A production process of high-purity antimony powder

Abstract

The invention discloses a production process of high-purity antimony powder, and relates to the technical field of high-purity antimony powder production. The production process of high-purity antimony powder includes the following steps: S1: presetting, pre-preparing a high-purity antimony powder production device; S2: feeding, feeding crude antimony into the high-purity antimony powder production device; S3: purification, after step S2, the high-purity antimony powder production device purifies the crude antimony put in, and collects the purified high-purity antimony powder. The production process of high-purity antimony powder, under a negative pressure state, heats and insulates the crucible body in different zones, so that impurities such as arsenic with a lower boiling point can be volatilized first and condensed and collected, and then the bottom of the crucible is continuously heated, so that the antimony is volatilized, condensed and crushed, and high-purity antimony powder is formed for collection; when heating in different zones, it is convenient to control the temperature of the different zones, and the annular cover and the conical titanium plate can be cooled to improve the efficiency of condensation, thereby improving the efficiency and quality of high-purity antimony powder production.

Description

Technical Field

[0001] The invention relates to the technical field of high-purity antimony powder production, in particular to a production process of high-purity antimony powder. Background Art

[0002] Antimony powder is a shiny silvery white or dark gray metal powder. High-purity antimony powder is mainly used in the semiconductor manufacturing industry. Silver antimonide and gallium antimonide are typical antimonide semiconductors formed by high-purity antimony. In addition, high-purity antimony can be used as a dopant for semiconductor silicon and germanium to improve their performance. It can also be used to prepare thermoelectric conversion elements, cooling elements, piezoelectric crystals and infrared detectors. With the development of modern information materials, the use of high-purity antimony is becoming more and more extensive. The purity of antimony in the prior art is not enough, and crude antimony needs to be purified. The traditional production method of high-purity antimony powder can be divided into three categories according to the method of preparing high-purity antimony from different raw materials: preparing high-purity by purifying antimony compounds; preparing high-purity antimony by pyrometallurgical smelting of industrial pure metal antimony; preparing high-purity antimony by electrolytic refining of antimony; these methods all use certain characteristics of antimony or other compounds, and adopt unit operations such as recrystallization, distillation, electrolysis, hydrogen reduction, fuming, extraction, and regional melting to separate impurity elements, thereby achieving the purpose of purification.

[0003] However, the existing production process of high-purity antimony powder is not convenient and fast enough when used, and the purified purity is not high enough, which affects the production efficiency and quality of the high-purity antimony powder. Summary of the invention

[0004] The purpose of the present invention is to provide a production process of high-purity antimony powder to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a production process of high-purity antimony powder, comprising the following steps:

[0006] S1: Pre-set, pre-prepare high purity antimony powder production equipment;

[0007] S2: feeding the crude antimony into the high-purity antimony powder production device;

[0008] S3: Purification: After step S2, the high-purity antimony powder production device purifies the input crude antimony and collects the purified high-purity antimony powder;

[0009] The high-purity antimony powder production device comprises a crucible body and a vacuum box body, and the crucible body comprises a crucible cover, the vacuum box body comprises a box door and a heating module arranged at the bottom, and a fixed tube is fixedly inserted at the top of the crucible cover, an exhaust pipe is fixedly inserted at the side wall of the fixed pipe, and a one-way valve is arranged in the exhaust pipe, the top of the crucible cover is fixedly connected to a limiting ring, and the side wall of the fixed pipe is sequentially sleeved with a conical titanium plate, a stainless steel cover and a stainless steel sealing sleeve from bottom to top, a plurality of air holes arranged in an array are opened on the side wall of the fixed pipe in the stainless steel sealing sleeve, a plurality of first through holes arranged in an array are opened on the top of the crucible cover, and a A first sealing mechanism for plugging and sealing the first through hole is provided, a second sealing mechanism is provided in the fixed tube, a first annular groove is provided on the side wall of the stainless steel sealing sleeve, two semicircular collecting plates are inserted in the first annular groove, and a U-shaped block is fixedly connected to the side wall of the stainless steel sealing sleeve, a second annular groove is provided on the inner side wall of the conical titanium plate, and a plurality of powder collecting holes arranged in an array are provided at the bottom of the second annular groove, a third annular groove is provided on the side wall of the conical titanium plate, and two arc-shaped collecting grooves are inserted in the third annular groove, and a crushing mechanism for crushing the condensed high-purity antimony is provided in the second annular groove;

[0010] The two opposite side walls of the vacuum box body are both provided with a control mechanism for controlling the heating temperature of the crucible body, and the top of the vacuum box body is provided with a cooling mechanism for cooling the conical titanium plate and the stainless steel sealing sleeve.

[0011] Preferably, the crushing mechanism includes a rotating ring rotatably connected to the inner side wall of the second annular groove, and the side wall of the rotating ring is fixedly connected to a plurality of connecting blocks arranged in an array, the bottom of each connecting block is connected to a U-shaped plate via a lifting mechanism, and the side wall of the U-shaped plate is rotatably connected to a rolling roller via a rotating shaft, the outer side wall of the conical titanium plate is fixedly connected to a fixed block, and the top of the fixed block is fixedly connected to a motor, the output end of the motor is fixedly connected to a driving wheel, and the driving wheel is inserted in the conical titanium plate and abuts against the side wall of the rotating ring.

[0012] Preferably, each of the control mechanisms includes a first movable plate, and the first movable plate is connected to the inner wall of the vacuum box body through a movable mechanism, a plurality of insulating tubes arranged in an array are fixedly inserted into the side wall of the first movable plate, and a temperature sensor is arranged in each insulating tube, a hollow arc-shaped cover is fixedly inserted into the side walls of the two insulating tubes located above, and the side wall of the vacuum box body is fixedly connected to a first cooling box, two symmetrically arranged first liquid supply pumps are fixedly connected to one side of the first cooling box, and the other end of each first liquid supply pump is fixedly connected to a first solenoid valve, a first liquid inlet pipe is fixedly connected between the first solenoid valve and the arc-shaped cover, and two symmetrically arranged connecting pipes are connected to the other side of the first cooling box, and the other end of each connecting pipe is fixedly connected to a heat exchanger, the inlet of the heat exchanger is fixedly connected to a second solenoid valve, and a first liquid return pipe is fixedly connected between the second solenoid valve and the arc-shaped cover.

[0013] Preferably, the cooling mechanism includes a second movable plate, and the second movable plate is connected to the top of the vacuum box body through a lifting module, the side wall of the second movable plate is fixedly connected with a hollow annular cover and a hollow conical cover, and the top of the vacuum box body is fixedly connected with a second cooling box, one side of the second cooling box is fixedly connected with a third connecting pipe, and the annular cover and the conical cover and the third connecting pipe are fixedly connected with a second liquid return pipe, the other side of the second cooling box is fixedly connected with a second liquid supply pump, and the outlet of the second liquid supply pump is fixedly connected with a second liquid inlet pipe, a fifth connecting pipe is fixedly connected between the annular cover and the second liquid inlet pipe, and a sixth connecting pipe is fixedly connected between the annular cover and the second liquid inlet pipe, and the side walls of the fifth connecting pipe and the sixth connecting pipe are provided with an on-off mechanism.

[0014] Preferably, the first sealing mechanism includes a first annular plate arranged at the bottom of the crucible cover, and a plurality of second through holes arranged in an array are opened at the bottom of the first annular plate, an inner side wall of the first annular plate is fixedly connected to a connecting plate, and a moving rod is fixedly connected to the top of the connecting plate, and the moving rod is inserted in the fixed tube and connected to the top of the fixed tube through a moving assembly.

[0015] Preferably, the second sealing mechanism includes a second fixing ring fixedly connected to the bottom of the fixed tube, and the top of the second fixing ring is provided with a plurality of third through holes arranged in an array, the side wall fixing sleeve of the movable rod is provided with a fourth fixing ring, and the bottom of the fourth fixing ring is provided with a plurality of fourth through holes arranged in an array.

[0016] Preferably, the moving assembly includes a ring fixedly mounted on the side wall of the moving rod, and a first spring is fixedly connected between the ring and the top of the fixed tube, the side wall of the second moving plate is connected to a first push plate through a moving module, and the first push plate includes an inclined surface.

[0017] Preferably, the lifting mechanism includes two symmetrically arranged sliding rods fixedly connected to the top of each U-shaped plate, and the upper end of the sliding rod is fixedly connected with a stop block, the side wall of each sliding rod is provided with a second spring, and the side wall of the second annular groove is fixedly connected with a plurality of triangular blocks arranged in an array.

[0018] Preferably, the on-off mechanism is fixedly inserted into the first fixed cover on the side wall of the fifth connecting tube, and the first sliding plate is slidably connected in the first fixed cover, the side wall of the first sliding plate is provided with a fifth through hole, and a third spring is fixedly connected between the first sliding plate and the first fixed cover, the side wall of the sixth connecting tube is fixedly inserted with the second fixed cover, and the second sliding plate is inserted in the second fixed cover, the side wall of the second sliding plate is provided with a sixth through hole, and a fourth spring is fixedly connected between the second sliding plate and the second fixed cover, the side wall of the second movable plate is fixedly connected with an L-shaped plate, and the top of the L-shaped plate is fixedly connected with an L-shaped block, the side wall of the L-shaped block is fixedly connected with an inclined plate, the side wall of the L-shaped plate is fixedly connected with a connecting rod, and the other end of the connecting rod is fixedly connected with a pushing block arranged in a triangle.

[0019] Preferably, the moving mechanism includes two symmetrically arranged sleeve rods fixedly connected to the inner side wall of the vacuum box body, and the side wall of the sleeve rod is sleeved with a sleeve, the other end of the sleeve is fixed to the side wall of the first moving plate, and the side wall of each sleeve is sleeved with a fifth spring, the side wall of the first moving plate is fixedly connected to the second push plate, and the top of the second push plate is provided with an inclined groove, the inner side wall of the vacuum box body is fixedly connected to a guide rail, and a moving block is slidably connected to the guide rail, the top of the moving block is fixedly connected to a pushing pin, the pushing pin is inserted in the inclined groove, and the side wall of the moving block is fixedly connected to the pushing rod.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The production process of the high-purity antimony powder comprises the following steps: firstly putting the crude antimony into a crucible body, then placing the crucible body on a heating module in a vacuum box body, sleeve a conical titanium plate on the side wall of a fixed tube and place it on a crucible cover, then cover with a stainless steel cover and a stainless steel sealing sleeve and sleeve them on the side wall of the fixed tube, close the box door, start a water cooling system, start a vacuum pump, control the vacuum degree below 13 Pa, then drive the annular cover through the lifting module and the second moving plate, and finally The conical cover is moved downward, and the annular cover is fitted with the top of the stainless steel sealing sleeve, and the conical cover is fitted with the top of the conical titanium plate. Then, the bottom temperature of the crucible body is controlled at 600-900°C, and the middle temperature is controlled at 500-650°C and the upper temperature is controlled at 350-450°C by the control mechanism. The temperature is kept at 13 hours to make the impurities such as arsenic with a lower boiling point evaporate first. At this time, the first annular plate can seal the first through hole so that it can only enter through the third through hole and the fourth through hole. The first push plate is driven by the moving module to move in a direction away from the second moving plate, so that the inclined surface abuts against the upper end of the moving rod. At this time, the moving rod and the fourth fixed ring can be pushed to move downward. At the same time, the first spring is compressed, so that the bottom of the fourth fixed ring abuts against the top of the second fixed ring, and the third through hole and the fourth fixed ring are staggered with each other. At this time, the fourth fixed ring and the second fixed ring can be used to seal the fixed tube. At the same time, when the moving rod moves downward, the first annular plate can be driven downward by the connecting plate to expose the bottom of the first through hole, and the bottom of the crucible is continued to be heated to 650-900°C. At the same time, the control mechanism is stopped. At this time, antimony can evaporate from the first through hole and condense under the action of the conical titanium plate. After condensation, the high-purity antimony powder can fall into the second annular groove and fall into the collection tank for collection after filtering through the powder collection hole.

[0022] The production process of this high-purity antimony powder is to set up a crushing mechanism, etc., and start the motor after the high-purity antimony powder falls into the second annular groove. The rotation of the motor drives the rotation of the driving wheel, thereby driving the rotating ring to rotate, and then driving the U-shaped plate and the rotating shaft to move through the connecting block and the lifting mechanism. At this time, the rolling roller can further crush the particles and lumps in the high-purity antimony powder at the bottom of the second annular groove, and when the stop block abuts against the side wall of the triangular block, it can push the U-shaped plate and the rotating shaft to move upward. At the same time, the second spring is compressed. When the stop block passes over the triangular block, the U-shaped plate and the rotating shaft can move downward and reset under the action of the second spring. This reciprocating process can make the rolling roller move up and down, which not only makes the crushing effect better, but also can form a vibration effect on the second annular groove, so that the filtering effect of the powder collection hole is better, thereby ensuring the collection efficiency and effect of the high-purity antimony powder.

[0023] The production process of high-purity antimony powder is provided with a control mechanism, etc., so that when the box door is closed, it can abut against the end of the push rod during the production of high-purity antimony powder. At this time, the moving block can be pushed to move along the guide rail, and the pushing pin can be driven to slide along the inclined groove, so that the first moving plate can be pushed to move in the direction close to the crucible body. At the same time, the fifth spring is compressed, and the arc cover is driven to fit the side wall of the crucible body through the insulating tube. In addition, the upper arc cover is located on the upper part of the crucible body, and the lower arc cover is located in the middle of the crucible body. The bottom of the crucible body is heated by the heating module, and the temperature is detected by the temperature sensor. If the temperature in the middle is higher than 650°C, or when the temperature of the upper part is higher than 450°C, the first solenoid valve and the second solenoid valve can be opened, and the first liquid supply pump can be started. At this time, the coolant in the first cooling box can enter the arc cover through the first liquid inlet pipe, and can return to the first cooling box through the first liquid return pipe, the heat exchanger and the connecting pipe, so that the coolant circulates, thereby being able to cool the middle or upper part to ensure that the temperature is within the required range. After the cooling is completed, the first solenoid valve, the second solenoid valve and the first liquid supply pump can be closed, so as to facilitate the control of the temperature of the middle and upper parts of the crucible body, which is more convenient and quick to use, and ensures the efficiency and effect of the production of high-purity antimony powder.

[0024] The production process of high-purity antimony powder is provided with a cooling mechanism, etc., so that when the high-purity antimony powder is produced, when the impurities such as arsenic with a low boiling point are condensed, the fifth through hole is aligned with the fifth connecting pipe, the sixth through hole is staggered with the sixth connecting pipe, and the second liquid supply pump is started, so that the coolant in the second cooling box can enter the annular cover through the second liquid inlet pipe and the fifth connecting pipe, and return to the second cooling box through the second liquid return pipe for cooling, and the annular cover can be continuously cooled in this way to ensure the efficiency and effect of its condensation, and when the antimony is condensed, when the first push plate moves in the direction away from the second moving plate, the L-shaped plate and the L-shaped block belt can be used to cool the antimony powder. The movable inclined plate moves so that the inclined plate abuts against the top of the first sliding plate, thereby pushing the first sliding plate to move downward. At the same time, the third spring is compressed, so that the fifth through hole and the fifth connecting pipe are staggered. At the same time, the pushing block is driven to move by the connecting rod. When the pushing block is disengaged from the top of the second sliding plate, the second sliding plate can move upward and reset under the action of the fourth spring, so that the sixth through hole is aligned with the sixth connecting pipe. At this time, the coolant can enter the conical cover through the sixth connecting pipe and return to the second cooling box through the second return pipe, so that the area of ​​the conical titanium plate above the second annular groove can be continuously cooled to ensure the efficiency and effect of antimony condensation. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the structure of the high purity antimony powder production device of the present invention.

[0026] Figure 2 It is a schematic diagram of the overall structure of the vacuum box body in the present invention.

[0027] Figure 3 This is a schematic diagram of the overall structure of the vacuum box body in the present invention from another perspective.

[0028] Figure 4 It is a schematic diagram of the position of the cooling mechanism in the present invention.

[0029] Figure 5 It is a structural schematic diagram of the cooling mechanism in the present invention.

[0030] Figure 6 It is a schematic structural diagram of the crucible body in the present invention.

[0031] Figure 7 It is a schematic diagram of the partial cross-sectional structure of the crucible body in the present invention.

[0032] Figure 8 It is a schematic diagram of the partial cross-sectional structure of the crucible body in the present invention from another viewing angle.

[0033] Fig. 9 for Figure 3 Schematic diagram of the enlarged structure at point A in the middle.

[0034] Fig.10 for Figure 5 Schematic diagram of the enlarged structure at point B in the middle.

[0035] Fig.11 for Figure 5 Schematic diagram of the enlarged structure at point C in the middle.

[0036] Fig.12 for Figure 6 Schematic diagram of the enlarged structure at D in the middle.

[0037] Fig.13 for Figure 6 Schematic diagram of the enlarged structure at E in the middle.

[0038] Fig.14 for Figure 7 Schematic diagram of the enlarged structure at F in the middle.

[0039] Fig.15 for Figure 8 Schematic diagram of the enlarged structure at G in the middle.

[0040] Fig.16 for Figure 8 Schematic diagram of the enlarged structure at H in the middle.

[0041] In the figure: 1, crucible body; 101, crucible cover; 201, first moving plate; 202, insulation pipe; 203, temperature sensor; 204, arc cover; 205, first cooling box; 206, first liquid supply pump; 207, first solenoid valve; 208, first liquid inlet pipe; 209, first liquid return pipe; 210, second solenoid valve; 211, heat exchanger; 212, connecting pipe; 301, lifting module; 302, second moving plate; 304, annular cover; 305, conical cover; 306, second cooling box; 307, third connecting pipe; 308, second liquid return pipe; 30 9, fifth connecting pipe; 310, sixth connecting pipe; 311, second liquid inlet pipe; 312, second liquid supply pump; 401, moving rod; 402, connecting plate; 403, first annular plate; 404, second through hole; 501, second fixing ring; 502, third through hole; 503, fourth fixing ring; 504, fourth through hole; 601, circular ring; 602, first spring; 603, moving module; 604, first push plate; 605, inclined plane; 701, connecting block; 702, U-shaped plate; 703, rotating shaft; 704, rotating ring; 705, driving wheel; 706, fixed Fixed block; 707, motor; 708, rolling roller; 801, sliding rod; 802, stopper; 803, second spring; 804, triangular block; 901, guide rail; 902, moving block; 903, push rod; 904, sleeve rod; 905, sleeve; 906, fifth spring; 907, second push plate; 908, inclined slot; 909, push pin; 1001, first fixed cover; 1002, first sliding plate; 1003, fifth through hole; 1004, third spring; 1005, second fixed cover; 1006, second sliding plate; 1007, sixth through hole; 10 08. Fourth spring; 1009. L-shaped block; 1010. Inclined plate; 1011. L-shaped plate; 1012. Connecting rod; 1013. Pushing block; 11. Vacuum box body; 1101. Box door; 1102. Heating module; 12. Fixed tube; 13. Limiting ring; 14. Conical titanium plate; 15. Stainless steel cover; 16. Stainless steel sealing sleeve; 17. First through hole; 18. Air hole; 19. First annular groove; 20. Collecting plate; 21. Second annular groove; 22. Powder collecting hole; 23. Third annular groove; 24. Collecting groove; 25. Exhaust pipe; 26. U-shaped block. DETAILED DESCRIPTION

[0042] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0043] See also Figure 1-Figure 16 The present invention provides a technical solution: a production process of high-purity antimony powder, comprising the following steps:

[0044] S1: Pre-set, pre-prepare high purity antimony powder production equipment;

[0045] S2: feeding the crude antimony into the high-purity antimony powder production device;

[0046] S3: Purification: After step S2, the high-purity antimony powder production device purifies the input crude antimony and collects the purified high-purity antimony powder;

[0047] The high-purity antimony powder production device includes a crucible body 1 and a vacuum box body 11, and the crucible body 1 includes a crucible cover 101, the vacuum box body 11 includes a box door 1101 and a heating module 1102 arranged at the bottom, and a fixed tube 12 is fixedly inserted at the top of the crucible cover 101, and an exhaust pipe 25 is fixedly inserted at the side wall of the fixed tube 12, and a one-way valve is arranged in the exhaust pipe 25, and the conduction direction of the one-way valve is from the fixed tube 12 to the outside, so as to ensure that the crucible body 1, the stainless steel sealing sleeve 16 and the conical titanium plate 14 can be vacuumed, and impurities such as arsenic with a lower boiling point will not overflow after volatilization, the top of the crucible cover 101 is fixedly connected to a limiting ring 13, and the side wall of the fixed tube 12 is sequentially sleeved with a conical titanium plate 14, a stainless steel cover 15 and a stainless steel sealing sleeve 16 from bottom to top, and the side wall of the fixed tube 12 located in the stainless steel sealing sleeve 16 is provided with a plurality of arrays The crucible cover 101 is provided with a plurality of first through holes 17 arranged in an array on the top, and a first sealing mechanism for sealing the first through holes 17 is provided at the bottom of the crucible cover 101, a second sealing mechanism is provided in the fixed tube 12, and a first annular groove 19 is provided on the side wall of the stainless steel sealing sleeve 16, two semicircular collecting plates 20 are inserted in the first annular groove 19, and a U-shaped block 26 is fixedly connected to the side wall of the stainless steel sealing sleeve 16, a second annular groove 21 is provided on the inner side wall of the conical titanium plate 14, and a plurality of powder collecting holes 22 arranged in an array are provided at the bottom of the second annular groove 21, a third annular groove 23 is provided on the side wall of the conical titanium plate 14, and two arc-shaped collecting grooves 24 are inserted in the third annular groove 23, and a crushing mechanism for crushing the condensed high-purity antimony is provided in the second annular groove 21;

[0048] The two opposite side walls of the vacuum box body 11 are provided with a control mechanism for controlling the heating temperature of the crucible body 1, and the top of the vacuum box body 11 is provided with a cooling mechanism for cooling the conical titanium plate 14 and the stainless steel sealing sleeve 16. Under negative pressure, the crucible body 1 is heated and kept warm in zones, so that impurities such as arsenic with a lower boiling point can be evaporated first and condensed and collected. Then, the bottom of the crucible is heated continuously, so that antimony can be evaporated, condensed and crushed to form high-purity antimony powder for collection, thereby improving the purity of the high-purity antimony powder. During zone heating, it is convenient to control the zone temperature, and the annular cover 304 and the conical titanium plate 14 can be cooled to improve the condensation efficiency, thereby improving the efficiency and quality of the production of high-purity antimony powder.

[0049] The crushing mechanism includes a rotating ring 704 rotatably connected to the inner wall of the second annular groove 21, and the side wall of the rotating ring 704 is fixedly connected with a plurality of connecting blocks 701 arranged in an array, the bottom of each connecting block 701 is connected with a U-shaped plate 702 through a lifting mechanism, and the side wall of the U-shaped plate 702 is rotatably connected with a rolling roller 708 through a rotating shaft 703, the outer wall of the conical titanium plate 14 is fixedly connected with a fixed block 706, and the top of the fixed block 706 is fixedly connected with a motor 707, the output end of the motor 707 is fixedly connected with a driving wheel 705, and the driving wheel 705 is inserted in the conical titanium plate 14 and abuts against the side wall of the rotating ring 704, after the high-purity antimony powder falls into the second annular groove 21, the motor 707 is started, and the rotation of the motor 707 drives the rotation of the driving wheel 705, thereby driving the rotating ring 704 to rotate, and then The U-shaped plate 702 and the rotating shaft 703 are driven to move by the connecting block 701 and the lifting mechanism. At this time, the rolling roller 708 can further crush the particles and lumps in the high-purity antimony powder at the bottom of the second annular groove 21, and when the stop block 802 abuts against the side wall of the triangular block 804, the U-shaped plate 702 and the rotating shaft 703 can be pushed to move upward. At the same time, the second spring 803 is compressed. When the stop block 802 passes the triangular block 804, the U-shaped plate 702 and the rotating shaft 703 can move downward and reset under the action of the second spring 803. This reciprocating movement can make the rolling roller 708 move up and down, which not only makes the crushing effect better, but also can form a vibration effect on the second annular groove 21, so that the filtering effect of the powder collection hole 22 is better, thereby ensuring the collection efficiency and effect of the high-purity antimony powder.

[0050] Each control mechanism includes a first movable plate 201, and the first movable plate 201 is connected to the inner wall of the vacuum box body 11 through a movable mechanism, a plurality of array-arranged insulating tubes 202 are fixedly inserted into the side wall of the first movable plate 201, and a temperature sensor 203 is arranged in each insulating tube 202, a hollow arc cover 204 is fixedly inserted into the side wall of the two insulating tubes 202 located at the top, and a first cooling box 205 is fixedly connected to the side wall of the vacuum box body 11, and two symmetrically arranged first liquid supply pumps 206 are fixedly connected to one side of the first cooling box 205, and each first liquid supply pump 206 The other end of the first cooling box 205 is fixedly connected to a first solenoid valve 207, a first liquid inlet pipe 208 is fixedly connected between the first solenoid valve 207 and the arc cover 204, and the other side of the first cooling box 205 is connected to two symmetrically arranged connecting pipes 212, the other end of each connecting pipe 212 is fixedly connected to a heat exchanger 211, the inlet of the heat exchanger 211 is fixedly connected to a second solenoid valve 210, and a first liquid return pipe 209 is fixedly connected between the second solenoid valve 210 and the arc cover 204. When the high-purity antimony powder is produced, when the box door 1101 is closed, the first movable plate 20 1 moves toward the crucible body 1, and then drives the arc cover 204 to fit with the side wall of the crucible body 1 through the insulation tube 202, and the upper arc cover 204 is located at the upper part of the crucible body 1, and the lower arc cover 204 is located in the middle of the crucible body 1. The bottom of the crucible body 1 is heated by the heating module 1102, and the temperature is detected by the temperature sensor 203. If the temperature in the middle is higher than 650°C, or the temperature in the upper part is higher than 450°C, the first solenoid valve 207 and the second solenoid valve 210 can be opened, and the first liquid supply pump 206 is started. At this time, the first cooling The coolant in the box 205 can enter the arc cover 204 through the first liquid inlet pipe 208, and can return to the first cooling box 205 through the first liquid return pipe 209, the heat exchanger 211 and the connecting pipe 212, so that the coolant circulates, thereby being able to cool the middle or upper part to ensure that the temperature is within the required range. After the cooling is completed, the first solenoid valve 207, the second solenoid valve 210 and the first liquid supply pump 206 can be closed, so as to facilitate the control of the temperature in the middle and upper parts of the crucible body 1, which is more convenient and quick to use, ensuring the efficiency and effect of the production of high-purity antimony powder.

[0051] The cooling mechanism includes a second movable plate 302, and the second movable plate 302 is connected to the top of the vacuum box body 11 through the lifting module 301, the side wall of the second movable plate 302 is fixedly connected with a hollow annular cover 304 and a hollow conical cover 305, and the top of the vacuum box body 11 is fixedly connected with a second cooling box 306, one side of the second cooling box 306 is fixedly connected with a third connecting pipe 307, and a second liquid return pipe 308 is fixedly connected between the annular cover 304 and the conical cover 305 and the third connecting pipe 307, the other side of the second cooling box 306 is fixedly connected with a second liquid supply pump 312, and the outlet of the second liquid supply pump 312 is fixedly connected with a second liquid inlet pipe 311, a fifth connecting pipe 309 is fixedly connected between the annular cover 304 and the second liquid inlet pipe 311, and a sixth connecting pipe 310 is fixedly connected between the annular cover 304 and the second liquid inlet pipe 311, the fifth connecting pipe 309 and the sixth connecting pipe 310 are fixedly connected The side wall is provided with an on-off mechanism. When high-purity antimony powder is produced, when impurities such as arsenic with a lower boiling point are condensed, at this time, the fifth through hole 1003 is aligned with the fifth connecting pipe 309, and the sixth through hole 1007 is staggered with the sixth connecting pipe 310. The second liquid supply pump 312 is started, so that the coolant in the second cooling box 306 can enter the annular cover 304 through the second liquid inlet pipe 311 and the fifth connecting pipe 309, and return to the second cooling box 306 through the second liquid return pipe 308 for cooling. In this way, the annular cover 304 can be continuously cooled to ensure the efficiency and effect of its condensation. In addition, when antimony is condensed, the coolant can enter the conical cover 305 through the sixth connecting pipe 310, and return to the second cooling box 306 through the second liquid return pipe 308, so that the area of ​​the conical titanium plate 14 above the second annular groove 21 can be continuously cooled to ensure the efficiency and effect of antimony condensation.

[0052] The first sealing mechanism includes a first annular plate 403 arranged at the bottom of the crucible cover 101, and a plurality of second through holes 404 arranged in an array are opened at the bottom of the first annular plate 403, a connecting plate 402 is fixedly connected to the inner wall of the first annular plate 403, and a moving rod 401 is fixedly connected to the top of the connecting plate 402, and the moving rod 401 is inserted into the fixed tube 12 and connected to the top of the fixed tube 12 through a moving component. When impurities such as arsenic with a lower boiling point are volatilized, the first annular plate 403 can block and seal the first through hole 17. When antimony needs to be volatilized, the first annular plate 403 is driven to move downward by the moving component, thereby exposing the bottom of the first through hole 17.

[0053] The second sealing mechanism includes a second fixing ring 501 fixedly connected to the bottom of the fixing tube 12, and a plurality of third through holes 502 arranged in an array are provided on the top of the second fixing ring 501, and a fourth fixing ring 503 is provided on the side wall fixing sleeve of the moving rod 401, and a plurality of fourth through holes 504 arranged in an array are provided on the bottom of the fourth fixing ring 503. When impurities such as arsenic with a lower boiling point are volatilized, they can only enter the fixing tube 12 through the third through holes 502 and the fourth through holes 504, and enter the stainless steel sealing sleeve 16 through the air holes 18 for condensation and fall into the collecting plate 20 for collection. When antimony needs to be volatilized, the fourth fixing ring 503 is moved downward, so that the bottom of the fourth fixing ring 503 is against the top of the second fixing ring 501, and the third through holes 502 and the fourth fixing ring 503 are staggered with each other. At this time, the fourth fixing ring 503 and the second fixing ring 501 can be used to seal the fixing tube 12.

[0054] The moving component includes a circular ring 601 fixedly mounted on the side wall of the moving rod 401, and a first spring 602 is fixedly connected between the circular ring 601 and the top of the fixed tube 12. The side wall of the second moving plate 302 is connected to a first push plate 604 through a moving module 603, and the first push plate 604 includes an inclined surface 605. The first push plate 604 is driven by the moving module 603 to move away from the second moving plate 302, so that the inclined surface 605 is against the upper end of the moving rod 401. At this time, the moving rod 401 and the fourth fixed ring 503 can be pushed downward.

[0055] The lifting mechanism includes two symmetrically arranged sliding rods 801 fixedly connected to the top of each U-shaped plate 702, and a stopper 802 is fixedly connected to the upper end of the sliding rod 801. The side wall of each sliding rod 801 is sleeved with a second spring 803, and the side wall of the second annular groove 21 is fixedly connected with a plurality of triangular blocks 804 arranged in an array. When the stopper 802 abuts against the side wall of the triangular block 804, the U-shaped plate 702 and the rotating shaft 703 can be pushed to move upward. At the same time, the second spring 803 is compressed. When the stopper 802 passes over the triangular block 804, the U-shaped plate 702 and the rotating shaft 703 can move downward and reset under the action of the second spring 803. This reciprocating motion can make the rolling roller 708 move back and forth up and down, which not only makes the crushing effect better, but also can form a vibration effect on the second annular groove 21.

[0056] The on-off mechanism is fixedly inserted into the first fixed cover 1001 on the side wall of the fifth connecting tube 309, and the first sliding plate 1002 is slidably connected in the first fixed cover 1001, and the side wall of the first sliding plate 1002 is provided with a fifth through hole 1003, and a third spring 1004 is fixedly connected between the first sliding plate 1002 and the first fixed cover 1001, and the side wall of the sixth connecting tube 310 is fixedly inserted with a second fixed cover 1005, and a second sliding plate 1006 is inserted in the second fixed cover 1005, and the side wall of the second sliding plate 1006 is provided with a sixth through hole 1007, and the second sliding plate 100 6 and the second fixed cover 1005 are fixedly connected with a fourth spring 1008, the side wall of the second movable plate 302 is fixedly connected with an L-shaped plate 1011, and the top of the L-shaped plate 1011 is fixedly connected with an L-shaped block 1009, the side wall of the L-shaped block 1009 is fixedly connected with an inclined plate 1010, the side wall of the L-shaped plate 1011 is fixedly connected with a connecting rod 1012, and the other end of the connecting rod 1012 is fixedly connected with a triangular push block 1013. When producing high-purity antimony powder, when condensing impurities such as arsenic with a lower boiling point, at this time, the fifth through hole 1003 and the fifth connecting pipe 30 9, the sixth through hole 1007 is staggered with the sixth connecting pipe 310, and the second liquid supply pump 312 is started, so that the coolant in the second cooling box 306 can enter the annular cover 304 through the second liquid inlet pipe 311 and the fifth connecting pipe 309, and return to the second cooling box 306 through the second liquid return pipe 308 for cooling, and so on, the annular cover 304 can be continuously cooled to ensure the efficiency and effect of its condensation, and when the antimony is condensed, when the first push plate 604 moves away from the second movable plate 302, it can be cooled by the L-shaped plate 1011 and the L-shaped block 1012. 09 drives the inclined plate 1010 to move, so that the inclined plate 1010 is against the top of the first sliding plate 1002, thereby pushing the first sliding plate 1002 to move downward. At the same time, the third spring 1004 is compressed, so that the fifth through hole 1003 and the fifth connecting tube 309 are staggered. At the same time, the pushing block 1013 is driven to move by the connecting rod 1012. When the pushing block 1013 is disengaged from the top of the second sliding plate 1006, the second sliding plate 1006 can be moved upward and reset under the action of the fourth spring 1008, so that the sixth through hole 1007 is aligned with the sixth connecting tube 310.

[0057] The moving mechanism includes two symmetrically arranged sleeve rods 904 fixedly connected to the inner side wall of the vacuum box body 11, and the side wall of the sleeve rod 904 is sleeved with a sleeve 905, the other end of the sleeve 905 is fixed to the side wall of the first moving plate 201, and the side wall of each sleeve 905 is sleeved with a fifth spring 906, the side wall of the first moving plate 201 is fixedly connected to the second push plate 907, and the top of the second push plate 907 is provided with an inclined groove 908, the inner side wall of the vacuum box body 11 is fixedly connected to the guide rail 901, and the guide rail 901 is slidably connected to the moving block 902, and the top of the moving block 902 is fixedly connected to the push plate 907. The movable pin 909, the pushing pin 909 is inserted in the inclined groove 908, and the side wall of the moving block 902 is fixedly connected with the pushing rod 903. When the high-purity antimony powder is produced, when the box door 1101 is closed, it can be against the end of the pushing rod 903. At this time, the moving block 902 can be pushed to move along the guide rail 901, and the pushing pin 909 can be driven to slide along the inclined groove 908, so as to push the first moving plate 201 to move in the direction close to the crucible body 1. At the same time, the fifth spring 906 is compressed, and then the arc cover 204 is driven to fit the side wall of the crucible body 1 through the insulating tube 202.

[0058] Working principle: When in use, during production, first put the crude antimony into the crucible body 1, then place the crucible body 1 on the heating module 1102 in the vacuum box body 11, sleeve the conical titanium plate 14 on the side wall of the fixed tube 12 and place it on the crucible cover 101, cover the stainless steel cover 15 and the stainless steel sealing sleeve 16 and sleeve them on the side wall of the fixed tube 12, close the box door 1101, turn on the water cooling system, start the vacuum pump, and control the vacuum degree below 13Pa, then drive the annular cover 304 and the conical cover 305 to move downward through the lifting module 301 and the second movable plate 302, and make the annular cover 304 fit with the top of the stainless steel sealing sleeve 16, and the conical cover 305 fit with the top of the conical titanium plate 14;

[0059] Next, the bottom temperature of the crucible body 1 is controlled at 600-900°C, and the middle temperature is controlled at 500-650°C and the upper temperature is controlled at 350-450°C by a control mechanism. The temperature is kept at 13 hours to allow impurities such as arsenic with a lower boiling point to evaporate first. At this time, the first annular plate 403 can block and seal the first through hole 17, so that it can only enter the fixed tube 12 through the third through hole 502 and the fourth through hole 504, and enter the stainless steel sealing sleeve 16 through the air hole 18 to condense and fall into the collection tray 20 for collection. Next, the first push plate 604 is driven by the moving module 603 to move away from the second moving plate 302, so that the inclined surface 605 is against the upper end of the moving rod 401. At this time, the moving rod 401 and the fourth fixed ring 503 can be pushed to move downward. At the same time, the first spring 602 is compressed, so that the fourth fixed ring 503 The bottom of the crucible is against the top of the second fixing ring 501, and the third through hole 502 and the fourth fixing ring 503 are staggered. At this time, the fourth fixing ring 503 and the second fixing ring 501 can be used to seal the fixing tube 12. At the same time, when the moving rod 401 moves downward, the first annular plate 403 can be driven to move downward through the connecting plate 402, so that the bottom of the first through hole 17 is exposed, and the bottom of the crucible is continuously heated to 650-900°C. At the same time, the control mechanism is stopped. At this time, antimony can be volatilized from the first through hole 17 and condensed under the action of the conical titanium plate 14. After condensation, the high-purity antimony powder can fall into the second annular groove 21, and fall into the collecting groove 24 for collection after filtering through the powder collecting hole 22. The antimony is completely volatilized by heat preservation, and finally impurities such as lead with a high boiling point are left in the crucible body 1, so as to achieve the purpose of purification;

[0060] After the high-purity antimony powder falls into the second annular groove 21, the motor 707 is started. The rotation of the motor 707 drives the rotation of the driving wheel 705, thereby driving the rotating ring 704 to rotate, and then driving the U-shaped plate 702 and the rotating shaft 703 to move through the connecting block 701 and the lifting mechanism. At this time, the rolling roller 708 can further crush the particles and agglomerates in the high-purity antimony powder at the bottom of the second annular groove 21, and when the stopper 802 abuts against the side wall of the triangular block 804, it can push the U-shaped plate 702 and the rotating shaft 703 to move. The plate 702 and the rotating shaft 703 move upward, and at the same time, the second spring 803 is compressed. When the stopper 802 passes over the triangular block 804, the U-shaped plate 702 and the rotating shaft 703 can move downward and reset under the action of the second spring 803, and so on, so that the rolling roller 708 can move up and down reciprocatingly, which not only makes the crushing effect better, but also can form a vibration effect on the second annular groove 21, so that the filtering effect of the powder collection hole 22 is better, thereby ensuring the collection efficiency and effect of the high-purity antimony powder;

[0061] At the same time, when producing high-purity antimony powder, when the box door 1101 is closed, it can be against the end of the push rod 903. At this time, the moving block 902 can be pushed to move along the guide rail 901, and the pushing pin 909 can be driven to slide along the inclined groove 908, so that the first moving plate 201 can be pushed to move in the direction close to the crucible body 1. At the same time, the fifth spring 906 is compressed, and then the arc cover 204 is driven to fit the side wall of the crucible body 1 through the insulating tube 202. In addition, the upper arc cover 204 is located at the upper part of the crucible body 1, and the lower arc cover 204 is located in the middle of the crucible body 1. The bottom of the crucible body 1 is heated by the heating module 1102, and the temperature is detected by the temperature sensor 203. If the temperature in the middle is higher than 650°C, Or when the temperature of the upper part is higher than 450°C, the first solenoid valve 207 and the second solenoid valve 210 can be opened, and the first liquid supply pump 206 can be started. At this time, the coolant in the first cooling box 205 can enter the arc cover 204 through the first liquid inlet pipe 208, and can return to the first cooling box 205 through the first liquid return pipe 209, the heat exchanger 211 and the connecting pipe 212, so that the coolant circulates, so that the middle or upper part can be cooled to ensure that the temperature is within the required range. After the cooling is completed, the first solenoid valve 207, the second solenoid valve 210 and the first liquid supply pump 206 can be closed, so as to facilitate the control of the temperature of the middle and upper parts of the crucible body 1, which is more convenient and quick to use, and ensures the efficiency and effect of the production of high-purity antimony powder;

[0062] Furthermore, when producing high-purity antimony powder, when condensing impurities such as arsenic with a lower boiling point, the fifth through hole 1003 is aligned with the fifth connecting pipe 309, the sixth through hole 1007 is staggered with the sixth connecting pipe 310, and the second liquid supply pump 312 is started, so that the coolant in the second cooling box 306 can enter the annular cover 304 through the second liquid inlet pipe 311 and the fifth connecting pipe 309, and return to the second cooling box 306 through the second liquid return pipe 308 for cooling. In this way, the annular cover 304 can be continuously cooled to ensure the efficiency and effect of its condensation. Moreover, when condensing antimony, when the first push plate 604 moves in a direction away from the second movable plate 302, the inclined plate 1010 can be driven to move through the L-shaped plate 1011 and the L-shaped block 1009, so that the inclined plate 1010 It abuts against the top of the first sliding plate 1002, thereby pushing the first sliding plate 1002 to move downward. At the same time, the third spring 1004 is compressed, so that the fifth through hole 1003 and the fifth connecting tube 309 are offset. At the same time, the pushing block 1013 is driven to move by the connecting rod 1012. When the pushing block 1013 is disengaged from the top of the second sliding plate 1006, the second sliding plate 1006 can move upward and reset under the action of the fourth spring 1008, so that the sixth through hole 1007 is aligned with the sixth connecting tube 310. At this time, the coolant can enter the conical cover 305 through the sixth connecting tube 310, and return to the second cooling box 306 through the second return liquid pipe 308, so that the area of ​​the conical titanium plate 14 above the second annular groove 21 can be continuously cooled to ensure the efficiency and effect of antimony condensation.

Claims

1. A production process for high-purity antimony powder, characterized in that: The following steps are involved: S1: Pre-set, pre-prepare high purity antimony powder production equipment; S2: feeding the crude antimony into the high-purity antimony powder production device; S3: Purification: After step S2, the high-purity antimony powder production device purifies the input crude antimony and collects the purified high-purity antimony powder; The high-purity antimony powder production device comprises a crucible body (1) and a vacuum box body (11), wherein the crucible body (1) comprises a crucible cover (101), the vacuum box body (11) comprises a box door (1101) and a heating module (1102) arranged at the bottom, and a fixed tube (12) is fixedly inserted at the top of the crucible cover (101), an exhaust pipe (25) is fixedly inserted at the side wall of the fixed tube (12), and a one-way valve is arranged in the exhaust pipe (25), the top of the crucible cover (101) is fixedly connected to a limit ring (13), and the side wall of the fixed tube (12) is sequentially sleeved with a conical titanium plate (14), a stainless steel cover (15) and a stainless steel sealing sleeve (16) from bottom to top, the side wall of the fixed tube (12) located inside the stainless steel sealing sleeve (16) is provided with a plurality of air holes (18) arranged in an array, and the top of the crucible cover (101) is provided with a plurality of first through holes (18) arranged in an array 17), and a first sealing mechanism for sealing the first through hole (17) is provided at the bottom of the crucible cover (101), a second sealing mechanism is provided in the fixed tube (12), and a first annular groove (19) is provided on the side wall of the stainless steel sealing sleeve (16), two semicircular collecting plates (20) are inserted in the first annular groove (19), and a U-shaped block (26) is fixedly connected to the side wall of the stainless steel sealing sleeve (16), a second annular groove (21) is provided on the inner side wall of the conical titanium plate (14), and a plurality of powder collecting holes (22) arranged in an array are provided at the bottom of the second annular groove (21), a third annular groove (23) is provided on the side wall of the conical titanium plate (14), and two arc-shaped collecting grooves (24) are inserted in the third annular groove (23), and a pulverizing mechanism for pulverizing the condensed high-purity antimony is provided in the second annular groove (21); The two opposite side walls of the vacuum box body (11) are both provided with a control mechanism for controlling the heating temperature of the crucible body (1), and the top of the vacuum box body (11) is provided with a cooling mechanism for cooling the conical titanium plate (14) and the stainless steel sealing sleeve (16); Each of the control mechanisms comprises a first movable plate (201), and the first movable plate (201) is connected to the inner wall of the vacuum box body (11) via a movable mechanism, a plurality of array-arranged insulating tubes (202) are fixedly inserted into the side wall of the first movable plate (201), and a temperature sensor (203) is arranged in each insulating tube (202), a hollow arc-shaped cover (204) is fixedly inserted into the side wall of the two insulating tubes (202) located at the top, and a first cooling box (205) is fixedly connected to the side wall of the vacuum box body (11), and two symmetrically arranged second cooling boxes (205) are fixedly connected to one side of the first cooling box (205). A liquid supply pump (206), and the other end of each first liquid supply pump (206) is fixedly connected to a first solenoid valve (207), a first liquid inlet pipe (208) is fixedly connected between the first solenoid valve (207) and the arc cover (204), and the other side of the first cooling box (205) is connected to two symmetrically arranged connecting pipes (212), the other end of each connecting pipe (212) is fixedly connected to a heat exchanger (211), the inlet of the heat exchanger (211) is fixedly connected to a second solenoid valve (210), and a first liquid return pipe (209) is fixedly connected between the second solenoid valve (210) and the arc cover (204).

2. The production process of high-purity antimony powder according to claim 1, characterized in that: The pulverizing mechanism comprises a rotating ring (704) rotatably connected to the inner wall of the second annular groove (21), and the side wall of the rotating ring (704) is fixedly connected to a plurality of connecting blocks (701) arranged in an array, the bottom of each connecting block (701) is connected to a U-shaped plate (702) via a lifting mechanism, and the side wall of the U-shaped plate (702) is rotatably connected to a rolling roller (708) via a rotating shaft (703), the outer wall of the conical titanium plate (14) is fixedly connected to a fixed block (706), and the top of the fixed block (706) is fixedly connected to a motor (707), the output end of the motor (707) is fixedly connected to a driving wheel (705), and the driving wheel (705) is inserted into the conical titanium plate (14) and abuts against the side wall of the rotating ring (704).

3. The production process of high-purity antimony powder according to claim 1, characterized in that: The cooling mechanism comprises a second movable plate (302), and the second movable plate (302) is connected to the top of the vacuum box body (11) through a lifting module (301), a hollow annular cover (304) and a hollow conical cover (305) are fixedly connected to the side wall of the second movable plate (302), and a second cooling box (306) is fixedly connected to the top of the vacuum box body (11), and a third connecting pipe (307) is fixedly connected to one side of the second cooling box (306), and the annular cover (304), the conical cover (305) and the third connecting pipe (307) are fixedly connected to the second cooling box (306). ), a second liquid return pipe (308) is fixedly connected between the annular cover (304) and the second liquid inlet pipe (311), a second liquid supply pump (312) is fixedly connected to the other side of the second cooling box (306), and the outlet of the second liquid supply pump (312) is fixedly connected to the second liquid inlet pipe (311), a fifth connecting pipe (309) is fixedly connected between the annular cover (304) and the second liquid inlet pipe (311), and a sixth connecting pipe (310) is fixedly connected between the annular cover (304) and the second liquid inlet pipe (311), and the side walls of the fifth connecting pipe (309) and the sixth connecting pipe (310) are provided with on-off mechanisms.

4. The production process of high-purity antimony powder according to claim 3, characterized in that: The first sealing mechanism comprises a first annular plate (403) arranged at the bottom of the crucible cover (101), and a plurality of second through holes (404) arranged in an array are opened at the bottom of the first annular plate (403), a connecting plate (402) is fixedly connected to the inner side wall of the first annular plate (403), and a moving rod (401) is fixedly connected to the top of the connecting plate (402), and the moving rod (401) is inserted into the fixed tube (12) and connected to the top of the fixed tube (12) through a moving component.

5. The production process of high-purity antimony powder according to claim 4, characterized in that: The second sealing mechanism comprises a second fixing ring (501) fixedly connected to the bottom of the fixing tube (12), and a plurality of third through holes (502) arranged in an array are provided on the top of the second fixing ring (501), and a fourth fixing ring (503) is provided on the side wall fixing sleeve of the moving rod (401), and a plurality of fourth through holes (504) arranged in an array are provided on the bottom of the fourth fixing ring (503).

6. The production process of high-purity antimony powder according to claim 4, characterized in that: The moving assembly comprises a circular ring (601) fixedly sleeved on the side wall of the moving rod (401), and a first spring (602) is fixedly connected between the circular ring (601) and the top of the fixed tube (12), and the side wall of the second moving plate (302) is connected to a first push plate (604) via a moving module (603), and the first push plate (604) comprises an inclined surface (605).

7. The production process of high-purity antimony powder according to claim 2, characterized in that: The lifting mechanism comprises two symmetrically arranged sliding rods (801) fixedly connected to the top of each U-shaped plate (702), and a stopper (802) is fixedly connected to the upper end of the sliding rod (801), a second spring (803) is sleeved on the side wall of each sliding rod (801), and a plurality of triangular blocks (804) arranged in an array are fixedly connected to the side wall of the second annular groove (21).

8. The production process of high-purity antimony powder according to claim 3, characterized in that: The on-off mechanism is fixedly inserted into a first fixed cover (1001) on the side wall of the fifth connecting tube (309), and a first sliding plate (1002) is slidably connected in the first fixed cover (1001), a fifth through hole (1003) is opened in the side wall of the first sliding plate (1002), and a third spring (1004) is fixedly connected between the first sliding plate (1002) and the first fixed cover (1001), a second fixed cover (1005) is fixedly inserted into the side wall of the sixth connecting tube (310), and a second sliding plate (1006) is inserted in the second fixed cover (1005), and the second sliding plate (1006) ) is provided with a sixth through hole (1007), and a fourth spring (1008) is fixedly connected between the second sliding plate (1006) and the second fixed cover (1005), the side wall of the second movable plate (302) is fixedly connected with an L-shaped plate (1011), and the top of the L-shaped plate (1011) is fixedly connected with an L-shaped block (1009), the side wall of the L-shaped block (1009) is fixedly connected with an inclined plate (1010), the side wall of the L-shaped plate (1011) is fixedly connected with a connecting rod (1012), and the other end of the connecting rod (1012) is fixedly connected with a pushing block (1013) arranged in a triangle.

9. The production process of high-purity antimony powder according to claim 1, characterized in that: The moving mechanism comprises two symmetrically arranged sleeve rods (904) fixedly connected to the inner side wall of the vacuum box body (11), and the side wall of the sleeve rod (904) is sleeved with a sleeve (905), the other end of the sleeve (905) is fixed to the side wall of the first moving plate (201), and the side wall of each sleeve (905) is sleeved with a fifth spring (906), the side wall of the first moving plate (201) is fixedly connected to a second push plate (907), and the top of the second push plate (907) is provided with an inclined groove (908), the inner side wall of the vacuum box body (11) is fixedly connected to a guide rail (901), and a moving block (902) is slidably connected to the guide rail (901), the top of the moving block (902) is fixedly connected to a push pin (909), and the push pin (909) is inserted into the inclined groove (908), and the side wall of the moving block (902) is fixedly connected to a push rod (903).

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