Preparation device for producing high-purity selenium and preparation method thereof

CN116672739BActive Publication Date: 2026-09-11WUHAN TUOCAI TECH CO LTD
View PDF 3 Cites 0 Cited by

Patent Information

Application Number
CN202310793666.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-29
Publication Date
2026-09-11
Estimated Expiration
2043-06-29

AI Technical Summary

Technical Problem

[0004]为了克服现有技术的上述缺陷,本发明提供了一种高纯硒生产用制备装置及其制备方法,目的在于解决现有技术中还原和蒸馏进行分开操作,所以需要使用到两个设备,并且经还原完成之后需要再将其转移到蒸馏的设备内部,操作较为不便,且成本较高,而且目前氧化硒还原过程一般只是简单的通入二氧化硫,导致还原效果较差,并且在蒸馏的过程中一般采用底部加热的方式进行蒸馏,使得加热均匀度较低等问题

Benefits of technology

[0019]This invention uses a drive component to drive the connecting cylinder to rotate the chamber shell. This rotation of the chamber shell agitates the material for mixing. Furthermore, the hollow connecting cylinder facilitates the transport of sulfur dioxide, guiding it through the nozzles during the chamber's rotation. This ensures the sulfur dioxide is effectively distributed to all parts of the material, resulting in better reduction and reduced reduction time. Additionally, the convex panel and flow-guiding structure intermittently and evenly deliver the material to the heating plate, ensuring dispersed flow and uniform heating. This allows for automatic, multiple-stage heating in small batches, improving distillation efficiency. The device integrates reduction, stirring, distillation, and condensation into a single operation, offering convenient operation and low cost.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN116672739B_ABST
    Figure CN116672739B_ABST
Patent Text Reader

Abstract

This invention discloses a preparation device and method for high-purity selenium production, specifically relating to the field of high-purity selenium production technology. The invention uses a drive component to drive a connecting cylinder, which rotates the chamber shell. This rotation agitates the material for mixing. Furthermore, the hollow connecting cylinder facilitates the transport of sulfur dioxide, guiding it through a nozzle during the chamber's rotation. This ensures the nozzle effectively distributes sulfur dioxide to all parts of the material, resulting in better reduction and reduced reduction time. Additionally, the convex panel and guiding structure intermittently and evenly transport the material to the heating plate, ensuring dispersed flow and uniform heating. This enables automatic, multiple-stage heating in small batches, improving distillation efficiency. The device integrates reduction, stirring, distillation, and condensation into a single operation, offering convenient operation and low cost.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of high-purity selenium production technology, and more specifically, to a preparation apparatus and method for high-purity selenium production. Background Technology

[0002] Selenium is an important semiconductor material. High-purity selenium is mainly used in the electronics and medical fields, such as semiconductor devices, optoelectronic and thermoelectric devices, selenium-containing solar cells, laser devices, laser and infrared photoconductor materials, etc. With the increasing purity requirements of various selenium-containing materials and the increasing types of impurities to be controlled, the purity requirements of high-purity selenium are becoming higher and higher.

[0003] The reduction of selenium oxide (or selenite) with sulfur dioxide to prepare high-purity selenium is one of the more convenient methods. This process can be carried out by reducing selenium to obtain elemental selenium, and then distilling the fraction to obtain high-purity selenium. However, the reduction and distillation are often carried out separately, so two devices are required. After the reduction is completed, the selenium needs to be transferred to the distillation equipment, which is inconvenient and costly. Moreover, the current selenium oxide reduction process generally only involves simply introducing sulfur dioxide, resulting in poor reduction effect. Furthermore, the distillation process generally uses bottom heating, which results in low heating uniformity. Therefore, it is of great significance to study a new preparation device and method for high-purity selenium production to solve the above problems. Summary of the Invention

[0004] To overcome the aforementioned deficiencies of the prior art, this invention provides a preparation apparatus and method for producing high-purity selenium. The purpose is to solve the problems in the prior art where reduction and distillation are performed separately, requiring the use of two separate devices. After reduction, the selenium needs to be transferred to the distillation apparatus, which is inconvenient and costly. Furthermore, the current selenium oxide reduction process generally involves simply introducing sulfur dioxide, resulting in poor reduction efficiency. Additionally, the distillation process typically uses bottom heating, leading to low heating uniformity.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a preparation device for high-purity selenium production, comprising a base plate and a circular plate, wherein a condensation component is fixedly installed on the upper left side of the base plate, a box is provided on the right side of the condensation component, the upper side of the box is connected to one end of the condensation component, a connecting cylinder is provided in the box, a sulfur supply component is connected to the top of the connecting cylinder, the sulfur supply component is fixedly installed on the right side of the top of the box, a driving component is connected above the connecting cylinder, the driving component is fixedly installed on the top of the box, the connecting cylinder is divided into upper and lower cavities, multiple cavity shells are installed on the outside of the connecting cylinder, multiple nozzles are installed on each of the multiple cavity shells, and the multiple cavity shells are connected to the upper cavity;

[0006] Multiple drainage pipes are installed on the outside of the connecting cylinder, and these drainage pipes communicate with the cavity below. A drainage structure is provided in the cavity below, and a connecting rod is fixedly installed on the top of the drainage structure. Rollers are fixedly connected to both sides of the connecting rod, and a convex panel slides on the top of the two rollers. The convex panel is fixedly connected to the bottom of a circular plate, and a solenoid valve is installed on the circular plate. The circular plate is fixedly connected to the inner wall of the box, and a heating plate is installed in the inner cavity of the box. The heating plate is sleeved on the outside of the connecting cylinder.

[0007] As a further aspect of the present invention: a plurality of support rods are fixedly connected to the bottom of the box body, the plurality of support rods are fixedly connected to the top of the base plate, a feed hopper is installed on the top of the box body, and a vacuum head is provided on the top of the box body and behind the feed hopper.

[0008] As a further aspect of the present invention: the condensation assembly includes a collection box, which is fixedly installed on the top of the base plate, and a condenser is connected to the top of the collection box, with the top of the condenser connected to the upper side of the box body.

[0009] As a further aspect of the present invention: the drive assembly includes a motor, a fixing plate is fixedly connected to one side of the motor, the fixing plate is fixedly installed on the top of the housing, a first gear is fixedly connected to the output shaft of the motor, a second gear is meshed on the right side of the first gear, and the second gear is installed outside the connecting cylinder.

[0010] As a further aspect of the present invention: the sulfur supply assembly includes a sulfur supply device, which is fixedly installed on the top of the housing. A connecting pipe is connected to one side of the sulfur supply device, and the connecting pipe is connected to the cavity above. Four first bearings are rotatably connected to the connecting cylinder, two of which are installed on the upper and lower sides of the housing, and the other two are installed on the connecting pipe and the circular plate.

[0011] As a further aspect of the present invention: multiple blades and triangular pieces are fixedly connected to the outside of the connecting cylinder, the blades and triangular pieces are staggered, multiple liquid outlets are opened on the outside of the connecting cylinder, the multiple liquid outlets are connected to the cavity below, two openings are opened on the connecting cylinder, and the roller passes through the openings.

[0012] As a further embodiment of the present invention: the drainage structure includes a piston, on which a plurality of one-way valves are provided, the piston is sealed and slides in the lower cavity, the upper part of the piston is fixedly connected to a connecting rod, the liquid outlet is located above the piston, and a spring is fixedly connected to the lower part of the piston, the bottom end of the spring being fixedly connected to the bottom wall of the lower cavity.

[0013] A method for preparing high-purity selenium for production includes the following steps:

[0014] S1. When preparing high-purity selenium, first add selenite solution through the feed hopper, then close the feed hopper, and connect the vacuum pump to the vacuum head to evacuate the upper cavity of the chamber. Then control the sulfur supply device to operate, so that the sulfur supply device inputs sulfur dioxide into the upper cavity through the connecting pipe and enters the chamber shell, so that the sulfur dioxide is sprayed out through the nozzle to reduce the material. Then disconnect the vacuum pump, and connect the vacuum head to the feed pipe to transport the solution.

[0015] S2. Then control the motor to drive the first gear to rotate, so that the first gear drives the second gear to rotate, so that the second gear drives the connecting cylinder to rotate, and the connecting cylinder drives the cavity shell to rotate, so that the cavity shell stirs the material to react fully, and the nozzle continuously sprays sulfur dioxide for uniform reduction.

[0016] S3. After sufficient reaction, open the solenoid valve to discharge the material into the lower chamber of the box. Due to the rotation of the connecting cylinder, the connecting cylinder drives the triangular plate and blades to continuously stir the material. The connecting cylinder drives the roller to rotate through the opening, so that the roller rolls on the convex plate. When the roller contacts the convex surface of the convex plate, the convex plate squeezes the roller downward, which pushes the connecting rod downward. The connecting rod pushes the piston downward to compress the spring deformation, so that the one-way valve is kept open under pressure, allowing the material to enter the upper part of the piston. When the roller moves away from the convex surface of the convex plate, the spring force pushes the piston upward to reset, which closes the one-way valve, opens the drainage pipe, and introduces the material into the lower part of the piston. At the same time, the piston pushes the material out through the liquid outlet until the roller contacts the convex surface of the convex plate again, causing the piston to move downward again. In this way, the convex plate, together with the spring, drives the piston to move up and down repeatedly, and intermittently discharges the material into the upper part of the heating plate.

[0017] S4. The material flows intermittently on the heating plate, which keeps the heating plate heating the material. This causes the material heating steam to flow upward, so that when the steam enters the condenser, it can be quickly condensed into a solution, and the solution enters the collection box for collection.

[0018] The beneficial effects of this invention are as follows:

[0019] This invention uses a drive component to drive the connecting cylinder to rotate the chamber shell. This rotation of the chamber shell agitates the material for mixing. Furthermore, the hollow connecting cylinder facilitates the transport of sulfur dioxide, guiding it through the nozzles during the chamber's rotation. This ensures the sulfur dioxide is effectively distributed to all parts of the material, resulting in better reduction and reduced reduction time. Additionally, the convex panel and flow-guiding structure intermittently and evenly deliver the material to the heating plate, ensuring dispersed flow and uniform heating. This allows for automatic, multiple-stage heating in small batches, improving distillation efficiency. The device integrates reduction, stirring, distillation, and condensation into a single operation, offering convenient operation and low cost. Attached Figure Description

[0020] Figure 1 This is a three-dimensional structural schematic diagram of the present invention;

[0021] Figure 2 This is a three-dimensional cross-sectional structural diagram of the present invention;

[0022] Figure 3 This is a three-dimensional structural diagram of the cavity shell of the present invention;

[0023] Figure 4 This is a three-dimensional cross-sectional structural diagram of the connecting cylinder of the present invention;

[0024] Figure 5 This is a three-dimensional structural diagram of the drainage structure of the present invention;

[0025] Figure 6 This is a three-dimensional structural schematic diagram of the heating plate of the present invention;

[0026] In the diagram: 1. Base plate; 2. Box body; 3. Condensation assembly; 31. Collection box; 32. Condenser; 4. Support rod; 5. Feed hopper; 6. Drive assembly; 61. First gear; 62. Motor; 63. Fixing plate; 64. Second gear; 7. Drainage structure; 71. Piston; 72. One-way valve; 73. Spring; 8. First bearing; 9. Sulfur supply assembly; 91. Connecting pipe; 92. Sulfur supply device; 93. Second bearing; 10. Connecting cylinder; 11. Drainage pipe; 12. Nozzle; 13. Vacuum head; 14. Roller; 15. Connecting rod; 16. Convex panel; 17. Liquid outlet; 18. Blade; 19. Triangular plate; 20. Heating plate; 21. Solenoid valve; 22. Circular plate; 23. Cavity shell. Detailed Implementation

[0027] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0028] In the embodiments of the present invention, the underlying principle is as follows:

[0029] Sulfur dioxide, as a reducing agent, can reduce selenite to precipitate elemental selenium. The product is then transferred and selectively extracted by distillation. High-purity selenium is obtained by taking the product with a high boiling point (above 680℃).

[0030] according to Figure 1-4As shown, in one embodiment, a preparation apparatus for producing high-purity selenium is provided, including a base plate 1 and a circular plate 22. A condensation assembly 3 is fixedly installed on the upper left side of the base plate 1, and a housing 2 is provided on the right side of the condensation assembly 3. Multiple support rods 4 are fixedly connected to the bottom of the housing 2 and are fixedly connected to the upper part of the base plate 1. A feed hopper 5 is installed on the upper part of the housing 2. The feed hopper 5 facilitates the feeding of materials into the housing 2, and the feed hopper 5 can be sealed by a sealing element to maintain the airtightness of the housing 2. A vacuum valve is provided on the upper part of the housing 2 and behind the feed hopper 5. The vacuum head 13 can be connected to a vacuum pump to evacuate the housing 2 to a vacuum state. It can also be connected to a conveying pipe to facilitate the mixing of materials with those inside the housing 2. The upper side of the housing 2 is connected to one end of the condensation assembly 3. A connecting cylinder 10 is provided inside the housing 2, and the top of the connecting cylinder 10 is connected to a sulfur supply assembly 9. The sulfur supply assembly 9 includes a sulfur feeder 92, which is fixedly installed on the top of the housing 2. A connecting pipe 91 is connected to one side of the sulfur feeder 92, and the connecting pipe 91 communicates with the upper cavity. Four first bearings 8 are rotatably connected to the cylinder 10. Two of the first bearings 8 are installed on the upper and lower sides of the housing 2, and the other two are installed on the connecting pipe 91 and the circular plate 22. The first bearings 8 can support the connecting cylinder 10, maintain the stability of the connecting cylinder 10, and allow the connecting cylinder 10 to rotate smoothly within the first bearings 8. The sulfur supply assembly 9 is fixedly installed on the right side of the top of the housing 2. A drive assembly 6 is connected above the connecting cylinder 10 and is fixedly installed on the top of the housing 2. The drive assembly 6 includes a motor 62 and an electric motor 63. A fixing plate 63 is fixedly connected to one side of the motor 62. The fixing plate 63 can fix the motor 62, so that the stability of the motor 62 is guaranteed. The fixing plate 63 is fixedly installed on the top of the housing 2. The output shaft of the motor 62 is fixedly connected to the first gear 61. The right side of the first gear 61 is meshed with the second gear 64. The second gear 64 is installed on the outside of the connecting cylinder 10. The connecting cylinder 10 is divided into upper and lower cavities. Multiple cavity shells 23 are installed on the outside of the connecting cylinder 10. Multiple nozzles 12 are installed on each of the multiple cavity shells 23, and the multiple cavity shells 23 are connected to the upper cavity.

[0031] A flow-guiding structure 7 is provided in the lower cavity. A connecting rod 15 is fixedly installed on the top of the flow-guiding structure 7. Rollers 14 are fixedly connected to both sides of the connecting rod 15. The rollers 14 have good rolling properties, which reduces the friction between the rollers 14 and the convex plate 16, allowing the rollers 14 to move smoothly and making the operation smoother. The convex plate 16 slides in contact with the top of the two rollers 14. The convex plate 16 is fixedly connected to the bottom of the circular plate 22. A solenoid valve 21 is installed on the circular plate 22. When the solenoid valve 21 is opened, the material after the reduction reaction can be discharged into the lower cavity of the box 2 for distillation. The circular plate 22 is fixedly connected to the inner wall of the box 2. The circular plate 22 can separate the box 2, allowing the upper cavity of the box 2 to perform reduction and mixing operations, while the lower cavity of the box 2 can smoothly carry out distillation operations, maintaining the separation of reduction and distillation operations. A heating plate 20 is installed in the inner cavity of the box 2. The heating plate 20 can heat and evaporate materials. The outer periphery of the heating plate 20 has a notch, which allows the material to enter the lower cavity of the box 2 smoothly. This maintains the convection of materials from top to bottom, improves heating uniformity, and facilitates heating and evaporating materials in small batches. The heating plate 20 is sleeved on the outside of the connecting cylinder 10. Multiple blades 18 and triangular pieces 19 are fixedly connected to the outside of the connecting cylinder 10. The blades 18 and triangular pieces 19 are staggered. The staggered arrangement of the blades 18 and triangular pieces 19 can stir the material at different positions to flow, which can maintain the uniformity of the material and facilitate the uniform heating of the material. Multiple liquid outlets 17 are opened on the outside of the connecting cylinder 10. The multiple liquid outlets 17 are connected to the cavity below. Two openings are opened on the connecting cylinder 10, and the roller 14 passes through the openings. The openings can provide a moving point for the roller 14, so that the roller 14 can be smoothly connected to the connecting rod 15 and maintain the smooth up and down sliding of the roller 14.

[0032] In practical use, the motor 62 drives the first gear 61 to rotate, which in turn drives the second gear 64 to rotate. This power transmission drives the connecting cylinder 10 to rotate, which in turn drives the cavity shell 23 to rotate. The cavity shell 23 then drives the nozzle 12 to rotate, allowing the cavity shell 23 to stir and mix the material, maintaining a uniform mixture. Meanwhile, the sulfur supply unit 92 delivers sulfur dioxide into the connecting cylinder 10 through the connecting pipe 91, causing the sulfur dioxide to be sprayed out through the nozzle 12. The rotation of the nozzle 12 ensures that the sulfur dioxide is evenly distributed to all parts of the material, accelerating the reduction reaction and saving reduction time. This allows the stirring and reduction operations to be carried out simultaneously without the need for other driving equipment, which not only reduces costs but also simplifies operation.

[0033] Based on the above embodiments, such as Figure 1 , Figure 3 and Figure 5As shown, the flow-guiding structure 7 includes a piston 71, through which multiple one-way valves 72 are installed. The one-way valves 72 can keep the material flowing upward in one direction and prevent the material from flowing back downward. The piston 71 slides in a sealed manner in the lower cavity. The upper part of the piston 71 is fixedly connected to the connecting rod 15. The liquid outlet 17 is located above the piston 71. A spring 73 is fixedly connected to the lower part of the piston 71. The bottom end of the spring 73 is fixedly connected to the bottom wall of the lower cavity. Multiple flow-guiding pipes 11 are installed on the outside of the connecting cylinder 10. The flow-guiding pipes 11 are one-way liquid inlet pipes to prevent the material from flowing back outward. When the piston 71 moves downward, it maintains a seal so that the pressure can open the one-way valves 72, and the material can be smoothly guided to the upper part of the piston 71. The multiple flow-guiding pipes 11 are connected to the lower cavity.

[0034] The condenser assembly 3 includes a collection box 31, which is fixedly installed on the top of the base plate 1. A condenser 32 is connected to the top of the collection box 31, and the top of the condenser 32 is connected to the upper side of the box body 2.

[0035] In practical use, the present invention drives the roller 14 to rotate through the connecting cylinder 10, causing the roller 14 to be squeezed by the convex surface of the convex plate 16, which in turn compresses the piston 71 downward and the spring 73, while keeping the one-way valve 72 open, allowing material to enter the piston 71. When the roller 14 separates from the convex surface of the convex plate 16, the spring 73 pushes the piston 71 upward, forcing the material out through the discharge port. The material can also be introduced into the connecting cylinder 10 through the guide pipe 11. This allows the convex plate 16, in conjunction with the spring 73, to intermittently discharge material from bottom to top, allowing the material to flow along the heating plate 20. The material is dispersed and thinly dispersed on the heating plate 20, ensuring uniform heating. Evaporation can be performed quickly through multiple small-batch heating. After reduction, the material can be directly distilled. The condenser 32 liquefies and condenses the vapor, allowing the liquefied components to be collected in the collection box 31. This integrated device performs reduction, distillation, and condensation, simplifying operation, eliminating the need to transfer materials, and using a motor 62 as the drive source eliminates the need for additional drive equipment, thus reducing costs.

[0036] In the above embodiments, based on common knowledge in the art, the components of the device are made of high-temperature resistant materials, such as ceramics.

[0037] A method for preparing high-purity selenium for production includes the following steps:

[0038] S1. In the preparation of high-purity selenium, firstly, a 150g / L concentration of selenite solution is added through feed hopper 5, then feed hopper 5 is closed, and the upper chamber of housing 2 is evacuated by connecting a vacuum pump to vacuum head 13. At this time, the sulfur supply device 92 is controlled to operate, and the flow rate of sulfur dioxide is controlled to be 40-45m³.3 / h, so that the sulfur feeder 92 inputs sulfur dioxide into the upper cavity through the connecting pipe 91 and enters the cavity shell 23, so that the sulfur dioxide is sprayed out through the nozzle 12 to reduce the material, and the vacuum pump is removed, and then the vacuum head 13 is connected to the feed pipe to transport the solution.

[0039] S2. Then control the motor 62 to drive the first gear 61 to rotate, so that the first gear 61 drives the second gear 64 to rotate, so that the second gear 64 drives the connecting cylinder 10 to rotate, and the connecting cylinder 10 drives the cavity shell 23 to rotate, so that the cavity shell 23 stirs the material to react fully, and the nozzle 12 continuously sprays sulfur dioxide to carry out uniform reduction.

[0040] S3. After sufficient reaction, open solenoid valve 21 to discharge material into the lower cavity of housing 2. Due to the rotation of connecting cylinder 10, connecting cylinder 10 drives triangular plate 19 and blade 18 to continuously stir the material. Connecting cylinder 10 drives roller 14 to rotate through the opening, causing roller 14 to roll on convex plate 16. When roller 14 contacts the convex surface of convex plate 16, convex plate 16 squeezes roller 14 downward, causing roller 14 to push connecting rod 15 downward. Connecting rod 15 pushes piston 71 downward to compress spring 73, causing one-way valve 72 to... The pressure keeps the piston 71 open, allowing material to enter above the piston 71. When the roller 14 moves away from the convex surface of the convex plate 16, the spring 73 pushes the piston 71 upward to reset, causing the one-way valve 72 to close, the drain pipe 11 to open, and the material to be introduced below the piston 71. At the same time, the piston 71 pushes the material out through the outlet 17 until the roller 14 contacts the convex surface of the convex plate 16 again, causing the piston 71 to move downward again. This causes the convex plate 16, in conjunction with the spring 73, to drive the piston 71 to move up and down repeatedly, intermittently discharging the material into the top of the heating plate 20.

[0041] S4. The material flows intermittently on the heating plate 20, which keeps the heating plate 20 heating the material. The material heating steam flows upward, and when the steam enters the condenser 32, it can be quickly condensed into a solution. The solution enters the collection box 31 for collection. The collection box 31 collects the fraction above 700℃ to obtain high-purity selenium.

[0042] In the above preparation embodiments, in order to improve the reduction efficiency, the reduction temperature can be set to 60-80°C. Specifically, those skilled in the art can set a heating element in the cavity of the reduction reaction, or place the entire device in a temperature control box.

[0043] In the above preparation examples, during distillation, water, a small amount of selenite, and other low-boiling impurities are discharged first, and the fraction collected at temperatures above 700°C yields high-purity selenium (5N or higher).

[0044] Finally, the following points should be noted: First, in the description of this application, it should be noted that, unless otherwise specified and limited, the terms "installation", "connection", and "linkage" should be interpreted broadly, and can be mechanical or electrical connections, or internal connections between two components, or direct connections. "Up", "down", "left", "right", etc. are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may change.

[0045] Secondly: The accompanying drawings of the embodiments disclosed in this invention only involve the structures involved in the embodiments disclosed in this invention. Other structures can refer to the general design. In the absence of conflict, the same embodiment and different embodiments of this invention can be combined with each other.

[0046] In conclusion, the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A preparation apparatus for producing high-purity selenium, comprising a base plate (1) and a circular plate (22), characterized in that: A condensing component (3) is fixedly installed on the upper left side of the base plate (1). A box (2) is provided on the right side of the condensing component (3). The upper side of the box (2) is connected to one end of the condensing component (3). A connecting cylinder (10) is provided in the box (2). A sulfur supply component (9) is connected to the top of the connecting cylinder (10). The sulfur supply component (9) is fixedly installed on the right side of the top of the box (2). A driving component (6) is connected above the connecting cylinder (10). The driving component (6) is fixedly installed on the top of the box (2). The connecting cylinder (10) is divided into upper and lower cavities. Multiple cavity shells (23) are installed on the outside of the connecting cylinder (10). Multiple nozzles (12) are installed on each of the multiple cavity shells (23), and the multiple cavity shells (23) are connected to the upper cavity. Multiple drainage pipes (11) are installed on the outside of the connecting cylinder (10), and the multiple drainage pipes (11) are connected to the cavity below. A drainage structure (7) is provided in the cavity below. A connecting rod (15) is fixedly installed on the top of the drainage structure (7). Rollers (14) are fixedly connected to both sides of the connecting rod (15). A convex panel (16) slides on the top of the two rollers (14). The convex panel (16) is fixedly connected to the bottom of the circular plate (22). A solenoid valve (21) is installed on the circular plate (22). The circular plate (22) is fixedly connected to the inner wall of the box (2). A heating plate (20) is installed in the inner cavity of the box (2). A notch is provided on the outer periphery of the heating plate (20). The heating plate (20) is sleeved on the outside of the connecting cylinder (10). The connecting cylinder (10) has multiple liquid outlets (17) on its outside, and the multiple liquid outlets (17) are connected to the cavity below; The convex panel (16) works in conjunction with the flow-guiding structure (7) to intermittently and evenly convey the material to the heating plate.

2. The preparation apparatus for high-purity selenium production according to claim 1, characterized in that: The bottom of the box (2) is fixedly connected to multiple support rods (4), which are fixedly connected to the top of the base plate (1). A feeding hopper (5) is installed on the top of the box (2), and a vacuum head (13) is provided on the top of the box (2) and behind the feeding hopper (5).

3. The preparation apparatus for producing high-purity selenium according to claim 1, characterized in that: The condensation assembly (3) includes a collection box (31), which is fixedly installed on the top of the base plate (1). A condenser (32) is connected to the top of the collection box (31), and the top of the condenser (32) is connected to the upper side of the box body (2).

4. The preparation apparatus for producing high-purity selenium according to claim 1, characterized in that: The drive assembly (6) includes a motor (62), a fixing plate (63) is fixedly connected to one side of the motor (62), the fixing plate (63) is fixedly installed on the top of the housing (2), the output shaft of the motor (62) is fixedly connected to a first gear (61), a second gear (64) is meshed on the right side of the first gear (61), and the second gear (64) is installed outside the connecting cylinder (10).

5. The preparation apparatus for high-purity selenium production according to claim 1, characterized in that: The sulfur supply assembly (9) includes a sulfur supply device (92), which is fixedly installed on the top of the housing (2). A connecting pipe (91) is connected to one side of the sulfur supply device (92), and the connecting pipe (91) is connected to the cavity above. Four first bearings (8) are rotatably connected to the connecting cylinder (10), two of which are installed on the upper and lower sides of the housing (2), and the other two are installed on the connecting pipe (91) and the circular plate (22).

6. The preparation apparatus for producing high-purity selenium according to claim 1, characterized in that: The connecting cylinder (10) is fixedly connected to a plurality of blades (18) and triangular pieces (19), which are staggered. The connecting cylinder (10) has two openings, and the roller (14) passes through the openings.

7. The preparation apparatus for producing high-purity selenium according to claim 6, characterized in that: The drainage structure (7) includes a piston (71), on which multiple one-way valves (72) are provided. The piston (71) slides in a sealed manner in the lower cavity. The upper part of the piston (71) is fixedly connected to the connecting rod (15). The liquid outlet (17) is located above the piston (71). A spring (73) is fixedly connected to the lower part of the piston (71). The bottom end of the spring (73) is fixedly connected to the bottom wall of the lower cavity.

8. A method for preparing high-purity selenium for production, comprising a preparation apparatus for high-purity selenium for production according to any one of claims 1-7, characterized in that, Includes the following steps: S1. When preparing high-purity selenium, first add selenite solution through the feed hopper (5), then close the feed hopper (5), and connect the vacuum pump to the vacuum head (13) to evacuate the upper cavity of the box (2). Then control the sulfur supply device (92) to operate, so that the sulfur supply device (92) inputs sulfur dioxide into the upper cavity through the connecting pipe (91) and enters the cavity shell (23), so that the sulfur dioxide is sprayed out through the nozzle (12) to reduce the material. Then remove the vacuum pump and connect the vacuum head (13) to the feed pipe to transport the solution. S2. Then control the motor (62) to drive the first gear (61) to rotate, so that the first gear (61) drives the second gear (64) to rotate, so that the second gear (64) drives the connecting cylinder (10) to rotate, and the connecting cylinder (10) drives the cavity shell (23) to rotate, so that the cavity shell (23) stirs the material to react fully, and the nozzle (12) continuously sprays sulfur dioxide to carry out uniform reduction operation. S3. After sufficient reaction, open the solenoid valve (21) to discharge the material into the lower chamber of the box (2). Due to the rotation of the connecting cylinder (10), the connecting cylinder (10) drives the triangular piece (19) and the blade (18) to continuously stir the material. The connecting cylinder (10) drives the roller (14) to rotate through the opening, so that the roller (14) rolls on the convex plate (16). When the roller (14) contacts the convex surface of the convex plate (16), the convex plate (16) squeezes the roller (14) downward, so that the roller (14) pushes the connecting rod (15) downward, so that the connecting rod (15) pushes the piston (71) downward to compress the spring (73) and deform it, so that the one-way valve ( 72) The pressure keeps the valve open, allowing the material to enter the upper part of the piston (71). When the roller (14) moves away from the convex surface of the convex panel (16), the spring (73) pushes the piston (71) upward to reset, causing the one-way valve (72) to close, the drain pipe (11) to open, and the material to be introduced into the lower part of the piston (71). At the same time, the piston (71) pushes the material out through the liquid outlet (17) until the roller (14) contacts the convex surface of the convex panel (16) again, causing the piston (71) to move downward again. This causes the convex panel (16) to work with the spring (73) to drive the piston (71) to move up and down repeatedly, and to intermittently discharge the material into the upper part of the heating plate (20). S4. The material flows intermittently on the heating plate (20), so that the heating plate (20) keeps heating the material, so that the material heating steam flows upward, so that the steam enters the condenser (32) and condenses into a solution, so that the solution enters the collection box (31) for collection.

9. The preparation method according to claim 8, characterized in that, The collection box (31) collects fractions at temperatures above 700°C.

Citation Information

Patent Citations

  • Preparation system and purification method of neopentyl glycol copolymer

    CN113893566A

  • Rotary evaporator for extracting pinus sylvestris barks

    CN212119087U

  • Kettle type reaction system for synthesizing methylal by liquid-phase one-step oxidation of methanol

    CN213475848U