A tube sealing device and a tube sealing method

Abstract

The application discloses a tube sealing device and a tube sealing method. The tube sealing device comprises a charging bottle with a first connecting neck and a second connecting neck, a quartz fixing sleeve, a heater, a tube sealing assembly for tube sealing operation of the first connecting neck and the second connecting neck, a gas filling assembly for providing inert gas, a gas extraction assembly and a control unit. The quartz fixing sleeve is installed in the heater, the charging bottle is installed in the quartz fixing sleeve, the gas filling assembly is detachably connected with the first connecting neck for inert gas feeding into the charging bottle, the gas extraction assembly is detachably connected with the second connecting neck for vacuum gas extraction operation on the charging bottle, and the control unit is electrically connected with the heater, the tube sealing assembly and the gas extraction assembly. The double-neck structure of the application provides a more effective channel for inert gas feeding, facilitates vacuum gas extraction operation, can more thoroughly remove air in the charging bottle and reduces the risk of tube explosion.

Description

Technical Field

[0001] This invention relates to the field of processing equipment technology, and in particular to a sealing device and sealing method. Background Technology

[0002] Currently, the production of high-purity red phosphorus primarily involves the direct conversion of yellow phosphorus to red phosphorus. During the loading process, a water seal is typically used to isolate the yellow phosphorus from the air. This conversion process usually takes place under high temperature and atmospheric pressure or high pressure conditions, involving a series of steps including melting, sealing, conversion, ball milling, alkaline boiling, cleaning, dehydration, and drying of the yellow phosphorus. Existing quartz sealing devices mostly consist of a base, a vacuum sealing machine, a molecular pump unit, and a hydrogen-oxygen generator. These devices are generally only suitable for loading and sealing ordinary materials. In the yellow phosphorus to red phosphorus conversion process, existing traditional quartz conversion bottles have only one bottleneck, which is insufficient to meet the requirements and cannot effectively remove air from the bottle. This prevents the introduction of inert gas for protection during the yellow phosphorus to red phosphorus conversion reaction, leading to the formation of byproducts that affect product quality. Furthermore, the water seal method results in a certain amount of water remaining inside and on the surface of the yellow phosphorus. If the water is not completely removed, the loading bottle is prone to bursting during the conversion process, posing a safety hazard and endangering personal safety. Summary of the Invention

[0003] The technical problem this invention aims to solve is that existing traditional quartz conversion bottles have only one bottleneck, which is insufficient to meet the requirements and cannot effectively remove air from the bottle. This prevents the introduction of inert gas for protection during the yellow phosphorus to red phosphorus conversion reaction, leading to the formation of byproducts that affect product quality. Furthermore, the use of water-sealing results in a certain amount of water remaining inside and on the surface of the yellow phosphorus. If the water is not completely removed, the filling bottle is prone to bursting during the conversion process, posing a safety hazard and endangering personal safety.

[0004] To address the aforementioned technical problems, this invention provides a sealing device and a sealing method.

[0005] In a first aspect, the present invention provides a sealing device, comprising a filling bottle having a first connecting neck and a second connecting neck, a quartz retaining sleeve, a heater, a sealing assembly for sealing the first connecting neck and the second connecting neck, an inflation assembly for providing inert gas, a vacuum assembly, and a control unit. The quartz retaining sleeve is installed inside the heater, the filling bottle is installed inside the quartz retaining sleeve, the inflation assembly is detachably connected to the first connecting neck for introducing inert gas into the filling bottle, the vacuum assembly is detachably connected to the second connecting neck for vacuuming the filling bottle, and the control unit is electrically connected to the heater, the sealing assembly, and the vacuum assembly.

[0006] Secondly, the present invention provides a sealing method, comprising the following steps:

[0007] Provide a sealing device as described above, open the sealing device, and the filling bottle of the sealing device contains yellow phosphorus and water;

[0008] Open the inflation assembly and fill the filling bottle with inert gas through the first connecting neck;

[0009] Open the vacuum assembly and evacuate air from the filling bottle through the second connecting neck;

[0010] Turn on the heater to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component;

[0011] The sealing assembly is used to seal the first connecting neck of the filling bottle;

[0012] The vacuum assembly is kept open until the air pressure inside the filling bottle is 30-100 Pa.

[0013] The heater heats at a preset temperature for a predetermined time and keeps the vacuum assembly open to expel air and moisture from the filling bottle;

[0014] The sealing assembly is used to seal the second connecting neck of the filling bottle.

[0015] Thirdly, the present invention also provides a sealing method, comprising the following steps:

[0016] Provide a sealing device as described above, open the sealing device, and the filling bottle of the sealing device contains yellow phosphorus and water;

[0017] Open the inflation assembly and fill the filling bottle with inert gas through the first connecting neck;

[0018] Open the vacuum assembly and evacuate air from the filling bottle through the second connecting neck;

[0019] Turn on the heater to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component;

[0020] The vacuum assembly is kept open until the air pressure in the filling bottle is 30-100 Pa;

[0021] The heater heats at a preset temperature for a predetermined time and keeps the vacuum assembly open to expel air and moisture from the filling bottle;

[0022] The vacuum assembly is closed, and the second connecting neck of the filling bottle is sealed using the sealing assembly.

[0023] Open the inflation assembly and introduce a preset volume of the inert gas into the filling bottle;

[0024] The sealing assembly is used to seal the first connecting neck of the filling bottle.

[0025] Compared with the prior art, the sealing device and sealing method of this invention have the following advantages:

[0026] The double-neck structure of this invention provides a more efficient channel for the introduction of inert gases (such as nitrogen or argon), and also facilitates vacuum evacuation operations. This allows for a more thorough removal of air from the filling bottle, creating a better vacuum or positive pressure environment to promote the conversion of yellow phosphorus to red phosphorus, reducing byproduct formation, and thus improving product purity. Furthermore, in conjunction with the gas filling and evacuation components, it facilitates the rapid removal of residual moisture and prevents external moisture from entering, further ensuring dry conditions during the conversion process, reducing the risk of tube bursting. Combined with the use of the sealing component, it ensures that both the first and second connecting necks are sealed during operation to maintain good sealing performance, preventing external air ingress and internal gas leakage. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the sealing device provided in an embodiment of the present invention;

[0028] Figure 2 This is a schematic diagram of the structure of the filling bottle provided in an embodiment of the present invention;

[0029] In the diagram, 1. Filling bottle; 11. First connecting neck; 12. Second connecting neck; 13. Body; 2. Quartz retaining sleeve; 3. Heater; 4. Sealing assembly; 41. Hydrogen-oxygen cylinder; 42. Moving platform; 421. Base plate; 422. Pulley; 43. Flamethrower; 44. First connecting pipe; 5. Gas filling assembly; 51. Inert gas cylinder; 52. Second connecting pipe; 53. Control valve; 54. Flow sensor; 6. Vacuuming assembly; 61. Vacuuming component; 62. Third connecting pipe; 63. Pressure gauge; 7. Control unit; 8. Support assembly; 9. Mounting platform. Detailed Implementation

[0030] The specific embodiments of the present invention will be described in further detail below with reference to the accompanying drawings and examples. The following examples are for illustrative purposes only and are not intended to limit the scope of the invention.

[0031] like Figure 1 and Figure 2As shown, the present invention provides a sealing device, including a filling bottle 1 having a first connecting neck 11 and a second connecting neck 12, a quartz retaining sleeve 2, a heater 3, a sealing assembly 4 for sealing the first connecting neck 11 and the second connecting neck 12, an inflation assembly 5 for providing inert gas, an air extraction assembly 6, and a control unit 7. The filling bottle 1 is installed inside the quartz retaining sleeve 2, which is used to stably install and fix the filling bottle 1, ensuring that the bottle will not move or tilt against the heater 3 during heating or other processes. Inside the heater 3, the necessary heat is provided for the conversion reaction. The gas filling component 5 is detachably connected to the first connecting neck 11 and is used to introduce inert gas into the material chamber to protect the yellow phosphorus from contact with oxygen in the air and reduce the generation of by-products. The gas extraction component 6 is detachably connected to the second connecting neck 12 and is used to perform gas extraction operation into the material chamber to extract air and other gases, remove air or create a near-vacuum environment, which helps to improve the conversion efficiency. The control unit 7 is electrically connected to the heater 3, the sealing tube component 4 and the gas extraction component 6 to realize the automated control of the operation of these components.

[0032] This embodiment uses a quartz retaining sleeve 2 to fix the filling bottle 1, improving stability during experiments or production and reducing safety hazards caused by bottle movement. Simultaneously, the combined use of the heater 3 and the quartz retaining sleeve 2, along with the support of the control unit 7, makes the heating process more uniform and controllable, avoiding localized overheating and promoting the smooth progress of the yellow phosphorus to red phosphorus conversion reaction. Combined with the gas filling component 5 and the vacuum component 6, it achieves effective management of inert gases and effective removal of air, further reducing the possibility of by-product formation and accelerating the moisture removal process, thus improving the purity of the final product. Furthermore, the sealing component 4 ensures that the first connecting neck 11 and the second connecting neck 12 are sealed during operation to maintain good sealing performance, preventing external air from entering and also preventing internal gas leakage.

[0033] It should be noted that in this embodiment, the synergistic effect of the air extraction component 6 and the heater 3 is used to shorten the dehydration time from 11 hours to 1 hour, which greatly improves the dehydration efficiency and sealing efficiency, saving valuable time resources in the production process. After sealing the filling bottle 1, it can be flexibly moved to a variety of high temperature and atmospheric pressure conversion devices that meet the process requirements, so as to produce different allotropic phosphorus, and is not limited to producing a certain type of red phosphorus.

[0034] The filling bottle 1 also includes a body 13, which has a filling chamber for containing yellow phosphorus. A first connecting neck 11 and a second connecting neck 12 are positioned opposite each other at one end of the body 13, and both the first connecting neck 11 and the second connecting neck 12 are connected to the filling chamber. The end face of the body 13 facing away from the first connecting neck 11 is arc-shaped. Compared to the traditional flat-bottom design, this arc-shaped structure allows for more uniform heating of the entire filling bottle during the heating process, reducing the occurrence of local overheating and improving the stability of the yellow phosphorus to red phosphorus conversion reaction. It also reduces the safety risks caused by uneven temperature. Furthermore, the double-neck structure provides a more efficient channel for the introduction of inert gases (such as nitrogen or argon) and facilitates vacuum evacuation operations, allowing for more thorough removal of air from the filling bottle. This creates a better vacuum or positive pressure environment to promote the conversion of yellow phosphorus to red phosphorus, reducing the formation of byproducts and thus improving product purity. In addition, it facilitates the rapid removal of residual moisture and prevents external moisture from entering, further ensuring dry conditions during the conversion process and reducing the risk of tube explosion.

[0035] It should be noted that after the filling bottle 1 is sealed, it can serve as an independent conversion bottle. Based on the production of multiple allotropes of phosphorus from yellow phosphorus, it has greater flexibility in production needs. Since the filling bottle 1 generally adopts high temperature and normal pressure or high temperature and high pressure conversion conditions, there is a certain risk of tube bursting. A certain pressure can be applied to the outside of the conversion bottle to maintain the pressure difference between the inside and outside of the conversion bottle, thereby reducing the risk of tube bursting. The production method of isolating the sealing device from the conversion device is safer.

[0036] In practical applications, this sealing device can be used to seal the filling bottle 1, thereby creating different reaction environments in the filling bottle 1, including a high-temperature vacuum environment and a high-temperature positive pressure environment.

[0037] The following example illustrates the construction of a high-temperature vacuum environment:

[0038] At the start of the sealing operation, the gas filling assembly 5 is configured to fill the filling bottle 1 with inert gas through the first connecting neck 11 to expel the air inside the bottle and protect the yellow phosphorus from contact with oxygen; the vacuum assembly 6 is configured to vacuum the filling bottle 1 through the second connecting neck 12 to assist in expelling the air and other possible gases inside the filling bottle 1, creating a near-vacuum environment for subsequent operations; the heater 3 is configured to heat the yellow phosphorus to gradually increase the temperature until the yellow phosphorus reaches its melting point and melts completely.

[0039] After the yellow phosphorus is heated to a molten state, the gas filling component 5 is configured to be closed, the gas extraction component 6 is configured to remain open, the tube sealing component 4 is configured to seal the first connecting neck 11 to prevent outside air from entering, and the gas extraction component 6 is configured to remain open until the gas pressure inside the filling bottle 1 is 30-100 Pa, so as to continuously extract residual gas and maintain the corresponding gas pressure environment.

[0040] After the pressure inside the filling bottle 1 reaches 30-100 Pa and the first connecting neck 11 is sealed, the evacuation assembly 6 is configured to remain on, and the heater 3 is configured to heat at a preset temperature for a predetermined time. Continuous evacuation in this state helps to remove any residual air and moisture as much as possible, ensuring that the reaction environment is as pure as possible.

[0041] After the heater 3 heats at the preset temperature for a predetermined time, the vacuum assembly 6 is configured to be in the off state, and the sealing assembly 4 is configured to seal the second connecting neck 12 to completely seal the filling bottle 1, so that the reaction products or materials inside are in a completely isolated state.

[0042] This embodiment ensures that the entire process is carried out in a strictly controlled environment, which not only improves the selectivity and efficiency of the reaction, but also guarantees the safety of the sealing tube.

[0043] The following example demonstrates how to create a vacuum positive pressure environment:

[0044] At the start of the sealing operation, the gas filling assembly 5 is configured to fill the filling bottle 1 with inert gas through the first connecting neck 11 to expel the air in the filling bottle 1, ensuring that the yellow phosphorus does not come into contact with oxygen and reducing the generation of by-products; the vacuum assembly 6 is configured to vacuum the filling bottle 1 through the second connecting neck 12 to assist in expelling the air and other possible gases in the filling bottle 1, creating a near-vacuum environment for subsequent operations; the heater 3 is configured to heat the yellow phosphorus to gradually increase the temperature until the yellow phosphorus reaches its melting point and melts completely.

[0045] After the yellow phosphorus is heated to a molten state, the gas filling component 5 is configured to be closed, and the gas extraction component 6 is configured to be kept open until the gas pressure inside the filling bottle 1 is 30-100Pa, so as to continuously extract residual gas and maintain the corresponding gas pressure environment.

[0046] After the gas pressure in the filling bottle 1 is 30-100Pa, the vacuum component 6 is configured to remain on, and the heater 3 is configured to heat at a preset temperature for a predetermined time. In this state, continuous vacuuming helps to remove any possible residual air and moisture, ensuring that the reaction environment is as pure as possible.

[0047] After the heater 3 heats at the preset temperature for a predetermined time, the air extraction component 6 is configured to be in the off state, and the sealing component 4 is configured to seal the second connecting neck 12 to close the interface at that end and prevent air from entering.

[0048] After the second connecting neck 12 is sealed, the inflation component 5 is configured to be in the open state and fills the filling bottle 1 with a preset amount of inert gas, adjusting the gas pressure inside the bottle to a safe level to avoid bottle rupture or other safety hazards due to excessive pressure difference between the inside and outside.

[0049] After the filling bottle 1 is filled with a preset amount of inert gas, the sealing assembly 4 is configured to seal the first connecting neck 11 of the filling bottle 1, completing the entire sealing process and ensuring that the environment inside the filling bottle 1 is completely isolated from the outside world, thus maintaining the purity and stability of the internal substances.

[0050] This embodiment ensures that the entire process is carried out in a strictly controlled environment, which not only improves the selectivity and efficiency of the reaction, but also guarantees the safety of the sealing tube.

[0051] Furthermore, the end face of the body 13 facing away from the first connecting neck 11 is arc-shaped, which helps to distribute heat more evenly throughout the entire filling bottle, reducing the occurrence of local overheating and improving the stability of the yellow phosphorus to red phosphorus conversion reaction. It also reduces safety risks caused by uneven temperature. Compared to a flat-bottom design, the round bottom reduces "hot spots" during heat conduction, resulting in a more uniform temperature throughout the reaction system.

[0052] Furthermore, the sealing assembly 4 includes an oxygen-hydrogen cylinder 41, a moving platform 42, a flame gun 43, and a first connecting pipe 44. The oxygen-hydrogen cylinder 41 is connected to the flame gun 43 through the first connecting pipe 44. The mixed gas provided by the oxygen-hydrogen cylinder 41 generates a high-temperature flame to heat and melt the glass material, thereby sealing the first connecting neck 11 or the second connecting neck 12. The flame gun 43 is mounted on the moving platform 42 to support and precisely control the position of the flame gun 43, ensuring that it can be accurately aligned with the position to be sealed. The flame gun 43 is electrically connected to the control unit 7.

[0053] In this embodiment, the flame gun 43 can be precisely positioned to the location where the tube needs to be sealed via the mobile platform 42 and is electrically connected via the control unit 7. The operation of the flame gun 43 (such as starting, stopping, adjusting flame intensity, etc.) can be automatically completed by the control system, reducing the possibility of human error and facilitating the realization of automated production processes.

[0054] Furthermore, the mobile platform 42 includes a base plate 421 and pulleys 422. The base plate 421 serves as the main support structure of the mobile platform 42, and the flamethrower 43 is mounted on the base plate 421. The pulleys 422 are mounted on the side of the base plate 421 opposite to the flamethrower 43, allowing the entire mobile platform 42 to move along a predetermined track or path. In this embodiment, the pulleys 422 enable the base plate 421 to move smoothly in the horizontal direction, allowing the flamethrower 43 mounted on it to reach the required working position, thereby achieving a better sealing effect.

[0055] Furthermore, the inflation assembly 5 includes an inert gas cylinder 51, a second connecting pipe 52, and a control valve 53. The inert gas cylinder 51 is detachably connected to the first connecting neck 11 via the second connecting pipe 52 for conveying gas from the inert gas cylinder 51 to the first connecting neck 11 of the filling bottle 1. The control valve 53 is installed on the second connecting pipe 52 for regulating and controlling the flow rate of the inert gas. The control valve 53 can be opened, closed, or the gas flow rate adjusted to ensure that gas is supplied to the filling bottle as needed.

[0056] In this embodiment, the inert gas cylinder 51 supplies inert gas to the filling bottle 1 through the second connecting pipe 52 to remove air and create an oxygen-free environment. This helps prevent yellow phosphorus from contacting oxygen in the air, reducing oxidation reactions and thus improving the purity of the red phosphorus product and reducing the formation of byproducts. Furthermore, the detachable connection between the second connecting pipe 52 and the first connecting neck 11 allows the inflation assembly 5 to be easily separated from the first connecting neck 11 for subsequent sealing operations.

[0057] Furthermore, the inflation assembly 5 also includes a flow rate sensor 54, which is installed in the second connecting pipe and located between the inert gas cylinder 51 and the control valve 53. The flow rate sensor 54 is electrically connected to the control unit 7.

[0058] In this embodiment, the flow rate sensor 54 can monitor the inert gas flow rate through the second connecting pipe 52 in real time, ensuring that the gas enters the filling bottle 1 at an appropriate rate, which helps maintain stable reaction conditions. Since the flow rate sensor 54 is electrically connected to the control unit 7, it can transmit the detected gas flow rate data to the control unit 7 in real time. The control unit 7 can adjust the opening of the control valve 53 based on this data, thereby achieving closed-loop control of the gas flow rate.

[0059] Furthermore, it also includes a support assembly 8, and the vacuum assembly 6 is slidably mounted on the support assembly 8 so as to move up and down relative to the support assembly 8. Different batches or different specifications of filling bottles 1 may have different heights and shapes. Through the up and down movement, the vacuum assembly 6 can adapt to filling bottles of different sizes and accurately align with the second connecting neck 12 of the filling bottle 1 to ensure the accuracy of the vacuuming operation.

[0060] Furthermore, the support assembly 8 comprises a magnetic bearing, a support member, and a drive member. The support member is slidably connected to the suction assembly 6, providing a platform for the suction assembly 6 to be slidably installed. The support member and the suction assembly 6 are connected via the magnetic bearing, providing a contactless connection, thereby reducing friction and wear, and improving the stability and accuracy of the system. The drive member controls the magnetic bearing to drive the suction assembly 6 to perform lifting and lowering movements. In this embodiment, the drive member controls the vertical movement of the rotor in the magnetic bearing, thereby driving the suction assembly 6 to perform lifting and lowering movements.

[0061] Furthermore, the vacuum assembly 6 includes a vacuum component 61, a third connecting pipe 62, and a pressure gauge 63. The vacuum component 61 is detachably connected to the second connecting neck 12 via the third connecting pipe 62, drawing air and other gases from the filling bottle 1 to create a near-vacuum environment. The pressure gauge 63 is installed on the third connecting pipe 62 to monitor the pressure within the pipe in real time. The pressure gauge 63 can display the current pressure value, helping operators understand the system's operating status. The vacuum component 61 and the pressure gauge 63 are electrically connected to the control unit 7, allowing adjustment of the vacuum component 61's operating status based on data feedback from the pressure gauge 63, thus achieving precise control of the vacuuming process.

[0062] Furthermore, the extraction unit 61 is a molecular pump unit, which can provide a very low pressure environment and does not use oil as a working medium, so it will not cause pollution to the system and is suitable for creating a highly clean environment.

[0063] In addition, the pumping unit 61 can also be a vacuum pump, which is suitable for a variety of different vacuum requirements. Compared with molecular pumps, vacuum pumps are usually less expensive and easier to maintain, thus saving costs.

[0064] Furthermore, heater 3 includes a resistance wire heater, a microwave heating device, or an infrared heating device.

[0065] Among these, resistance wire heaters can achieve relatively uniform heating through a well-designed heating element layout. They are also simple in structure, relatively low in cost, and easy to maintain. Microwave heating devices can rapidly increase the temperature of materials, making them suitable for rapid temperature rise. Furthermore, infrared heating devices can achieve directional heating, heating only specific areas to avoid unnecessary heat loss. Infrared heating also has a fast response speed, reaching the desired temperature in a short time.

[0066] Furthermore, a flange is provided at the connection between the inflation assembly 5 and the first connecting neck 11, and a flange is provided at the connection between the air extraction assembly 6 and the second connecting neck 12. In this embodiment, flanges are provided at the above two locations to effectively prevent gas leakage. Good sealing performance helps maintain the purity of the inert gas and reduces the entry of outside air, thereby improving conversion efficiency and product quality. It is also easy to disassemble.

[0067] Furthermore, it also includes an installation platform 9, on which the heater 3, sealing tube assembly 4, inflation assembly 5, vacuum assembly 6, and control unit 7 are installed. The circuit wiring of the heater 3, sealing tube assembly 4, and vacuum assembly 6 is embedded in the installation platform 9 and controlled by the control unit 7, which has an emergency stop button that can cut off all power with one click.

[0068] The present invention also provides a tube sealing method, which includes the following steps:

[0069] S130. A sealing device is provided, the sealing device is opened, and the filling bottle 1 of the sealing device contains yellow phosphorus and water.

[0070] S110. Open the inflation assembly 5 and inert gas into the filling bottle 1 through the first connecting neck 11 to expel the air in the bottle and protect the yellow phosphorus from contact with oxygen.

[0071] S120, Open the vacuum assembly 6 and draw air from the filling bottle 1 through the second connecting neck 12;

[0072] This step creates a flowing gas environment, which helps to expel air and other possible gases from the filling bottle 1, creating a near-vacuum environment for subsequent operations.

[0073] S130. Turn on heater 3 to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component.

[0074] This step uses heater 3 to heat the loading bottle 1 to melt the yellow phosphorus, so that the yellow phosphorus reaches the preset state to facilitate the subsequent reaction.

[0075] S150. The first connecting neck 11 of the filling bottle 1 is sealed using the sealing assembly 4. This step ensures that the port is sealed to prevent outside air from entering.

[0076] S160, The vacuum assembly 6 is kept open until the air pressure inside the filling bottle 1 is 30-100Pa;

[0077] This step aims to bring the filling bottle 1 into a vacuum state, which can effectively remove air and moisture from the bottle, reduce the risk of oxidation reaction, and provide a pure environment for subsequent conversion reactions.

[0078] S170, the heater 3 heats at a preset temperature for a predetermined time and keeps the vacuum component 6 open to remove air and moisture from the filling bottle 1;

[0079] This step uses high temperature to accelerate the movement of gas molecules, making them easier to extract. At the same time, high temperature also helps to maintain the melting of yellow phosphorus, preparing it for subsequent conversion reactions.

[0080] S180. The second connecting neck 12 of the filling bottle 1 is sealed using the sealing assembly 4. This step ensures that the port is sealed to prevent outside air from entering.

[0081] It should be noted that, through the above steps, a high-temperature vacuum environment can be formed in this embodiment. By simultaneously heating at high temperature while constructing the high-vacuum environment, air and moisture can be effectively removed, minimizing the risk of tube bursting due to moisture. This ensures operational safety, reduces the generation of oxidation byproducts, and improves the purity of the final product. Furthermore, the high temperature and vacuum environment help promote the conversion reaction of yellow phosphorus to red phosphorus, thereby improving the conversion efficiency.

[0082] In addition, during the sealing process in this embodiment, the temperature of the flame gun 43 is set at around 2800°C, and it is connected to the hydrogen-oxygen cylinder 41 through the first connecting pipe 44 to provide raw materials for the combustion of the flame gun 43.

[0083] Furthermore, the preset temperature is 130-120℃, and the preset time is 1 hour.

[0084] Understandably, this step aims to ensure the environment is as dry as possible, and the high temperature accelerates the movement of gas molecules, making them easier to extract. Simultaneously, the high temperature also facilitates the melting of yellow phosphorus, preparing it for subsequent conversion reactions; preferably, this preset temperature is 110°C.

[0085] The present invention also provides another sealing method, comprising the following steps:

[0086] S210. A sealing device is provided, the sealing device is opened, and the filling bottle 1 of the sealing device contains yellow phosphorus and water;

[0087] S220. Open the inflation assembly 5 and inert gas into the filling bottle 1 through the first connecting neck 11 to expel the air in the filling bottle 1, ensuring that the yellow phosphorus does not come into contact with oxygen and reducing the generation of by-products.

[0088] S230, Open the vacuum assembly 6 and draw air from the filling bottle 1 through the second connecting neck 12;

[0089] This step creates a flowing gas environment, which helps to expel air and other possible gases from the filling bottle 1, creating a near-vacuum environment for subsequent operations.

[0090] S240. Turn on heater 3 to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component.

[0091] This step uses heater 3 to heat the loading bottle 1 to melt the yellow phosphorus, so that the yellow phosphorus reaches the preset state to facilitate the subsequent reaction.

[0092] S250, the vacuum assembly 6 remains open until the air pressure in the filling bottle 1 is 30-100Pa;

[0093] This step aims to bring the filling bottle 1 into a vacuum state, which can effectively remove air and moisture from the bottle, reduce the risk of oxidation reaction, and provide a pure environment for subsequent conversion reactions.

[0094] S260, the heater 3 heats at a preset temperature for a predetermined time and keeps the vacuum component 6 open to remove air and moisture from the filling bottle 1;

[0095] This step ensures the environment is as dry as possible, and the high temperature used accelerates the movement of gas molecules, making them easier to extract. Simultaneously, the high temperature helps maintain the molten state of the yellow phosphorus, preparing it for subsequent conversion reactions.

[0096] S270. Close the vacuum assembly 6 and use the sealing assembly 4 to seal the second connecting neck 12 of the filling bottle 1 to seal the port and prevent outside air from entering.

[0097] S280. Open the gas filling component 5 and introduce a preset amount of inert gas into the filling bottle 1 to form a positive pressure environment, protect the yellow phosphorus from contact with oxygen, and provide a stable reaction condition.

[0098] It should be noted that in this embodiment, the flange and control valve 53 at the connection between the two are closed only after the gas pressure in the filling bottle 1 is restored to atmospheric pressure of 1 atm. Furthermore, the preset capacity of the inert gas is 0.5-8 kg.

[0099] S290. The first connecting neck 11 of the filling bottle 1 is sealed using the sealing assembly 4 to seal the port and prevent outside air from entering.

[0100] It should be noted that, through the above steps, a high-temperature positive pressure environment can be formed in this embodiment. By using a high vacuum environment and high-temperature heating, air and moisture can be eliminated as much as possible, reducing the risk of tube bursting due to moisture. This ensures the safety of operation, reduces the generation of oxidation byproducts, and improves the purity of the final product. In addition, the positive pressure environment formed by high temperature and inert gas can effectively protect yellow phosphorus from contact with oxygen, which helps to promote the conversion reaction of yellow phosphorus to red phosphorus and improve the conversion efficiency.

[0101] In addition, during the sealing process in this embodiment, the temperature of the flame gun 43 is set at around 2800°C, and it is connected to the hydrogen-oxygen cylinder 41 through the first connecting pipe 44 to provide raw materials for the combustion of the flame gun 43.

[0102] Furthermore, the preset temperature is 130-120℃, and the preset time is 1 hour.

[0103] Understandably, this step aims to ensure the environment is as dry as possible, and the high temperature accelerates the movement of gas molecules, making them easier to extract. Simultaneously, the high temperature also facilitates the melting of yellow phosphorus, preparing it for subsequent conversion reactions; preferably, this preset temperature is 110°C.

[0104] Both of the above-mentioned sealing methods, under high-temperature vacuum conditions, provide an ideal chemical environment for the conversion of yellow phosphorus to red phosphorus by eliminating air and moisture, which is beneficial to improving the conversion rate. Under high-temperature positive pressure conditions, maintaining a certain inert gas pressure can further protect yellow phosphorus from oxidation and help maintain the uniformity of the reaction temperature.

[0105] Understandably, both of the above sealing methods, whether in step S110 or step S220, involve opening the gas filling component 5 and filling the filling bottle 1 with inert gas to expel the air inside the filling bottle 1, creating an oxygen-free environment to prevent yellow phosphorus from contacting oxygen and undergoing an oxidation reaction. The yellow phosphorus inside the filling bottle 1 is then melted by the heater 3 to reach a suitable state for conversion.

[0106] Specifically, the inflation assembly 5 is opened to fill the filling bottle 1 with inert gas, and this process is maintained for 4-6 minutes to purge the air from the filling bottle 1. Preferably, the inert gas cylinder 51 is ventilated for 5 minutes during this step.

[0107] It should be noted that steps S110 and S120 can be performed simultaneously or separately. When performed simultaneously, the inert gas cylinder 51 of the filling assembly 5 fills the filling bottle 1 with inert gas (such as nitrogen or argon) through the second connecting pipe 52, while the suction component 61 of the suction assembly 6 extracts gas from the other end through the third connecting pipe 62, forming a flowing gas environment, which helps to quickly remove the air from the bottle. By simultaneously filling with inert gas and performing suction operations, the air in the filling bottle 1 can be effectively removed. The above dynamic gas replacement method is more effective than simply filling or suctioning, and can achieve the required oxygen-free environment more quickly. Similarly, steps S220 and S230 can be performed simultaneously or separately.

[0108] Understandably, in both of the above sealing methods, whether in step S130 or step S240, the yellow phosphorus is heated to a molten state by heater 3. Specifically, in this step, heater 3 is used to heat the filling bottle 1 to 40-60°C. This temperature range is sufficient to melt the yellow phosphorus, but not so high that it would cause other unnecessary reactions.

[0109] Furthermore, the inflation component 5 introduces inert gas into the filling bottle 1 at a flow rate of 2-5 m / s under a working pressure of 5-10 MPa.

[0110] This embodiment utilizes high pressure and high flow rate to rapidly expel air and moisture from the bottle, ensuring a quick transition to an inert gas environment. This rapid air replacement not only helps remove air but also prevents outside air from re-entering the bottle, effectively reducing the chance of yellow phosphorus contacting oxygen, thereby minimizing oxidation and improving the purity of the final product. Both of the above sealing methods can employ the aforementioned flow rate to introduce inert gas.

[0111] In summary, the embodiments of the present invention provide a sealing device and a sealing method. The sealing device is very simple to operate. Through the double-necked structure of the filling bottle 1 and the sealing device, as well as the use of inert gas, air in the filling bottle 1 is effectively discharged, reducing the side reaction between yellow phosphorus and air, lowering the risk of the filling bottle 1 exploding, and enhancing the safety of the entire production process. In addition, the filling and sealing can be completed directly on the sealing device, saving a lot of production time. After sealing, the filling bottle can serve as an independent conversion bottle, which can be used to produce various allotropic phosphorus using yellow phosphorus as raw material. The integrated sealing device has high process flexibility and is more convenient for operators to use.

[0112] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and substitutions can be made without departing from the technical principles of the present invention, and these improvements and substitutions should also be considered within the scope of protection of the present invention.

Claims

1. A sealing tube device, characterized in that, The device includes a filling bottle with a first connecting neck and a second connecting neck, a quartz retaining sleeve, a heater, a sealing assembly for sealing the first connecting neck and the second connecting neck, an inflation assembly for providing inert gas, a vacuum assembly, and a control unit. The quartz retaining sleeve is installed inside the heater, and the filling bottle is installed inside the quartz retaining sleeve. The inflation assembly is detachably connected to the first connecting neck and is used to introduce inert gas into the filling bottle. The vacuum assembly is detachably connected to the second connecting neck and is used to perform a vacuuming operation into the filling bottle. The control unit is electrically connected to the heater, the sealing assembly, and the vacuum assembly, respectively.

2. The sealing device according to claim 1, characterized in that, The filling bottle is used to hold yellow phosphorus.

3. The sealing device according to claim 2, characterized in that, At the start of the sealing operation, the inflation assembly is configured to inflate the filling bottle with inert gas through the first connecting neck, the evacuation assembly is configured to evacuate gas from the filling bottle through the second connecting neck, and the heater is configured to heat the yellow phosphorus. After the yellow phosphorus is heated to a molten state, the gas filling component is configured to be closed, the gas extraction component is configured to remain open, the tube sealing component is configured to seal the first connecting neck, and the gas extraction component is configured to remain open until the gas pressure inside the filling bottle is 30-100 Pa. After the air pressure inside the filling bottle reaches 30-100Pa and the first connecting neck is sealed, the vacuum assembly is configured to remain open, and the heater is configured to heat at a preset temperature for a predetermined time. After the heater heats at a preset temperature for a predetermined time, the air extraction assembly is configured to be in a closed state, and the sealing assembly is configured to seal the second connecting neck.

4. The sealing device according to claim 2, characterized in that, At the start of the sealing operation, the inflation assembly is configured to inflate the filling bottle with inert gas through the first connecting neck, the evacuation assembly is configured to evacuate gas from the filling bottle through the second connecting neck, and the heater is configured to heat the yellow phosphorus. After the yellow phosphorus is heated to a molten state, the gas filling component is configured to be closed, and the gas extraction component is configured to remain open until the gas pressure inside the filling bottle is 30-100 Pa. After the air pressure inside the filling bottle reaches 30-100 Pa, the vacuum assembly is configured to remain on, and the heater is configured to heat at a preset temperature for a predetermined time. After the heater heats at a preset temperature for a predetermined time, the air extraction assembly is configured to be in a closed state, and the sealing assembly is configured to seal the second connecting neck. After the second connecting neck is sealed, the inflation assembly is configured to be open and fills the filling bottle with a preset capacity of inert gas. After the filling bottle is filled with a preset amount of inert gas, the sealing assembly is configured to seal the first connecting neck of the filling bottle.

5. The sealing device according to claim 1, characterized in that, The sealing assembly includes an oxygen-hydrogen cylinder, a mobile platform, a flame gun, and a first connecting pipe. The oxygen-hydrogen cylinder is connected to the flame gun through the first connecting pipe. The flame gun is mounted on the mobile platform and is electrically connected to the control unit.

6. The sealing device according to claim 5, characterized in that, The mobile platform includes a base plate and pulleys. The flamethrower is mounted on the base plate, and the pulleys are mounted on the side of the base plate opposite to the flamethrower.

7. The sealing tube device according to claim 1, characterized in that, The inflation assembly includes an inert gas cylinder, a second connecting pipe, and a control valve. The inert gas cylinder is detachably connected to the first connecting neck via the second connecting pipe, and the control valve is installed on the second connecting pipe.

8. The sealing device according to claim 7, characterized in that, The inflation assembly also includes a flow rate sensor, which is installed on the second connecting pipe and located between the inert gas cylinder and the control valve. The flow rate sensor is electrically connected to the control unit.

9. The sealing device according to claim 1, characterized in that, It also includes a support assembly, on which the air extraction assembly is slidably mounted to move up and down relative to the support assembly.

10. The sealing device according to claim 9, characterized in that, The support assembly comprises a magnetic bearing, a support member, and a drive member. The support member is slidably connected to the air extraction assembly, and the support member and the air extraction assembly are connected through the magnetic bearing. The drive member is used to control the magnetic bearing to drive the air extraction assembly to perform lifting and lowering movements.

11. The sealing device according to claim 1, characterized in that, The air extraction assembly includes an air extraction component, a third connecting pipe, and a pressure gauge. The air extraction component is detachably connected to the second connecting neck through the third connecting pipe. The pressure gauge is installed on the third connecting pipe. The air extraction component and the pressure gauge are electrically connected to the control unit, respectively.

12. The sealing device according to claim 1, characterized in that, A flange is provided at the connection between the inflation assembly and the first connecting neck, and a flange is provided at the connection between the air extraction assembly and the second connecting neck.

13. A method for sealing a tube, characterized in that, Includes the following steps: A sealing device as described in any one of claims 1-2 is provided, wherein the sealing device is opened, and the filling bottle of the sealing device contains yellow phosphorus and water; Open the inflation assembly and fill the filling bottle with inert gas through the first connecting neck; Open the vacuum assembly and evacuate air from the filling bottle through the second connecting neck; Turn on the heater to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component; The sealing assembly is used to seal the first connecting neck of the filling bottle; The vacuum assembly is kept open until the air pressure inside the filling bottle is 30-100 Pa. The heater heats at a preset temperature for a predetermined time and keeps the vacuum assembly open to expel air and moisture from the filling bottle; The sealing assembly is used to seal the second connecting neck of the filling bottle.

14. The sealing method according to claim 13, characterized in that, The preset temperature is 110-130℃, and the preset time is 1 hour.

15. A method for sealing a tube, characterized in that, Includes the following steps: A sealing device as described in any one of claims 1-12 is provided, wherein the sealing device is opened, and the filling bottle of the sealing device contains yellow phosphorus and water; Open the inflation assembly and fill the filling bottle with inert gas through the first connecting neck; Open the vacuum assembly and evacuate air from the filling bottle through the second connecting neck; Turn on the heater to heat the yellow phosphorus until it is completely melted, then turn off the gas filling component; The vacuum assembly is kept open until the air pressure in the filling bottle is 30-100 Pa; The heater heats at a preset temperature for a predetermined time and keeps the vacuum assembly open to expel air and moisture from the filling bottle; The vacuum assembly is closed, and the second connecting neck of the filling bottle is sealed using the sealing assembly. Open the inflation assembly and introduce a preset volume of inert gas into the filling bottle; The sealing assembly is used to seal the first connecting neck of the filling bottle.

16. The sealing method according to claim 15, characterized in that, The preset temperature is 110-130℃, and the preset time is 1 hour.

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