Vacuum distillation tube apparatus for high purity antimony

Abstract

The utility model relates to high -purity antimony processing equipment technical field, concretely is a kind of high -purity antimony vacuum distillation pipe device, including bushing, for guiding antimony steam to enter into tray inside;Tray, tray is provided with gas guide hole, grating, for condensing receiving material;Conical tube, conical tube is conical, for low boiling point impurity and a small amount of antimony condensation.The high -purity antimony vacuum distillation pipe device in this device, by setting 5-10 trays from top to bottom in bushing, and the gas guide hole of adjacent two layers of trays is cross arrangement, make steam present S type route movement.This design greatly increases the movement path and contact area of antimony steam in device, effectively controls steam flow state, avoids the phenomenon that antimony steam appears uneven distribution, over-condensation or condensation is not sufficient in condensation process, significantly improves the condensation efficiency and crystallization quality of high -purity antimony.

Description

Technical Field

[0001] This utility model relates to the technical field of high-purity antimony processing equipment, specifically, to a high-purity antimony vacuum distillation feed tube device. Background Technology

[0002] High-purity antimony plays an irreplaceable role in semiconductor manufacturing, infrared detection, and new energy batteries. In the semiconductor field, high-purity antimony serves as a core dopant, and its purity directly determines the performance of semiconductor devices. In infrared detection equipment, high-purity antimony-based materials can significantly improve the sensitivity and response speed of detectors. With the rapid development of emerging industries such as 5G communication and artificial intelligence, the market demand for high-purity antimony with a purity of 99.999% and above has increased dramatically, placing higher demands on its production processes and equipment.

[0003] Currently, vacuum distillation has become one of the mainstream technologies for high-purity antimony purification due to its advantages such as low energy consumption, low pollution, and good separation effect. This method utilizes the difference in saturated vapor pressure and volatilization rate between the main metal and impurities to achieve impurity separation through evaporation and condensation processes. For example, Chinese patent application number 202310378482.3 discloses a method and equipment for producing high-purity antimony. This technology involves heating the raw material antimony under vacuum to evaporate it. The antimony vapor enters the condensation chamber through a steam pipe and is then condensed and collected at the finished product outlet. Simultaneously, an aeration bubbling method is used to promote the circulation of the antimony liquid, improving the material exchange at the gas-liquid interface and thus enhancing the separation effect of impurities such as arsenic and lead from antimony.

[0004] However, this existing technology still has limitations. In actual production, its supporting receiving pipe device is insufficient in terms of condensation efficiency and impurity separation accuracy. The existing receiving pipe structure only guides antimony vapor into the condensation chamber through a simple steam pipe, lacking effective control over the steam flow pattern. This results in uneven distribution of antimony vapor in the condensation chamber, with some areas experiencing over-condensation or insufficient condensation, affecting the quality of high-purity antimony crystals. Simultaneously, the device lacks a dedicated condensation and separation structure for low-boiling-point impurities, making it easy for these impurities to mix into the high-purity antimony product during antimony vapor condensation, making it difficult to meet the production requirement of purity above 99.999%. Furthermore, the existing device uses a single heating method for temperature control, which cannot meet the precise temperature control requirements of different stages and regions in the vacuum distillation process, thus affecting the stability and production efficiency of the entire distillation process. Therefore, there is an urgent need to develop a new type of vacuum distillation receiving pipe device that can optimize the steam flow pattern, enhance impurity separation, and achieve precise temperature control to improve the production quality and efficiency of high-purity antimony. Utility Model Content

[0005] The purpose of this invention is to provide a high-purity antimony vacuum distillation feed pipe device to solve the problem mentioned in the background art that the existing feed pipe structure only guides antimony vapor into the condensation chamber through a simple steam pipe, lacks effective control of the steam flow state, resulting in uneven distribution of antimony vapor in the condensation chamber, and over-condensation or insufficient condensation in some areas, which affects the quality of high-purity antimony crystallization.

[0006] To achieve the above objectives, this utility model provides a high-purity antimony vacuum distillation feed tube device, including...

[0007] The sleeve is used to guide antimony vapor into the material tray;

[0008] The material tray is provided with air guide holes and a grid for receiving condensed material;

[0009] A conical tube, the conical tube being conical in shape, is used for the condensation of low-boiling-point impurities and small amounts of antimony.

[0010] This setup guides antimony vapor into the feed pan through a sleeve, and uses the air guide holes and grid in the feed pan to condense and collect the antimony vapor. At the same time, the conical tube specifically condenses low-boiling-point impurities, forming a three-stage separation structure.

[0011] Preferably, the number of the material trays is 5-10, arranged sequentially from top to bottom inside the sleeve.

[0012] This feature involves placing 5-10 trays from top to bottom inside the casing to form a multi-stage condensation zone.

[0013] Preferably, the sleeve, tray, and conical tube are installed inside the vacuum distillation chamber, and are equipped with two heating devices and two temperature measuring points on the outside.

[0014] This setup involves installing the sleeve, tray, and conical tube inside the vacuum distillation chamber, with two heating devices and two temperature measurement points externally configured.

[0015] Preferably, the material tray has ≥2 air guide holes, which are located within a semicircle on one side of the material tray, and the hole diameter is 10-30mm.

[0016] This setting requires the material tray to have ≥2 air guide holes, located within a semicircle on one side, with a hole diameter of 10-30mm.

[0017] Preferably, the grid of the material tray is located in the middle of the material tray, dividing the material tray into two semicircles, and the height of the grid is 5-15mm lower than the height of the side wall of the material tray.

[0018] This setting places the grid in the middle of the tray, dividing the tray into two semicircles, with its height 5-15mm lower than the side wall of the tray.

[0019] Preferably, the material trays are arranged in multiple layers from top to bottom, with each layer having a height of 5-10cm. The air guide holes of two adjacent material trays are arranged in an intersecting manner, so that the steam moves in an S-shaped path.

[0020] This design features a multi-layered tray with intersecting air guide holes, causing the steam to move in an S-shaped path.

[0021] Preferably, the tapered tube has a taper of 2-5° and a length of 15-30cm.

[0022] This design utilizes a conical structure to create a specific temperature gradient, causing low-boiling-point impurities to condense in a specific area, effectively separating them and improving product purity.

[0023] Preferably, the sleeve is connected to the crucible inside the vacuum distillation furnace, and the temperature of the sleeve and the material tray is controlled by heating in the medium-temperature section of the vacuum distillation furnace, while the temperature of the conical tube is controlled by heating in the low-temperature section of the vacuum distillation furnace.

[0024] In this configuration, the sleeve and the tray are heated in the medium-temperature section of the vacuum distillation furnace, while the conical tube is heated in the low-temperature section.

[0025] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0026] In this high-purity antimony vacuum distillation feed tube device, 5-10 feed trays are arranged from top to bottom inside the sleeve, with the gas guide holes of adjacent feed trays intersecting, causing the steam to move in an S-shaped path. This design greatly increases the movement path and contact area of ​​antimony vapor within the device, effectively controlling the vapor flow state and avoiding uneven distribution, over-condensation, or insufficient condensation of antimony vapor during the condensation process. This significantly improves the condensation efficiency and crystallization quality of high-purity antimony.

[0027] Enhanced impurity separation ensures product purity: The air guide holes and grids within the material tray, along with the special design of the conical tube, form a multi-stage impurity separation structure. The air guide holes and grids guide the orderly flow of antimony vapor within the material tray, promoting the condensation and collection of antimony, while also providing preliminary filtration of impurities. The conical tube, with its conical shape, is specifically designed for the condensation of low-boiling-point impurities and small amounts of antimony. Through its unique structural design, it effectively separates and collects low-boiling-point impurities, preventing them from contaminating the high-purity antimony product, thus meeting the production requirement of over 99.999% purity and ensuring the high purity of the product.

[0028] Precise temperature control ensures a stable distillation process: the temperature of the sleeve and tray is controlled by heating in the medium-temperature section of the vacuum distillation furnace, while the temperature of the conical tube is controlled by heating in the low-temperature section. The apparatus is also equipped with two external heating devices and two temperature measurement points. This zoned, precise temperature control allows for accurate adjustment based on the temperature requirements of different stages and regions during vacuum distillation, avoiding the drawbacks of single heating methods in existing technologies. This effectively improves the stability and controllability of the entire distillation process, ensuring efficient and stable purification of high-purity antimony.

[0029] Simplified production process and improved production efficiency: This device integrates the casing, material tray, and tapered tube into a single design. Compared to the simple steam pipe receiving structure in existing technologies, it eliminates the need for additional complex auxiliary equipment and operating procedures, reducing equipment investment and operational complexity. Simultaneously, through optimized structural design and precise temperature control, it shortens the production cycle, improves production efficiency, and reduces production costs, demonstrating significant economic benefits and promising application prospects. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0031] Figure 2 This is a top view of the material tray in this utility model.

[0032] Figure 3 This is a side view of the material tray structure in this utility model;

[0033] The meanings of the labels in the diagram are as follows:

[0034] 1. Sleeve; 2. Material tray; 21. Air guide hole; 22. Grating; 3. Conical tube. Detailed Implementation

[0035] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0036] This utility model provides a high-purity antimony vacuum distillation feed tube device, such as... Figure 1 , Figure 2 , Figure 3 As shown, it includes a sleeve 1 for guiding antimony vapor into the material tray 2;

[0037] Material tray 2, which is equipped with air guide holes 21 and grid 22 for receiving condensed material;

[0038] Conical tube 3, which is conical in shape, is used for condensing low-boiling-point impurities and small amounts of antimony.

[0039] Antimony vapor is guided into the feed pan 2 through the sleeve 1. The antimony vapor is condensed and collected using the air guide holes 21 and the grid 22 within the feed pan 2. Simultaneously, the conical tube 3 specifically condenses low-boiling-point impurities, forming a three-stage separation structure. The guiding effect of the sleeve 1 ensures the directional flow of antimony vapor. The combination of the air guide holes 21 and the grid 22 within the feed pan 2 promotes full contact between the vapor and the feed pan surface during condensation. The conical structure of the conical tube 3 utilizes the vapor pressure difference to achieve targeted condensation of impurities. These three elements work synergistically to improve the purity of high-purity antimony.

[0040] In this embodiment, as Figure 1 As shown, there are 5 to 10 material trays 2, which are arranged sequentially from top to bottom inside the sleeve 1.

[0041] Five to ten trays 2 are arranged from top to bottom inside the sleeve 1 to form a multi-level condensation zone, with each tray 2 serving as an independent condensation unit. The multi-level trays 2 segment the condensation path, extending the residence time of steam in the sleeve 1. By condensing layer by layer, the amount of impurities entrained in the antimony vapor is reduced, resulting in more uniform crystal particles and improving condensation efficiency by more than 40%.

[0042] Specifically, such as Figure 1 As shown, the sleeve 1, the material tray 2, and the conical tube 3 are installed inside the vacuum distillation chamber, and are equipped with two heating devices and two temperature measuring points on the outside.

[0043] The sleeve 1, tray 2, and conical tube 3 are integrated into the vacuum distillation chamber. Two external heating devices are configured to correspond to the medium-temperature section of sleeve 1 and tray 2, and the low-temperature section of conical tube 3, respectively. Two temperature measurement points monitor the temperature field in real time. Zoned temperature control maintains the temperature of sleeve 1 at 400-550℃, promoting stable antimony vapor flow, while conical tube 3 is maintained at 300-400℃ for precise condensation of low-boiling-point impurities. The temperature fluctuation range is ≤±5℃, which greatly improves the impurity separation efficiency compared to the existing single temperature control method.

[0044] Furthermore, such as Figure 2 , Figure 3 As shown, the material tray 2 has ≥2 air guide holes 21, which are located in the semicircle on one side of the material tray, and the hole diameter is 10-30mm.

[0045] The material tray 2 has at least two air guide holes 21, which are concentrated on one side of a semicircle, with a diameter of 10-30mm, forming an asymmetric ventilation structure. The asymmetric air guide holes 21 cause the steam to form a spiral upward airflow in the material tray 2, increasing the number of collisions between the steam and the grid 22 and the material tray wall, prompting impurities to condense in the turbulence in advance, and reducing the impurity content entering the next material tray.

[0046] Furthermore, such as Figure 2 , Figure 3 As shown, the grid 22 of the material tray 2 is located in the middle of the material tray 2, dividing the material tray 2 into two semicircles. The height of the grid 22 is 5-15mm lower than the height of the side wall of the material tray 2.

[0047] The grid 22 is located at the center of the material tray 2, dividing the tray into two semicircles. The height of the grid 22 is 5-15mm lower than the side wall of the material tray 2, forming a "semi-barrier" flow channel. The grid 22 forces the steam to circulate, forming an S-shaped flow trajectory within the material tray 2. At the same time, the condensed liquid antimony flows back to the bottom of the tray due to gravity along the grid 22, avoiding secondary evaporation and improving the antimony recovery rate.

[0048] Furthermore, such as Figure 2 , Figure 3 As shown, the material tray 2 is arranged in multiple layers from top to bottom, with a single layer height of 5-10cm. The air guide holes 21 of two adjacent material trays 2 are arranged in an intersecting manner, so that the steam moves in an S-shaped path.

[0049] The multi-layer feed tray 2 has a single layer height of 5-10cm. The air guide holes 21 of adjacent layers are arranged in a cross pattern, such as the upper layer's air guide hole being on the left semicircle and the lower layer's being on the right semicircle, forming a three-dimensional S-shaped steam channel. The cross air guide holes 21 extend the steam path to 2.5 times the straight-line distance, increasing the contact area between the steam and the feed tray 2. In the same distillation time, the amount of antimony condensed is increased compared to the traditional straight-discharge structure, and the impurity separation is more thorough.

[0050] Furthermore, the tapered tube has a taper of 2-5° and a length of 15-30cm.

[0051] The tapered tube 3 has a taper of 2-5° and a length of 15-30cm. The taper creates a gradual change in cross-section, which, combined with the low-temperature heating section, forms a temperature gradient. The tapered structure gradually increases the steam flow velocity. Low-boiling-point impurities preferentially condense on the inner wall of the tapered tube 3 due to their higher steam pressure, while antimony vapor continues to move towards the feed pan 2, achieving efficient separation of impurities and antimony and improving the removal rate of low-boiling-point impurities.

[0052] Furthermore, the sleeve 1 is connected to the charging crucible inside the vacuum distillation furnace, and the sleeve 1 and the material tray 2 are heated in the medium temperature section of the vacuum distillation furnace to achieve temperature control, while the conical tube 3 is heated in the low temperature section of the vacuum distillation furnace to achieve temperature control.

[0053] The sleeve 1 and the material tray 2 pass through a medium-temperature section (400-550℃) to maintain the fluidity of antimony vapor, while the conical tube 3 passes through a low-temperature section (300-400℃) to precisely control the condensation temperature of impurities. This segmented temperature control ensures that antimony vapor remains in a gaseous state within the sleeve 1 and material tray 2 area, while low-boiling-point impurities condense in the conical tube 3 area, preventing co-condensation of antimony and impurities. This results in the final product containing ≤5ppm of impurities such as arsenic and lead, meeting the requirements for high-purity antimony for semiconductor applications.

[0054] In use, the high-purity antimony vacuum distillation feed tube device of this invention first heats the raw antimony to a high temperature of 630-700℃ in the charging crucible inside the vacuum distillation furnace during the high-purity antimony vacuum distillation process, at which point the antimony becomes vapor. The generated antimony vapor is guided into the device through the sleeve 1 under the action of pressure difference, thus starting the purification process.

[0055] Antimony vapor first enters sleeve 1, which is connected to the charging crucible inside the vacuum distillation furnace. Its function is to provide a directional channel for the antimony vapor, ensuring that the vapor flows stably and orderly to the material tray 2. Sleeve 1 and material tray 2 are heated by the medium temperature section of the vacuum distillation furnace at 400-550℃. This temperature setting ensures that the antimony vapor does not condense prematurely during the flow process, maintaining its stable gaseous transmission.

[0056] Subsequently, antimony vapor enters 5-10 trays 2 arranged sequentially from top to bottom within the casing 1. The trays 2, as the core condensation and receiving components, feature an ingenious internal structure. Each semicircle on one side of the tray 2 has at least two vent holes 21 with a diameter of 10-30 mm. This asymmetrical structure causes the antimony vapor to form a spiral upward airflow upon entering the trays 2. A grid 22 located in the middle of the trays 2 divides the tray into two semicircles, and the height of the grid 22 is 5-15 mm lower than the side wall of the tray 2, forcing the vapor to circulate in an S-shaped flow trajectory. Simultaneously, the vent holes 21 of adjacent trays 2 are intersected, causing the vapor to move in a three-dimensional S-shaped path within the multi-layered trays 2. These designs significantly extend the antimony vapor's path by 2.5 times compared to a straight line, increasing the contact area between the vapor and the trays 2 by 60%. This ensures that the antimony vapor fully contacts the condensation surface within the trays 2, gradually condensing into a liquid and adhering to the trays 2, thus completing the collection of most of the high-purity antimony.

[0057] During the condensation of antimony vapor in the feed pan 2, some low-boiling-point impurities and a small amount of antimony vapor that has not condensed in time continue to move upwards and enter the conical tube 3. The conical tube 3 has a taper of 2-5° and a length of 15-30cm, and is heated by the low-temperature section of the vacuum distillation furnace. Its unique conical structure causes the internal space to gradually decrease, and the vapor flow velocity gradually increases, with the outlet velocity being 1.2 times higher than the inlet velocity. At the same time, a temperature gradient is formed due to the low temperature. Under these conditions, low-boiling-point impurities, due to their high vapor pressure, preferentially condense on the inner wall of the conical tube 3, while antimony vapor, due to its higher boiling point, continues to move towards the feed pan 2, thereby achieving efficient separation of low-boiling-point impurities and antimony vapor.

[0058] Throughout the process, two external heating devices and two temperature measurement points play a crucial role. The two heating devices precisely heat the sleeve 1 and the material tray 2, as well as the conical tube 3, respectively. The temperature measurement points monitor the temperature field in real time, ensuring that the temperature fluctuation range is ≤±5℃. This zoned temperature control method ensures that antimony vapor maintains gaseous flow in the sleeve 1 and material tray 2 areas for smooth condensation, while low-boiling-point impurities are precisely condensed in the conical tube 3 area, avoiding co-condensation of antimony and impurities. Ultimately, the product contains ≤5ppm of impurities such as arsenic and lead, producing high-purity antimony that meets semiconductor-grade standards.

[0059] After the distillation process is completed, heating is stopped, and the apparatus is allowed to cool to room temperature. High-purity argon gas is then introduced into the vacuum distillation furnace, the furnace lid is opened, and the conical tube 3, the material tray 2, and the sleeve 1 are removed in sequence. At this time, the material collected on the material tray 2 is high-purity antimony, while the material containing impurities adhering to the conical tube 3 and other components is returned to the head and tail materials for comprehensive recycling.

[0060] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. A high-purity antimony vacuum distillation feed tube device, characterized in that: include The sleeve (1) is used to guide antimony vapor into the material tray (2); The material tray (2) is provided with air guide holes (21) and grids (22) for receiving condensed material; The conical tube (3) is conical in shape and is used for the condensation of low-boiling-point impurities and a small amount of antimony.

2. The high-purity antimony vacuum distillation feed tube device according to claim 1, characterized in that: The number of the material trays (2) is 5-10, which are arranged in the sleeve (1) from top to bottom.

3. The high-purity antimony vacuum distillation feed tube device according to claim 1, characterized in that: The sleeve (1), the tray (2), and the conical tube (3) are installed inside the vacuum distillation chamber, and are equipped with two heating devices and two temperature measuring points on the outside.

4. The high-purity antimony vacuum distillation feed tube device according to claim 1, characterized in that: The material tray (2) is provided with ≥2 air guide holes (21), which are located in the semicircle on one side of the material tray, and the hole diameter is 10-30mm.

5. The high-purity antimony vacuum distillation feed tube device according to claim 1, characterized in that: The grid (22) of the material tray (2) is located in the middle of the material tray (2), dividing the material tray (2) into two semicircles. The height of the grid (22) is 5-15mm lower than the height of the side wall of the material tray (2).

6. The high-purity antimony vacuum distillation feed tube apparatus according to claim 1, characterized in that: The material tray (2) is arranged in multiple layers from top to bottom, with a single layer height of 5-10cm. The air guide holes (21) of the two adjacent material trays (2) are arranged in an intersecting manner, so that the steam moves in an S-shaped path.

7. The high-purity antimony vacuum distillation feed tube apparatus according to claim 1, characterized in that: The tapered tube (3) has a taper of 2-5° and a length of 15-30cm.

8. The high-purity antimony vacuum distillation feed tube apparatus according to claim 1, characterized in that: The sleeve (1) is connected to the crucible inside the vacuum distillation furnace. The sleeve (1) and the material tray (2) are heated in the medium temperature section of the vacuum distillation furnace to achieve temperature control. The conical tube (3) is heated in the low temperature section of the vacuum distillation furnace to achieve temperature control.

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