Boron trifluoride gas experiment device
By designing a boron trifluoride gas experimental device including a reactor, a condenser and a multi-stage purification tower, the problems of low reaction efficiency and safety and poor purification effect in the existing devices are solved, and the preparation and purification of high-purity boron trifluoride gas is achieved.
Patent Information
- Application Number
- CN202421370015.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-17
- Publication Date
- 2025-03-21
- Estimated Expiration
- 2034-06-17
AI Technical Summary
During the preparation and purification process of the existing boron trifluoride gas experimental equipment, there are problems such as unreasonable reaction kettle design, low reaction efficiency and safety, difficulty in meeting the high purity needs of purification equipment, and material selection affects gas purity and activity.
A boron trifluoride gas experimental device including a reactor, a condenser, a multi-stage purification tower and a gas buffer tank was designed. By setting a reducer, a stirring paddle and an insulation layer in the reactor, a three-stage purification tower and a tetrafluorosphere are used for purification, and the high purity of the gas is ensured through a multi-stage purification system.
The reaction efficiency and safety are improved, the purity of boron trifluoride gas is significantly improved, the preparation needs of high purity is met, and the strength and corrosion resistance of the equipment are improved through the preferred materials.
Smart Images
Figure CN222642029U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of experimental equipment, in particular to a boron trifluoride gas experimental device. Background Art
[0002] With the rapid development of the chemical industry, boron trifluoride, as an important inorganic compound, plays a vital role in organic synthesis, catalyst preparation, and high-energy fuel manufacturing. Its unique chemical properties make boron trifluoride an indispensable catalyst in industries such as medicine, pesticides, dyes, and fine chemicals. Therefore, the preparation of high-purity and high-activity boron trifluoride gas has become an important topic in chemical research.
[0003] At present, the preparation methods of boron trifluoride mainly include high-temperature thermal decomposition of fluoroborate, concentrated sulfuric acid co-heating method and direct fluorination method. Among them, the direct fluorination method has become the main method of industrial production due to its advantages such as low reaction temperature, high safety and less waste liquid. This method is to mix boric acid and fuming sulfuric acid and then introduce hydrogen fluoride gas. The boron trifluoride gas generated by the reaction needs to go through a series of purification steps, such as removing impurities through purification equipment such as a scrubber, to obtain high-purity boron trifluoride gas.
[0004] However, there are some problems in the preparation and purification process of the existing boron trifluoride gas experimental device. First, the design of the reactor is not reasonable enough, resulting in low reaction efficiency and safety. Secondly, the purification equipment can usually only remove some impurities, which is difficult to meet the preparation needs of high-purity boron trifluoride gas. In addition, the material selection of the experimental device may also affect the purity and activity of boron trifluoride gas. Utility Model Content
[0005] The purpose of the utility model is to provide a boron trifluoride gas experimental device to solve the problems that the design of the reactor proposed in the above background technology is not reasonable, resulting in low reaction efficiency and safety, the purification equipment can usually only remove part of the impurities, it is difficult to meet the preparation needs of high-purity boron trifluoride gas, and the material selection of the experimental device may also affect the purity and activity of the boron trifluoride gas.
[0006] To achieve the above-mentioned purpose, the utility model provides a boron trifluoride gas experimental device, including a reactor, a condenser, a first purification tower, a second purification tower, a third purification tower and a gas buffer tank, wherein the reactor, the condenser, the first purification tower, the second purification tower, the third purification tower and the gas buffer tank are connected in sequence through a gas pipeline, the reactor is composed of a reducer, a stirring paddle, a kettle cover and a kettle body, a cavity is arranged inside the kettle body, a jacket is arranged outside the cavity, an insulation layer is arranged on the outer wall of the jacket, and a gas inlet and outlet are arranged at the very end of the gas pipeline on the top side of the gas buffer tank.
[0007] Preferably, a valve is provided on the gas pipeline.
[0008] Preferably, the kettle cover is provided with a pressure gauge, a thermometer, a solid feed port and a liquid feed pipe. The solid feed port of the reactor is a sloped wide mouth for easy solid feeding, and the liquid feed pipe is inserted into the bottom of the cavity.
[0009] Preferably, the jacket is provided with a cold and hot medium outlet and a cold and hot medium inlet, and the condenser is provided with a refrigerant inlet and a refrigerant outlet.
[0010] Preferably, a first discharge port is provided at the bottom of the kettle body, the first discharge port is connected with the cavity after passing through the insulation layer and the jacket, and a downward-expanding discharge valve is provided on the first discharge port.
[0011] Preferably, a second discharge port is provided at the bottom of the first purification tower, a third discharge port is provided at the bottom of the second purification tower, a fourth discharge port is provided at the bottom of the third purification tower, and a fifth discharge port is provided at the bottom of the gas buffer tank. The first purification tower, the second purification tower and the third purification tower are all filled with polytetrafluoroethylene balls with a diameter of 0.5mm-5mm.
[0012] Preferably, the reactor, condenser, first purification tower, second purification tower, third purification tower and gas buffer tank are fixed by a load-bearing bracket through a fixing arm and fixing bolts, and a base is installed at the bottom of the load-bearing bracket.
[0013] Preferably, the overall material of the boron trifluoride gas experimental device is carbon steel, 316L stainless steel, Hastelloy, Monel alloy or nickel-copper alloy.
[0014] Compared with the prior art, the utility model has the following beneficial effects:
[0015] 1. In the boron trifluoride gas experimental device, the jacket and insulation layer design of the reactor make the temperature control during the reaction process more accurate and stable, thereby improving the reaction efficiency. At the same time, the setting of the stirring paddle ensures that the reactants are mixed evenly, further improving the reaction speed and efficiency. Through the design of the three-stage purification tower, combined with the loaded tetrafluoroethylene balls with a diameter of 0.5mm-5mm, impurities and particulate matter in the boron trifluoride gas are effectively removed, significantly improving the purity of the gas. The multi-stage purification system ensures that the boron trifluoride gas finally obtained meets the high purity requirements.
[0016] 2. In the boron trifluoride gas experimental device, the whole set of equipment is fixed by bolts, and no further assembly is required during the experiment after installation, thereby achieving convenient feeding, good air tightness, and the function of purifying the boron trifluoride gas generated by the reaction.
[0017] 3. In the boron trifluoride gas experimental device, a liquid feeding pipe is provided on the kettle cover, and the liquid feeding pipe is inserted into the bottom of the reactor cavity, so that the liquid hydrogen fluoride can fully contact with the reaction liquid after entering the reactor, and the reaction is more complete. The condenser is provided with a refrigerant inlet and a refrigerant outlet. Through the condensation effect of the low-temperature refrigerant enhancing condenser, the unreacted hydrogen fluoride is condensed and refluxed into the reactor to continue the reaction. Three purification towers are provided, and the purification towers are filled with tetrafluoro balls with a diameter of 0.5mm to 5mm to purify the generated boron trifluoride gas, reduce impurities, and improve the purity of the boron trifluoride gas. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 It is a schematic diagram of the overall structure of the utility model;
[0019] Figure 2 It is a partial structural schematic diagram of the utility model.
[0020] The meaning of each number in the figure is:
[0021] 1. Reactor; 2. Condenser; 3. First purification tower; 4. Second purification tower; 5. Third purification tower; 6. Gas buffer tank; 7. Gas pipeline; 8. Valve; 9. Reducer; 10. Agitator; 11. Kettle cover; 12. Kettle body; 13. Pressure gauge; 14. Thermometer; 15. Solid feed port; 16. Liquid feed pipe; 17. Cavity; 18. Jacket; 19. Cold and hot medium outlet; 20. Cold and hot medium inlet; 21. Insulation layer; 22. First discharge port; 23. Refrigerant inlet; 24. Refrigerant outlet; 25. Second discharge port; 26. Third discharge port; 27. Fourth discharge port; 28. Fifth discharge port; 29. Load-bearing bracket; 30. Fixed arm; 31. Fixing bolt; 32. Base; 33. Gas inlet and outlet. DETAILED DESCRIPTION
[0022] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0023] The utility model provides a boron trifluoride gas experimental device, such as Figure 1-Figure 2As shown, it includes a reactor 1, a condenser 2, a first purification tower 3, a second purification tower 4, a third purification tower 5 and a gas buffer tank 6. The reactor 1, the condenser 2, the first purification tower 3, the second purification tower 4, the third purification tower 5 and the gas buffer tank 6 are connected in sequence through a gas pipeline 7. The reactor 1 is composed of a reducer 9, a stirring paddle 10, a reactor cover 11 and a reactor body 12. The interior of the reactor body 12 is provided with a cavity 17, the exterior of the cavity 17 is provided with a jacket 18, and the outer wall of the jacket 18 is provided with an insulation layer 21. A gas inlet and outlet 33 is provided at the end of the gas pipeline 7 on the top side of the gas buffer tank 6. When in use, nitrogen is flushed into the entire device system through the gas pipeline to check the airtightness of the entire device. After the airtightness is confirmed, the valve is opened to release the pressure, and then the reactor is cooled and cooled. The liquid feeding pipe of the reactor adds fuming sulfuric acid into the cavity, closes the liquid feeding pipe, starts stirring the reactor, and then circulates the cold and hot media in the reactor jacket through the cold and hot media inlet and outlet of the reactor, controls the temperature of the liquid in the reactor cavity to the process temperature, and then adds boric acid into the cavity through the solid feeding port of the reactor, closes the solid feeding port, and then slowly adds hydrogen fluoride into the cavity through the liquid feeding pipe, controls the temperature of the liquid in the reactor cavity to the process temperature by controlling the temperature of the cold and hot media in the reactor jacket, realizes the boron trifluoride gas generation reaction in the reactor cavity, and the boron trifluoride gas generated by the reaction is cooled by the condenser and purified by the purification tower before entering the buffer tank, and the gas in the buffer tank can be passed into the boron trifluoride gas storage tank or into the organic solvent for complexation as needed. The device is convenient for feeding, has good air tightness, and can purify the boron trifluoride gas generated by the reaction.
[0024] In this embodiment, a valve 8 is provided on the gas pipeline 7 .
[0025] Specifically, the reactor cover 11 is provided with a pressure gauge 13, a thermometer 14, a solid feed port 15, and a liquid feed pipe 16. The solid feed port 15 of the reactor 1 is a sloped wide mouth, which is convenient for solid feeding. The liquid feed pipe 16 is inserted into the bottom of the cavity 17 to ensure accurate material feeding.
[0026] Furthermore, the jacket 18 is provided with a cold and hot medium outlet 19 and a cold and hot medium inlet 20 for the entry and discharge of the cold and hot medium, and the condenser 2 is provided with a refrigerant inlet 23 and a refrigerant outlet 24 for the entry and discharge of the refrigerant.
[0027] Furthermore, a first discharge port 22 is provided at the bottom of the kettle body 12. The first discharge port 22 is connected to the cavity 17 after passing through the insulation layer 21 and the jacket 18. A downward-expanding discharge valve is provided on the first discharge port 22 to facilitate the switching of the discharge.
[0028] Furthermore, a second discharge port 25 is provided at the bottom of the first purification tower 3, a third discharge port 26 is provided at the bottom of the second purification tower 4, a fourth discharge port 27 is provided at the bottom of the third purification tower 5, and a fifth discharge port 28 is provided at the bottom of the gas buffer tank 6. The first purification tower 3, the second purification tower 4, and the third purification tower 5 are all filled with polytetrafluoroethylene balls with a diameter of 0.5mm-5mm.
[0029] Furthermore, the reactor 1, the condenser 2, the first purification tower 3, the second purification tower 4, the third purification tower 5 and the gas buffer tank 6 are fixed by the load-bearing bracket 29 through the fixed arm 30 and the fixing bolt 31, and a base 32 is installed at the bottom of the load-bearing bracket 29 to ensure the overall support stability of the equipment.
[0030] Furthermore, the overall material of the boron trifluoride gas experimental device is carbon steel, 316L stainless steel, Hastelloy, Monel alloy or nickel-copper alloy. In this embodiment, 316L stainless steel is preferred to ensure good strength and anti-corrosion properties.
[0031] When the boron trifluoride gas experimental device of the utility model is used, first confirm whether the tetrafluoro balls in the first purification tower 3, the second purification tower 4, and the third purification tower 5 are completely filled, and close the discharge port of the purification tower; then check the airtightness of the device, close the solid feeding port 15, the liquid feeding pipe 16 and the discharge ports on all equipment, open all valves 8 on the gas pipeline 7, and flush nitrogen into the device through the gas inlet and outlet 33 to maintain the pressure in the device at 0.05-0.10MPa, close the nitrogen valve, observe the changes in the pressure gauge, and confirm that the airtightness is intact if there is no pressure change after 0.5-1 hour; after the airtightness is confirmed, open the gas inlet and outlet 33 to release the pressure, and after the pressure release is completed, open the liquid feeding pipe 16 of the reactor 1, add oleum into the reactor cavity, and after the feeding is completed, close the liquid feeding pipe; connect the cold and hot medium to the cold and hot medium inlet 19 and the cold and hot medium outlet 20 on the reactor 1, open The cold and hot media circulate, start the reactor stirring, and control the liquid in the reactor cavity at a suitable temperature; open the solid feeding port 15, add the solid raw material boric acid into the reactor cavity, and after the addition is completed, close the solid feeding port valve; continue stirring, and control the liquid in the reactor cavity at a suitable temperature; connect the refrigerant to the refrigerant inlet 23 and the refrigerant outlet 24 of the condenser 2, start the refrigerant circulation, and control the inside of the condenser at a suitable temperature; open the liquid feeding pipe, and slowly add hydrogen fluoride into the reactor cavity through a peristaltic pump or a feeding pump to start the reaction. After the feeding is completed, close the liquid feeding pipe and continue stirring the reaction; the boron trifluoride gas generated by the reaction is cooled by the condenser 2, purified by the first purification tower 3, the second purification tower 4, and the third purification tower 5, and then enters the buffer tank 6, and then by controlling the gas inlet and outlet 33, according to research needs, the prepared boron trifluoride gas is passed into the boron trifluoride gas storage tank or the complex solvent.
[0032] The above shows and describes the basic principle, main features and advantages of the utility model. Those skilled in the art should understand that the utility model is not limited by the above embodiments. The above embodiments and descriptions are only preferred examples of the utility model and are not used to limit the utility model. Without departing from the spirit and scope of the utility model, the utility model may have various changes and improvements, which fall within the scope of the utility model to be protected. The scope of protection of the utility model is defined by the attached claims and their equivalents.
Claims
1. A boron trifluoride gas experimental device, characterized in that: The invention comprises a reactor (1), a condenser (2), a first purification tower (3), a second purification tower (4), a third purification tower (5) and a gas buffer tank (6); the reactor (1), the condenser (2), the first purification tower (3), the second purification tower (4), the third purification tower (5) and the gas buffer tank (6) are connected in sequence through a gas pipeline (7); the reactor (1) comprises a reducer (9), a stirring paddle (10), a reactor cover (11) and a reactor body (12); a cavity (17) is arranged inside the reactor body (12); a jacket (18) is arranged outside the cavity (17); an insulating layer (21) is arranged on the outer wall of the jacket (18); and a gas inlet and outlet (33) is arranged at the end of the gas pipeline (7) on one side of the top of the gas buffer tank (6).
2. The boron trifluoride gas experimental device according to claim 1, characterized in that: The gas pipeline (7) is provided with a valve (8).
3. The boron trifluoride gas experimental device according to claim 1, characterized in that: The kettle cover (11) is provided with a pressure gauge (13), a thermometer (14), a solid feeding port (15), and a liquid feeding pipe (16). The solid feeding port (15) of the reactor (1) is a sloped wide opening for facilitating solid feeding. The liquid feeding pipe (16) is inserted into the bottom of the cavity (17).
4. The boron trifluoride gas experimental device according to claim 1, characterized in that: The jacket (18) is provided with a cold and hot medium outlet (19) and a cold and hot medium inlet (20), and the condenser (2) is provided with a refrigerant inlet (23) and a refrigerant outlet (24).
5. The boron trifluoride gas experimental device according to claim 1, characterized in that: A first discharge port (22) is provided at the bottom of the kettle body (12). The first discharge port (22) is connected to the cavity (17) after passing through the insulation layer (21) and the jacket (18). A downward-expanding discharge valve is provided on the first discharge port (22).
6. The boron trifluoride gas experimental device according to claim 1, characterized in that: The first purification tower (3) is provided with a second discharge port (25) at the bottom, the second purification tower (4) is provided with a third discharge port (26) at the bottom, the third purification tower (5) is provided with a fourth discharge port (27) at the bottom, and the gas buffer tank (6) is provided with a fifth discharge port (28) at the bottom. The first purification tower (3), the second purification tower (4) and the third purification tower (5) are all filled with polytetrafluoroethylene balls with a diameter of 0.5 mm to 5 mm.
7. The boron trifluoride gas experimental device according to claim 1, characterized in that: The reactor (1), the condenser (2), the first purification tower (3), the second purification tower (4), the third purification tower (5) and the gas buffer tank (6) are fixed by a load-bearing bracket (29) through a fixing arm (30) and fixing bolts (31), and a base (32) is installed at the bottom of the load-bearing bracket (29).
8. The boron trifluoride gas experimental device according to claim 1, characterized in that: The overall material of the boron trifluoride gas experimental device is carbon steel, 316L stainless steel, Hastelloy, Monel alloy or nickel-copper alloy.