadedly sleeved on the surface of the lead screw area (81). An upper plug plate (12) is fixedly installed on the surface of the moving sleeve. A lower plug plate (11) is rotatably sleeved on the surface of the moving sleeve through a self-resetting rotating shaft. A plurality of round holes are provided in both the upper plug plate (12) and the lower plug plate (11). A rotating motor (13) is installed on the surface of the moving sleeve. The output end of the rotating motor (13) is connected to a pulling rope (14), and the tail end of the pulling rope (14) is connected to the bottom surface of the lower plug plate (11); A plurality of first stirring rods (9) are installed on the surface of the rotating rod (8) and are distributed above and below the lead screw area (81). A plurality of chutes (82) are provided on the surface of the rotating rod (8) and are arranged at intervals with the first stirring rods (9). A wedge-shaped slider (83) is slidably connected inside the chute (82). A plugging rod is connected to the surface of the wedge-shaped slider (83). A plurality of second stirring rods (10) arranged up and down are fixedly installed on the surface of the plugging rod; Circular grooves (15) are provided on the surfaces of the upper plug plate (12) and the lower plug plate (11) facing away from each other. A plurality of rotating hoops are rotatably clamped inside the circular grooves (15). The end of the circular groove (15) is connected to the rotating hoop. When the moving sleeve moves to the end position of the lead screw area (81), the wedge-shaped slider (83) moves to the end of the chute (82); The distance between the bottom end of the lower chute (82) and the bottom end of the rotating rod (8) does not exceed one-fifth of the length value of the rotating rod (8) itself. A filter screen (7) is rotatably connected to the surface of the rotating rod (8) through a bushing and is located below the lowermost chute (82). A plurality of filter holes are provided inside the filter screen (7); Heating layers are installed inside the vacuum distillation cylinder (5), the reduction reaction cylinder (4), and the rectification cylinder (3). The inside of the vacuum distillation cylinder (5) is divided into two independent cavities arranged up and down by a heat insulation plate. The two independent cavities are connected by a diversion pipe with a built-in check valve. The heating layer is arranged in the lower independent cavity. A refrigerator is installed on the back of the vacuum distillation cylinder (5). The input end of the refrigerator is connected to the upper independent cavity through a hose.

2. The purification device for metallic antimony according to claim 1, wherein: In the initial state, the centers of the round holes inside the lower plug plate (11) and the round holes inside the upper plug plate (12) are on the same axis, and the length of the pulling rope (14) is less than half of the circumference of the moving sleeve.

3. The purification device for metallic antimony according to claim 2, wherein: A one-way valve is installed inside the air supply pipe. The lower plugging rod is located outside the rotating motor (13). The diameter of the round hole is larger than the diameter of the filter holes inside the filter screen (7).

4. A purification device for metallic antimony according to claim 3, characterized in that: An electronic valve is installed inside the air delivery pipe. A displacement sensor is installed inside the upper plug plate (12), and the displacement sensor is in signal connection with the electronic valve and the rotating motor (13). When the upper plug plate (12) moves upward, the electronic valve opens; when the upper plug plate (12) moves downward, the rotating motor (13) closes and restarts after 2 - 3 s.

5. A method for purifying antimony metal, using the purification device as described in claim 4, characterized in that, It includes the following working steps: S1. Put the crude antimony ore into the chlorination cylinder (1) through the feed inlet. By the cooperation of the upper plug plate (12), the lower plug plate (11), the first stirring rod (9) and the second stirring rod (10), perform dynamic extrusion and stirring treatment on the chlorine gas and the crude antimony ore that are intermittently introduced into the chlorination cylinder (1) multiple times to generate antimony trichloride, and then send the antimony trichloride into the rectification cylinder (3) through the screw feeder (2); S2. Use the heating layer inside the rectification cylinder (3) for heating treatment to purify the antimony trichloride in S1 to generate gaseous antimony trichloride, and transfer it unidirectionally to the reduction reaction cylinder (4) through the gas guiding pipe; S3. The gaseous antimony trichloride is mixed with hydrogen in the reduction reaction cylinder (4) for dynamic reduction treatment, and the temperature inside the reduction reaction cylinder (4) is controlled at 550 - 600 °C to generate granular antimony products; S4. Put the generated granular antimony products into the vacuum distillation cylinder (5) for distillation treatment, and control the heating temperature inside the vacuum distillation cylinder (5) at 800 - 900 °C to separate lead and bismuth impurities, and obtain high-purity antimony products after condensing the obtained steam.

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