Vacuum distillation preparation device for high-purity selenium

Abstract

The utility model discloses a vacuum distillation preparation device for high-purity selenium. Comprising a heating assembly, a sealing shell, a vacuumizing assembly and a gas supply assembly, wherein the heating assembly is arranged in the vertical direction in a layered mode so as to correspondingly provide heating temperature in a layered mode; the sealing shell is arranged in the heating assembly; the vacuumizing assembly is connected with the sealing shell and used for vacuumizing the sealing shell; the containing shell is arranged in the sealing shell and is used for containing a raw material selenium; the reflux tower tray is arranged in the sealing shell, is positioned above the containing shell, is communicated with the containing shell and is used for refluxing high-boiling-point impurities; the condensing shell is arranged in the sealing shell, is positioned above the reflux tower tray, is communicated with the reflux tower tray and is used for condensing to form solid selenium; and the collecting assembly is arranged above the condensing shell, is communicated with the condensing shell and is used for collecting impurities with low boiling points.

Description

Technical Field

[0001] This utility model relates to the field of chemical material preparation equipment technology, and in particular, to a high-purity selenium vacuum distillation preparation device. Background Technology

[0002] High-purity selenium refers to selenium products with a selenium content of 99.999% 5N and 99.9999% 6N. It is mainly used in the preparation of compound semiconductors, optoelectronic materials, electrostatic photography and optical instruments. Its applications are wide-ranging and unique, and it has a promising market prospect.

[0003] The existing high-purity selenium is mainly prepared by vacuum distillation. The principle is that, under vacuum regulation, the vapor pressure and evaporation rate of selenium and impurity elements are different at the same temperature. By controlling a certain temperature and vacuum, selenium and some impurities volatilize and selectively condense, thereby separating selenium from impurity elements and finally obtaining high-purity selenium.

[0004] For example, Chinese invention patent CN109646979B discloses a high-purity oxygen-free selenium vacuum distillation device, which first prepares liquid raw material selenium through a quartz crucible, and then distills and condenses the liquid raw material selenium into solid selenium, that is, a stepwise method is used to prepare high-purity selenium.

[0005] However, the aforementioned high-purity selenium preparation device involves the transfer of liquid selenium. The sealing of liquid selenium during storage and transportation cannot be guaranteed, which can easily cause selenium to oxidize and volatilize, forming selenium oxide mist that pollutes the environment, reduces the selenium recovery rate, and causes resource waste. Utility Model Content

[0006] This invention provides a high-purity selenium vacuum distillation preparation device to solve the technical problems of existing high-purity selenium preparation devices that easily cause selenium oxidation and volatilization, resulting in environmental pollution and low selenium recovery rate.

[0007] According to one aspect of the present invention, a high-purity selenium vacuum distillation preparation apparatus is provided, comprising a heating assembly arranged vertically in layers to provide heating temperatures for each layer, a sealed shell disposed within the heating assembly, a vacuum pumping assembly connected to the sealed shell for evacuating the sealed shell, a gas supply assembly connected to the sealed shell for introducing protective gas into the sealed shell, a holding shell disposed within the sealed shell for holding raw material selenium, a reflux tray disposed within the sealed shell above and communicating with the holding shell for refluxing high-boiling-point impurities, a condensing shell disposed within the sealed shell above and communicating with the reflux tray for condensing to form solid selenium, and a collecting assembly disposed above and communicating with the condensing shell for collecting low-boiling-point impurities.

[0008] As a further improvement to the above technical solution:

[0009] Furthermore, the heating assembly includes a distillation heating layer, a reflux heating layer, and a condensation heating layer arranged sequentially in a vertically upward direction. A first preset temperature difference is maintained between the distillation heating layer and the reflux heating layer, and a second preset temperature difference is maintained between the reflux heating layer and the condensation heating layer. The distillation heating layer is arranged correspondingly to the container shell, the reflux heating layer is arranged correspondingly to the reflux tray, and the condensation heating layer is arranged correspondingly to the condensation shell.

[0010] Furthermore, a distillation thermometer is installed in the distillation heating layer; and / or a reflux thermometer is installed in the reflux heating layer; and / or a condensation thermometer is installed in the condensation heating layer.

[0011] Furthermore, the inner wall surface of the condenser shell is arranged in a conical shape, extending outward from bottom to top.

[0012] Furthermore, a cooling water jacket corresponding to the collection assembly is fitted onto the outer wall of the sealed housing.

[0013] Furthermore, the collection assembly includes a blocking cover connected to the top of the condensation shell for preventing low-boiling-point impurities from moving upward, and a collection shell connected to the lower end face of the blocking cover for collecting low-boiling-point impurities. The top side wall of the collection shell is provided with a collection port for low-boiling-point impurities to enter the inner cavity of the collection shell.

[0014] Furthermore, the lower end face of the barrier cover is arranged in a conical shape, extending inward from bottom to top.

[0015] Furthermore, the reflux tray includes reflux channels spirally upwards in the vertical direction.

[0016] Furthermore, the top of the sealing housing is provided with a top opening and a sealing cover for opening or closing the top opening of the sealing housing, and a sealing ring is provided between the sealing cover and the sealing housing.

[0017] Furthermore, a three-way valve is installed on the sealing cover, which is connected to the inner cavity of the sealing housing, the vacuum assembly, and the gas supply assembly, respectively.

[0018] This utility model has the following beneficial effects:

[0019] This invention relates to a high-purity selenium vacuum distillation preparation apparatus. First, the raw material selenium is placed in a container shell. Then, a reflux tray, a condenser shell, a collection assembly, a vacuum assembly, and a gas supply assembly are installed sequentially. The vacuum assembly then evacuates the sealed container to a preset vacuum level. After reaching this preset vacuum, the heating assembly provides distillation, reflux, and condensation temperatures vertically in layers to heat the container shell, reflux tray, and condenser shell respectively. This causes the raw material selenium in the container shell to evaporate into selenium vapor at the distillation temperature. The selenium vapor rises and flows through the reflux tray, extending its flow path. This allows high-boiling-point impurities in the selenium vapor to condense and return to the container shell at the reflux temperature, increasing the purity of the selenium. When the selenium vapor rises into the condenser shell, it condenses on the inner surface of the condenser shell. High-purity solid selenium is crystallized, while low-boiling-point impurities rise to the collection component. After a preset processing time, the vacuum component stops working, and protective gas is introduced into the sealed shell through the gas supply component to relieve pressure. Then, the heating component stops working, and finally, the sealed shell is opened and the condensation shell is removed to obtain 5N-6N high-purity selenium. This scheme achieves a fully enclosed one-step preparation of high-purity selenium through the coordinated operation of the heating component, sealed shell, vacuum component, gas supply component, container shell, reflux tray, condensation shell, and collection component. Compared with existing technologies, it reduces the preparation process, and since both the incoming and outgoing materials are solid, it avoids the oxidation and volatilization of liquid selenium, preventing waste of selenium and environmental pollution. At the same time, it has a high degree of automation, simple operation, and strong practicality, making it suitable for widespread promotion and application.

[0020] In addition to the objectives, features, and advantages described above, this utility model has other objectives, features, and advantages. The present utility model will now be described in further detail with reference to the figures. Attached Figure Description

[0021] The accompanying drawings, which form part of this application, are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an undue limitation of the present invention. In the drawings:

[0022] Figure 1 This is a schematic diagram of the high-purity selenium vacuum distillation preparation apparatus according to a preferred embodiment of the present invention.

[0023] Legend:

[0024] 100. Heating assembly; 110. Distillation heating layer; 120. Reflux heating layer; 130. Condensation heating layer; 140. Distillation thermometer; 150. Reflux thermometer; 160. Condensation thermometer; 200. Sealed housing; 300. Container housing; 400. Reflux tray; 500. Condensation housing; 600. Collection assembly; 610. Barrier cover; 620. Collection housing; 630. Collection port; 700. Cooling water jacket. Detailed Implementation

[0025] The embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, the present invention can be implemented in many different ways as defined and covered below.

[0026] Figure 1 This is a schematic diagram of the high-purity selenium vacuum distillation preparation apparatus according to a preferred embodiment of the present invention.

[0027] like Figure 1As shown, the high-purity selenium vacuum distillation preparation apparatus of this embodiment includes a heating component 100 for vertically layered arrangement to provide heating temperature for each layer, a sealed housing 200 arranged within the heating component 100, a vacuum pumping component connected to the sealed housing 200 for evacuating the sealed housing 200, a gas supply component connected to the sealed housing 200 for introducing protective gas into the sealed housing 200, a holding housing 300 arranged within the sealed housing 200 for holding raw material selenium, a reflux tray 400 arranged within the sealed housing 200 above and connected to the holding housing 300 for refluxing high-boiling-point impurities, a condensing housing 500 arranged within the sealed housing 200 above and connected to the reflux tray 400 for condensing to form solid selenium, and a collecting component 600 arranged above and connected to the condensing housing 500 for collecting low-boiling-point impurities. Specifically, the high-purity selenium vacuum distillation preparation apparatus of this invention first places the raw material selenium in the holding shell 300, then sequentially installs the reflux tray 400, condenser shell 500, collecting assembly 600, vacuum assembly, and gas supply assembly. The vacuum assembly then evacuates the sealed shell 200 to a preset vacuum level. The heating assembly 100 provides distillation temperature, reflux temperature, and condensation temperature in a vertical direction to heat the holding shell 300, reflux tray 400, and condenser shell 500 respectively. This causes the raw material selenium in the holding shell 300 to evaporate into selenium vapor at the distillation temperature. The selenium vapor rises and flows through the reflux tray 400, extending the flow path of the selenium vapor. This allows high-boiling-point impurities in the selenium vapor to condense and return to the holding shell 300 at the reflux temperature, improving the purity of the selenium. When the selenium vapor rises into the condenser shell 500, it is heated... High-purity solid selenium is condensed and crystallized on the inner surface of the 0-tonne container, while low-boiling-point impurities rise to the collection component 600. After a preset processing time, the vacuum component stops working, and protective gas is introduced into the sealed housing 200 through the gas supply component to relieve pressure. Then, the heating component 100 stops working. Finally, the sealed housing 200 is opened, and the condensation housing 500 is removed to obtain 5N-6N high-purity selenium. This scheme achieves a fully enclosed one-step preparation of high-purity selenium through the coordinated operation of the heating component 100, the sealed housing 200, the vacuum component, the gas supply component, the holding housing 300, the reflux tray 400, the condensation housing 500, and the collection component 600. Compared with existing technologies, this reduces the preparation process, and since both the incoming and outgoing materials are solid, it avoids the oxidation and volatilization of liquid selenium, preventing waste of selenium and environmental pollution. It also features high automation, simple operation, and strong practicality, making it suitable for widespread promotion and application. It should be understood that high-boiling-point impurities refer to substances with boiling points higher than selenium, while low-boiling-point impurities refer to substances with boiling points lower than selenium. Optionally, the protective gas is high-purity argon.

[0028] like Figure 1 As shown, in this embodiment, the heating assembly 100 includes a distillation heating layer 110, a reflux heating layer 120, and a condensation heating layer 130 arranged sequentially in a vertically upward direction. A first preset temperature difference is maintained between the distillation heating layer 110 and the reflux heating layer 120, and a second preset temperature difference is maintained between the reflux heating layer 120 and the condensation heating layer 130. The distillation heating layer 110 is arranged correspondingly to the container shell 300, the reflux heating layer 120 is arranged correspondingly to the reflux tray 400, and the condensation heating layer 130 is arranged correspondingly to the condensation shell 500. Specifically, a first preset temperature difference is maintained between the distillation heating layer 110 and the reflux heating layer 120, and a second preset temperature difference is maintained between the reflux heating layer 120 and the condensation heating layer 130. This ensures that the heating temperature in the distillation heating layer 110 is the highest, the heating temperature in the reflux heating layer 120 is the second highest, and the heating temperature in the condensation heating layer 130 is the lowest. This allows the container shell 300, the reflux tray 400, and the condensation shell 500 to be heated by the distillation temperature, the splitting temperature, and the condensation temperature, respectively. Optionally, the heating assembly 100 uses resistance wire heating or electromagnetic heating. It should be understood that the first and second preset temperature differences can be adaptively selected according to requirements, as long as the above functions are achieved.

[0029] like Figure 1 As shown, in this embodiment, a distillation thermometer 140 is installed inside the distillation heating layer 110. Specifically, the distillation thermometer 140 detects and displays the heating temperature of the distillation heating layer 110 to achieve regulation and control of the distillation temperature, ensuring that the raw material selenium in the container 300 is vaporized at the distillation temperature.

[0030] like Figure 1 As shown, in this embodiment, a reflux thermometer 150 is installed inside the reflux heating layer 120. Specifically, the reflux thermometer 150 detects and displays the heating temperature of the reflux heating layer 120 to achieve regulation and control of the reflux temperature. This ensures that high-boiling-point impurities in the selenium vapor in the reflux tray 400 are liquefied and refluxed at the reflux temperature, thereby improving the purity of selenium and preventing selenium from condensing at the reflux temperature, thus improving the selenium recovery rate.

[0031] like Figure 1 As shown, in this embodiment, a condensation thermometer 160 is installed inside the condensation heating layer 130. Specifically, the condensation thermometer 160 detects and displays the heating temperature of the condensation heating layer 130 to achieve regulation and control of the condensation temperature, ensuring that the selenium vapor inside the condensation shell 500 solidifies at the condensation temperature, while avoiding the solidification of low-boiling-point impurities, thereby improving the purity of selenium and obtaining high-purity selenium.

[0032] like Figure 1As shown, in this embodiment, the inner wall surface of the condenser shell 500 is arranged in a conical shape, extending outward from bottom to top. Specifically, the conical shape increases the inner wall area of ​​the condenser shell 500, facilitating the crystallization and solidification of selenium.

[0033] like Figure 1 As shown, in this embodiment, a cooling water jacket 700, corresponding to the collection component 600, is fitted onto the outer wall of the sealed housing 200. Specifically, the cooling water jacket 700 further reduces the temperature inside the collection component 600 to achieve the condensation of low-boiling-point impurities and thus the collection of low-boiling-point impurities.

[0034] like Figure 1 As shown, in this embodiment, the collection assembly 600 includes a blocking cover 610 connected to the top of the condensation shell 500 to prevent low-boiling-point impurities from moving upwards, and a collection shell 620 connected to the lower end face of the blocking cover 610 to collect low-boiling-point impurities. A collection port 630 is provided on the top sidewall of the collection shell 620 to allow low-boiling-point impurities to enter the inner cavity of the collection shell 620. Specifically, by blocking the upward movement of low-boiling-point impurities through the blocking cover 610, the low-boiling-point impurities enter the collection shell 620 through the collection port 630, thereby achieving the collection of low-boiling-point impurities. Optionally, multiple collection ports 630 are arranged at intervals along the circumference of the collection shell 620.

[0035] like Figure 1 As shown, in this embodiment, the lower end face of the blocking cover 610 is arranged in a conical shape, extending inward from bottom to top. Specifically, the conical surface blocks and guides low-boiling-point impurities, thereby improving collection efficiency.

[0036] In this embodiment, the reflux tray 400 includes a reflux channel spirally upward in the vertical direction. Specifically, the reflux channel greatly extends the flow path of selenium vapor, facilitating the liquefaction and reflux of high-boiling-point impurities, which is beneficial to improving the purity of selenium.

[0037] like Figure 1 As shown, in this embodiment, the top of the sealing housing 200 is provided with a top opening and a sealing cover for opening or closing the top opening of the sealing housing 200. A sealing ring is provided between the sealing cover and the sealing housing 200. Specifically, before the purification operation, the sealing cover is opened to open the top opening of the sealing housing 200 so that the raw material selenium, the reflux tray 400, the condenser housing 500, and the collection assembly 600 can be assembled into the sealing housing 200. During the purification operation, the sealing cover is closed to close the top opening of the sealing housing 200, and the sealing ring improves the sealing performance, facilitating the vacuuming assembly.

[0038] In this embodiment, a three-way valve is provided on the sealing cover, which is connected to the inner cavity of the sealing housing 200, the vacuum assembly, and the gas supply assembly. Specifically, during the purification operation, the three-way valve is connected to the inner cavity of the sealing housing 200 and the vacuum assembly to achieve vacuum distillation through vacuuming. During the collection operation, the three-way valve is connected to the inner cavity of the sealing housing 200 and the gas supply assembly to introduce protective gas for depressurization.

[0039] In this embodiment, a selenium raw material with a purity of 99.61% is used for purification. First, the raw selenium is crushed until the particle size is ≤10mm, then weighed to 15kg and placed into the holding shell 300. Next, the reflux tray 400, condenser shell 500, and collecting assembly 600 are sequentially installed and placed into the sealing shell 200, which is then sealed. The vacuum assembly is then activated, and after reaching the preset vacuum level, the heating assembly 100 is activated. The raw selenium is then distilled and refluxed at the distillation temperature, reflux temperature, and condensation temperature, respectively. After purification processes such as flow and condensation, the protective gas supply component is activated to introduce high-purity argon gas for depressurization. After cooling, the condenser shell 500 is removed. High-boiling-point impurities are contained in the holding shell 300, and are collected and weighed at 1.13 kg. Solid selenium at both ends of the condenser shell 500 is removed, and is collected and weighed at 1.67 kg. The high-purity selenium in the middle part is obtained, and is collected and weighed at 11.84 kg. Low-boiling-point impurities are contained in the collecting component 600, and are collected and weighed at 0.31 kg. The purification rate of high-purity selenium is calculated to be 78.9%.

[0040] The above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A vacuum distillation apparatus for preparing high-purity selenium, characterized in that, This includes a heating assembly (100) arranged vertically in layers to provide heating temperatures for each layer; a sealed housing (200) disposed within the heating assembly (100); a vacuum pumping assembly connected to the sealed housing (200) for evacuating the sealed housing (200); a gas supply assembly connected to the sealed housing (200) for introducing protective gas into the sealed housing (200); a storage housing (300) disposed within the sealed housing (200) for holding the raw material selenium; and other components arranged in the sealed housing. The enclosure (200) contains a reflux tray (400) for refluxing high-boiling-point impurities, located above and connected to the holding shell (300); a condenser shell (500) for condensing and forming solid selenium, located above and connected to the reflux tray (400) within the enclosure (200); and a collection assembly (600) for collecting low-boiling-point impurities, located above and connected to the condenser shell (500).

2. The high-purity selenium vacuum distillation preparation apparatus according to claim 1, characterized in that, The heating assembly (100) includes a distillation heating layer (110), a reflux heating layer (120), and a condensation heating layer (130) arranged sequentially in a vertically upward direction. A first preset temperature difference is maintained between the distillation heating layer (110) and the reflux heating layer (120), and a second preset temperature difference is maintained between the reflux heating layer (120) and the condensation heating layer (130). The distillation heating layer (110) is arranged correspondingly to the container shell (300), the reflux heating layer (120) is arranged correspondingly to the reflux tray (400), and the condensation heating layer (130) is arranged correspondingly to the condensation shell (500).

3. The high-purity selenium vacuum distillation preparation apparatus according to claim 2, characterized in that, A distillation thermometer (140) is installed inside the distillation heating layer (110); and / or A reflux thermometer (150) is installed inside the reflux heating layer (120); and / or A condensation thermometer (160) is installed inside the condensation heating layer (130).

4. The high-purity selenium vacuum distillation preparation apparatus according to claim 1, characterized in that, The inner wall of the condenser shell (500) is arranged in a conical shape that extends outward from bottom to top.

5. The high-purity selenium vacuum distillation preparation apparatus according to claim 1, characterized in that, A cooling water jacket (700) corresponding to the collection assembly (600) is fitted on the outer wall of the sealed housing (200).

6. The high-purity selenium vacuum distillation preparation apparatus according to any one of claims 1-5, characterized in that, The collection assembly (600) includes a blocking cover (610) connected to the top of the condenser housing (500) for blocking low-boiling-point impurities from moving upward, and a collection housing (620) connected to the lower end face of the blocking cover (610) for collecting low-boiling-point impurities. The top side wall of the collection housing (620) is provided with a collection port (630) for low-boiling-point impurities to enter the inner cavity of the collection housing (620).

7. The high-purity selenium vacuum distillation preparation apparatus according to claim 6, characterized in that, The lower end face of the blocking cover (610) is arranged in a conical shape that extends inward from bottom to top.

8. The high-purity selenium vacuum distillation preparation apparatus according to any one of claims 1-5, characterized in that, The reflux tray (400) includes reflux channels spirally upward in the vertical direction.

9. The high-purity selenium vacuum distillation preparation apparatus according to any one of claims 1-5, characterized in that, The top of the sealing housing (200) is provided with a top opening and a sealing cover for opening or closing the top opening of the sealing housing (200), and a sealing ring is provided between the sealing cover and the sealing housing (200).

10. The high-purity selenium vacuum distillation preparation apparatus according to claim 9, characterized in that, The sealing cover is equipped with a three-way valve, which is connected to the inner cavity of the sealing housing (200), the vacuum assembly, and the gas supply assembly.

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