Method and equipment for purifying diborane

Abstract

The invention relates to a diborane purification method and equipment, and relates to the technical field of diborane preparation, and the method comprises the following steps: S1, preparing crude diborane, S2, carrying out low-temperature pressurized distillation, S3, carrying out multi-stage purification treatment, S4, carrying out gas-solid separation, S5, carrying out inert gas purging, and S6, carrying out continuous rectification and adsorption combined purification. By adopting the technical scheme, impurities in the diborane can be effectively removed, the purity and the stability of the diborane are improved, and the requirements of high-requirement applications such as the semiconductor industry are met.

Description

Technical Field

[0001] The present application relates to the technical field of diborane preparation, and in particular to a diborane purification method and equipment. Background Art

[0002] Diborane is a colorless gas with a special odor and active chemical properties. It is used in the electronics industry as a gaseous impurity source, ion implantation, and a dopant for boron doping oxidation diffusion. It is mainly used in the production of P-type semiconductor chips.

[0003] In the related art, reference may be made to the Chinese invention patent with the authorization announcement number CN113120862A, which discloses a method for continuously producing high-purity diborane. First, materials are added to a reaction kettle for reaction, then the reaction materials are transferred to a purification kettle and diborane is collected in a collector, and then the diborane is distilled.

[0004] However, when preparing diborane, the temperature of the reactor needs to be constantly changed, and boron trichloride / boron trifluoride gas is added at a uniform rate at different temperatures, so that the staff needs to control the temperature of the reactor at all times, which places high operational requirements on the staff and has a high work intensity. Summary of the invention

[0005] In order to reduce the operational difficulty during the preparation of diborane, the present application provides a diborane purification method and equipment.

[0006] The present application provides a diborane purification method, which adopts the following technical scheme:

[0007] A method for purifying diborane, comprising:

[0008] S1. Preparation of crude diborane: sodium hydride is used as a starting material in a reactor, nitrogen is introduced to replace the air in the reactor, tetrahydrofuran is added, the mineral oil in the sodium hydride is cleaned, twice in total, trimethyl borate is added dropwise to the sodium hydride tetrahydrofuran mixture, the temperature is controlled to 68° C., a condensation reaction occurs, the fraction is condensed and all refluxed into the reactor, and the temperature is kept for 5 hours to obtain sodium trimethoxyborohydride, excess trimethyl borate is distilled off, boron trichloride tetrahydrofuran solution is added to the sodium trimethoxyborohydride tetrahydrofuran solution, the temperature is controlled, a double decomposition reaction occurs, and the reaction time is 5 to 10 hours to obtain crude diborane;

[0009] S2. Low temperature pressure distillation: A packed tower filled with adsorbent is used to purify crude diborane containing low-boiling point and high-boiling point impurities by low temperature pressure distillation. The adsorbent is usually zeolite molecular sieve. The temperature of the reboiler is controlled between -90°C and -20°C. The pressure of the distillation system is 0.01MPa to 1.5MPa.

[0010] S3, multi-stage purification treatment: using potassium borohydride to perform preliminary purification treatment at 20-40°C to obtain a first treated gas, further purifying the first treated gas using sodium hydroxide at 15-30°C to obtain a second treated gas, and adsorbing the second treated gas using 13X molecular sieve at -40 to -20°C to obtain a third treated gas;

[0011] S4, gas-solid separation: performing gas-solid separation on the third treated gas at a temperature lower than the solidification point of diborane to obtain solid diborane;

[0012] S5. Inert gas purging: In the method using excess diborane, the obtained product is purged with an inert gas (such as nitrogen or argon) to remove excess diborane;

[0013] S6. Combined purification by continuous distillation and adsorption: The continuous distillation method and the combined adsorption purification method are used to remove low-boiling point and high-boiling point impurities through reboilers, packed towers, condensers and other equipment to improve the purity of diborane.

[0014] By adopting the above technical solution, impurities in diborane can be effectively removed, its purity and stability can be improved, and the needs of high-demand applications such as the semiconductor industry can be met.

[0015] The second object of the present application is to provide an apparatus, comprising a kettle body and an electric heating tube arranged on the kettle body, wherein the kettle body is provided with a temperature regulating device for regulating the temperature in the kettle body, and the temperature regulating device comprises:

[0016] A heat dissipation pipe, which is arranged on the kettle body and is provided with a fan, and is used to discharge the hot air in the kettle body;

[0017] A switch plate, the switch plate is horizontally slidably arranged on the kettle body, and the switch plate is located at the connection between the heat dissipation pipe and the kettle body;

[0018] A moving mechanism, which is arranged on the kettle body and is used to control the movement of the switch plate;

[0019] The temperature sensor is arranged in the kettle body and is electrically connected to the moving mechanism.

[0020] By adopting the above technical scheme, the temperature sensor senses the working environment temperature in the kettle. When the temperature sensed by the temperature sensor is too high, the moving mechanism drives the switch plate to open the heat dissipation pipe, and the heat dissipation pipe dissipates heat and cools the inside of the kettle. When the temperature in the kettle is low, the moving mechanism drives the switch plate to close the heat dissipation pipe, so that the inside of the kettle is heated up under the action of the electric heating pipe, thereby completing the automatic temperature adjustment work inside the kettle, ensuring the stable and uniform temperature inside the kettle, without the need for manual real-time monitoring and adjustment, reducing work intensity and improving work efficiency.

[0021] Optionally, the moving mechanism includes:

[0022] A movable slide rail, wherein the movable slide rail is arranged on the kettle body, and the switch plate is slidably arranged on the movable slide rail;

[0023] A moving block, which is horizontally slidably arranged on the kettle body and connected to the switch plate;

[0024] A moving screw, which is rotatably disposed on the kettle body and is threadably connected to the moving block;

[0025] A transmission component is arranged on the kettle body, and receives the temperature signal of the temperature sensor and controls the moving screw to rotate.

[0026] By adopting the above technical solution, the transmission component receives the temperature signal sensed by the temperature sensor, and then controls the rotation of the moving screw through the temperature signal. The rotation of the moving screw drives the moving block to move, and the movement of the moving block drives the switch plate to slide on the moving slide rail, thereby realizing the movement of the switch plate.

[0027] Optionally, the transmission assembly includes:

[0028] A transmission motor, wherein the transmission motor is arranged on the kettle body and the output shaft is connected to the moving screw;

[0029] A temperature control meter, which is arranged on the kettle body and is electrically connected to the temperature sensor;

[0030] A high temperature relay and a high temperature travel switch, wherein the high temperature relay and the high temperature travel switch are both arranged on the kettle body and are electrically connected to the temperature control meter and the positive rotation electrode of the transmission motor;

[0031] A low temperature relay and a low temperature travel switch are both arranged on the kettle body and are electrically connected to the temperature control meter and the reverse electrode of the transmission motor.

[0032] By adopting the above technical solution, the temperature sensor is electrically connected to the temperature control meter, and the temperature control meter is divided into two branches: one branch is connected in series with the high temperature relay, the high temperature travel switch and the positive electrode of the transmission motor; the other branch is connected in series with the low temperature relay, the low temperature travel switch and the reverse electrode of the transmission motor. The temperature control meter can set the highest temperature point G and the lowest temperature point D. The temperature control meter automatically controls whether to connect to the high temperature relay or the low temperature relay according to the temperature value of the temperature sensor, which is greater than or equal to G, less than G and greater than D, and less than or equal to D. The switches of the temperature control meter, the high temperature relay and the low temperature relay are linked, and the working states of the two relays are mutually reversed, that is, when the temperature control meter is connected to the high temperature relay, the switch of the high temperature relay is closed, and the switch of the low temperature relay is open; conversely, when the temperature control meter is connected to the low temperature relay, the switch of the high temperature relay is open, and the switch of the low temperature relay is closed. When the temperature measured by the temperature sensor is less than or equal to D, the temperature control meter is connected to the low temperature relay, and the transmission motor rotates forward; when the measured temperature is less than G and greater than D, the temperature control meter disconnects the relay, and the transmission motor does not work; when the temperature is greater than or equal to G, the temperature control meter is connected to the high temperature relay, and the transmission motor reverses. The opening and closing of the heat dissipation pipe is controlled by the switch board through the forward and reverse rotation of the transmission motor, thereby adjusting the temperature in the kettle.

[0033] Optionally, a heating switch is provided on the kettle body, and the heating switch is electrically connected to the motor heat pipe. When the switch plate closes the heat pipe, the switch plate and the contacts of the heating switch are in contact, and the heating switch controls the electric heating pipe to be energized.

[0034] By adopting the above technical solution, a heating switch for controlling the operation of the electric heating tube is installed on the kettle body. When the switch board opens the heat dissipation tube for heat dissipation, the electric heating tube will also be automatically powered off synchronously, thereby accelerating the cooling speed and improving the heat dissipation efficiency.

[0035] Optionally, a first gear is provided on the output shaft of the transmission motor, a second gear is rotatably provided on the kettle body, the second gear is meshed with the first gear, a transmission wheel is provided on the movable screw, a key shaft is slidably provided on the second gear, a connecting groove is provided on the transmission wheel, the key shaft is plugged into the connecting groove, a limiting component is provided on the second gear, the limiting component limits the sliding position of the key shaft, and a manual rotation component is provided on the kettle body, and the manual rotation component is used to control the rotation of the transmission wheel.

[0036] By adopting the above technical solution, under normal circumstances, the transmission motor starts and drives the first gear to rotate, the rotation of the first gear drives the second gear to rotate, the rotation of the second gear drives the transmission wheel to rotate through the key shaft, the rotation of the transmission wheel drives the moving screw to rotate, and the rotation of the moving screw drives the switch plate to move; when the transmission motor fails or the power is cut off, the limit assembly is unlocked to disengage the key shaft from the transmission wheel, and then the manual rotation assembly is used to control the rotation of the transmission wheel to realize manual control of the switch plate position, which is convenient for operation in emergency conditions.

[0037] Optionally, the limiting component includes:

[0038] A limit block, wherein a sliding groove for horizontal sliding of the key shaft is provided on the second gear, a limit groove is provided on the inner side wall of the sliding groove along the radial direction of the second gear, and the limit block is slidably mounted on the limit groove;

[0039] A limit spring, wherein the limit spring is arranged on the bottom wall of the limit groove and connected to the limit block, a clamping groove is provided on the side wall of the key shaft, and the limit block partially passes out of the limit groove under the action of the limit spring and is clamped and matched with the clamping groove;

[0040] A first moving block, wherein the first moving block is arranged on the limiting block;

[0041] A second moving block, the second moving block is horizontally slidably arranged on the second gear and contacts the first moving block, a side wall of the first moving block and the second moving block contacting each other is arranged in an inclined state, and the first moving block is compressed by the limit spring and moves under the action of the second moving block;

[0042] A push rod, one end of which is arranged on the second moving block, and the other end of which extends out of the kettle body.

[0043] By adopting the above technical scheme, when the key shaft is plugged into the connecting groove, the limit block compresses the limit spring and is located in the limit groove as a whole; when the movable key shaft is disengaged from the connecting groove, the key shaft moves into the sliding groove, and the engaging groove on the key shaft is connected with the limit groove. Then, under the action of the limit spring, the limit block partially passes through the outside of the limit groove and engages with the engaging groove, thereby limiting the position of the key shaft; when the key shaft needs to be moved out, the push rod is pushed to drive the second moving block to move, and the movement of the second moving block pushes the first moving block to compress the limit spring to move, and the movement of the first moving block drives the limit block to move into the limit groove as a whole, which is convenient and quick.

[0044] Optionally, a movable spring is provided on the bottom wall of the sliding groove, and the movable spring is connected to the key shaft. Under the action of the movable spring, the head of the key shaft passes through the sliding groove and is plugged into the connecting groove. A pull rod is provided on the key shaft, and the end of the pull rod away from the key shaft extends out of the kettle body.

[0045] By adopting the above technical solution, under normal circumstances, the head of the key shaft passes through the sliding groove under the action of the moving spring and is plugged into the connecting groove, thereby reducing the probability of the key shaft and the transmission wheel being disengaged during the rotation of the second gear and the transmission wheel, and ensuring the stability of the transmission effect. When it is necessary to move the key shaft to disengage from the transmission wheel, just pull the pull rod, which is convenient and quick with high work efficiency.

[0046] Optionally, the manual rotation assembly includes:

[0047] A hand wheel, the hand wheel being rotatably arranged on the kettle body;

[0048] A rotating wheel, the rotating wheel is coaxially rotatable with the hand wheel, and the rotating wheel is located in the kettle body;

[0049] A transmission belt is sleeved on the rotating wheel and the transmission wheel.

[0050] By adopting the above technical solution, when the key shaft is disengaged from the transmission wheel, the handwheel is turned, the rotation of the handwheel drives the rotating wheel to rotate, the rotation of the rotating wheel drives the transmission belt to rotate, the rotation of the transmission belt drives the transmission wheel to rotate, the rotation of the transmission wheel drives the moving screw to rotate, and the rotation of the moving screw drives the switch plate to move, thereby realizing the manual control of the movement of the switch plate by turning the handwheel.

[0051] Optionally, an arc-shaped guide surface is provided on a side wall of one end of the limiting block that passes through the limiting groove and is close to the opening of the sliding groove.

[0052] By adopting the above technical solution, an arc-shaped guide surface is provided on the side wall of one end of the limit block passing through the limit groove near the opening of the sliding groove, so that when the pull rod is pulled to drive the key shaft to move into the sliding groove, the key shaft will first contact the guide surface, and the guide surface will generate a component force to drive the limit block to move into the limit groove, thereby eliminating the need to manually push the push rod to drive the limit block into the limit groove, thereby simplifying the working steps and improving work efficiency.

[0053] In summary, the present application includes at least one of the following beneficial technical effects:

[0054] 1. The working environment temperature in the kettle is sensed by the temperature sensor. When the temperature sensed by the temperature sensor is too high, the moving mechanism drives the switch plate to open the heat dissipation pipe, and the heat dissipation pipe dissipates heat and cools the inside of the kettle. When the temperature in the kettle is low, the moving mechanism drives the switch plate to close the heat dissipation pipe, so that the inside of the kettle is heated up under the action of the electric heating pipe, thereby completing the automatic temperature adjustment work inside the kettle, ensuring the stable and uniform temperature inside the kettle, without manual real-time monitoring and adjustment, reducing work intensity and improving work efficiency;

[0055] 2. By installing a heating switch on the kettle body to control the operation of the electric heating tube, when the switch board opens the heat dissipation tube for heat dissipation, the electric heating tube will also be automatically powered off synchronously, thereby speeding up the cooling speed and improving the heat dissipation efficiency;

[0056] 3. By providing an arc-shaped guide surface on the side wall of one end of the limit block passing through the limit groove and close to the opening of the sliding groove, when the pull rod is pulled to drive the key shaft to move into the sliding groove, the key shaft will first contact the guide surface, and the guide surface will generate a component force to drive the limit block to move into the limit groove, thereby eliminating the need to manually push the push rod to drive the limit block into the limit groove, simplifying the work steps and improving work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 It is a three-dimensional structural schematic diagram of the present application;

[0058] Figure 2 is a schematic diagram of the structure of the temperature control device in the present application, wherein the side wall of the kettle body is cut away;

[0059] Figure 3 is a schematic diagram of the structure of the moving mechanism and the transmission assembly in the present application, wherein the side wall of the kettle body is cut away;

[0060] Figure 4 is a schematic diagram of the structure of the limit assembly and the manual rotation assembly in the present application, wherein the second gear is cut away;

[0061] Figure 5 yes Figure 4 Enlarged schematic diagram of part A in the middle.

[0062] 1. the ignition coil; 2. the ignition coil; 3. the ignition line; 4. the ignition line; 5. the ignition line; 6. the ignition line; 7. the ignition line; 8. the ignition line; 9. the ignition line; 10. the ignition line; 11. the ignition line; 12. the ignition line; 13. the ignition line; 14. the ignition line; 15. the ignition line; 16. the ignition line; 17. the ignition line; 18. the ignition line; 19. the ignition line; 20. the ignition line; 21. the ignition line; 22. the ignition line; 23. the ignition line; 24. the ignition line; 25. the ignition line; 26. the ignition line; 27. the ignition line; 28. the ignition line; 29. ​​the ignition line; 30. the ignition line; 31. the ignition line; 32. the ignition line; 33. the ignition line; 34. the ignition line; 35. the ignition line; 36. the ignition line; 37. the ignition line; 38. the ignition line; 39. the ignition line; 41. the ignition line; 42. the ignition line; 43. the ignition line; 44. the ignition line; 45. the ignition line; 46. the ignition line; 51. the ignition line; 52. the ignition line; 53. the ignition line; 54. the ignition line; 55. the ignition line; 56. the ignition line; 57. the ignition line; DETAILED DESCRIPTION

[0063] The following is combined with Figure 1 -Attached Figure 5 This application is described in further detail.

[0064] Example 1 of the present application discloses a method for purifying diborane.

[0065] A diborane purification method includes S1, preparing crude diborane: sodium hydride is used as a starting material in a reactor, nitrogen is introduced to replace the air in the reactor, and tetrahydrofuran is added to clean the mineral oil in the sodium hydride, and the cleaning is performed twice. Trimethyl borate is added dropwise to the sodium hydride tetrahydrofuran mixture, the temperature is controlled to 68°C, a condensation reaction occurs, and the fractions are condensed and all refluxed into the reactor, and the temperature is kept for 5 hours to obtain sodium trimethoxyborohydride. Excess trimethyl borate is distilled off, and a boron trichloride tetrahydrofuran solution is added to the sodium trimethoxyborohydride tetrahydrofuran solution, the temperature is controlled, a double decomposition reaction occurs, and the reaction time is 5 to 10 hours to obtain a crude diborane product. S2. Low temperature and pressure distillation: A packed tower filled with adsorbent is used to purify crude diborane containing low-boiling and high-boiling impurities by low temperature and pressure distillation. The adsorbent is usually a zeolite molecular sieve. The temperature of the reboiler is controlled between -90°C and -20°C, and the pressure of the distillation system is 0.01MPa to 1.5MPa. S3. Multi-stage purification treatment: Potassium borohydride is used for preliminary purification at 20-40°C to obtain a first treated gas, and the first treated gas is further purified by sodium hydroxide at 15-30°C to obtain a second treated gas, and the second treated gas is adsorbed by 13X molecular sieve at -40 to -20°C to obtain a third treated gas. S4. Gas-solid separation: The third treated gas is subjected to gas-solid separation at a temperature below the solidification point of diborane to obtain solid diborane. S5. Inert gas purging: In the method using excess diborane, the obtained product is purged with an inert gas (such as nitrogen or argon) to remove excess diborane. S6. Combined purification by continuous distillation and adsorption: The continuous distillation method and the combined adsorption purification method are used to remove low-boiling point and high-boiling point impurities through reboilers, packed towers, condensers and other equipment to improve the purity of diborane.

[0066] The working principle of Example 1 of the present application is:

[0067] First, crude diborane is produced in a reactor, and then impurities in the diborane are removed through equipment such as filling towers, reboilers, packed towers, and condensers to improve its purity and stability to meet the needs of high-demand applications such as the semiconductor industry.

[0068] Example 2 of the present application discloses a diborane manufacturing device, referring to Figure 1 and Figure 2 , comprising a kettle body 1 and an electric heating tube 11 arranged on the kettle body 1 , and a temperature regulating device 2 for regulating the temperature inside the kettle body 1 is arranged on the kettle body 1 .

[0069] Reference Figure 1 and Figure 2The temperature control device 2 includes a heat dissipation pipe 21, a switch plate 22, a moving mechanism 23 and a temperature sensor 24. The heat dissipation pipe 21 is fixedly mounted on the upper surface of the kettle body 1 and communicated with the inside of the kettle body 1. The heat dissipation pipe 21 is used to discharge the hot air in the kettle body 1. The switch plate 22 is horizontally slidably mounted on the kettle body 1 through the moving mechanism 23 and is located at the connection between the heat dissipation pipe 21 and the kettle body 1. The switch plate 22 opens and closes the connection between the heat dissipation pipe 21 and the kettle body 1.

[0070] Reference Figure 2 and Figure 3 The temperature sensor 24 is fixedly mounted on the inner wall of the kettle body 1 and senses the working temperature inside the kettle body 1. The moving mechanism 23 includes a moving rail 31, a moving block 32, a moving screw 33 and a transmission assembly 34. The moving rail 31 is fixedly mounted on the inner top wall of the kettle body 1. The switch plate 22 is slidably mounted on the moving rail 31. The moving block 32 is fixedly mounted on the lower surface of the switch plate 22. The moving screw 33 is rotatably mounted on the inner wall of the kettle body 1 and is threadedly connected to the moving block 32. The transmission assembly 34 is arranged on the kettle body 1, and the transmission assembly 34 receives the temperature signal of the temperature sensor 24 and controls the moving screw 33 to rotate.

[0071] Reference Figure 3 and Figure 4 The transmission assembly 34 includes a transmission motor 41, a temperature control meter 42, a high temperature relay 43, a high temperature travel switch 44, a low temperature relay 45 and a low temperature travel switch 46. The transmission motor 41 is fixedly mounted on the inner top wall of the kettle body 1, and a first gear 35 is fixedly mounted on the output shaft of the transmission motor 41. A second gear 36 is rotatably mounted on the inner side wall of the kettle body 1. The second gear 36 meshes with the first gear 35. A transmission wheel 39 is fixedly mounted on one end of the moving screw 33 close to the second gear 36. A horizontal connecting groove is provided on the side wall of the transmission wheel 39 close to the second gear 36. A key shaft 37 is horizontally slidably mounted on the second gear 36, and the key shaft 37 is plugged into the connecting groove.

[0072] Reference Figure 3 and Figure 4 The transmission motor 41 starts to drive the first gear 35 to rotate, the first gear 35 rotates to drive the second gear 36, the second gear 36 rotates to drive the key shaft 37, the key shaft 37 rotates to drive the transmission wheel 39, and the transmission wheel 39 rotates to drive the moving screw 33. The moving screw 33 rotates to drive the moving block 32 to move, and the moving block 32 moves to drive the switch plate 22 to move, so that the movement of the switch plate 22 is achieved by controlling the transmission motor 41.

[0073] Reference Figure 3 and Figure 4The temperature control meter 42 is fixedly mounted on the inner wall of the kettle body 1 and is electrically connected to the temperature sensor 24. The high temperature relay 43 and the high temperature travel switch 44 are both fixed in the kettle body 1 and are electrically connected to the temperature control meter 42 and the positive electrode of the transmission motor 41. The low temperature relay 45 and the low temperature travel switch 46 are both fixedly mounted in the kettle body 1 and are electrically connected to the temperature control meter 42 and the reverse electrode of the transmission motor 41.

[0074] Reference Figure 3 and Figure 4 The temperature sensor 24 is electrically connected to the temperature control meter 42, and the temperature control meter 42 is divided into two branches: one branch is connected in series with the high-temperature relay 43, the high-temperature travel switch 44 and the positive rotation electrode of the transmission motor 41; the other branch is connected in series with the low-temperature relay 45, the low-temperature travel switch 46 and the reverse rotation electrode of the transmission motor 41.

[0075] Reference Figure 3 and Figure 4 The temperature control table 42 can set the highest temperature point G and the lowest temperature point D. The temperature control table 42 automatically controls whether to connect to the high temperature relay 43 or the low temperature relay 45 according to the temperature value of the temperature sensor 24, which is greater than or equal to G, less than G and greater than D, and less than or equal to D. The switches of the temperature control table 42, the high temperature relay 43 and the low temperature relay 45 are linked, and the working states of the two relays are mutually inverse, that is, when the temperature control table 42 is connected to the high temperature relay 43, the switch of the high temperature relay 43 is closed, and the switch of the low temperature relay 45 is open; conversely, when the temperature control table 42 is connected to the low temperature relay 43, the switch of the high temperature relay 43 is open, and the switch of the low temperature relay 45 is closed. When the temperature measured by the temperature sensor 24 is less than or equal to D, the temperature control table 42 is connected to the low temperature relay 45, and the transmission motor 41 rotates forward; when the measured temperature is less than G and greater than D, the temperature control table 42 disconnects the relay, and the transmission motor 41 does not work; when the temperature is greater than or equal to G, the temperature control table 42 is connected to the high temperature relay 43, and the transmission motor 41 is reversed. The switch plate 22 is controlled to open and close the heat dissipation pipe 21 by the forward and reverse rotation of the transmission motor 41 , thereby adjusting the temperature in the kettle body 1 .

[0076] Reference Figure 2 A heating switch 12 is fixedly mounted on the top wall of the kettle body 1. The heating switch 12 is electrically connected to the motor heat pipe. When the switch plate 22 closes the heat pipe 21, the switch plate 22 and the contact of the heating switch 12 collide, and the heating switch 12 controls the electric heating pipe 11 to be energized. Therefore, when the switch plate 22 opens the heat pipe 21 to perform heat dissipation, the electric heating pipe 11 will also be automatically powered off synchronously, thereby accelerating the cooling speed and improving the heat dissipation efficiency.

[0077] Reference Figure 5A moving spring 13 is fixedly installed on the inner bottom wall of the sliding groove 56, and the moving spring 13 is connected to the key shaft 37. Under the action of the moving spring 13, the head of the key shaft 37 passes through the sliding groove 56 and is plugged into the connecting groove. A pull rod 14 is fixedly installed at the end of the key shaft 37, and the end of the pull rod 14 away from the key shaft 37 extends out of the kettle body 1.

[0078] Reference Figure 4 and Figure 5 , a limiting assembly 38 is provided on the second gear 36, and the limiting assembly 38 limits the sliding position of the key shaft 37. The limiting assembly 38 includes a limiting block 51, a limiting spring 52, a first moving block 53, a second moving block 54 and a push rod 55. A sliding groove 56 for horizontal sliding of the key shaft 37 is provided on the side wall of the second gear 36, and a limiting groove 57 is provided on the inner side wall of the sliding groove 56 along the radial direction of the second gear 36, and the limiting block 51 is slidably installed on the limiting groove 57. The limiting spring 52 is fixedly installed on the inner bottom wall of the limiting groove 57 and connected to the limiting block 51. A clamping groove is provided on the side wall of the key shaft 37, and the limiting block 51 partially passes out of the limiting groove 57 under the action of the limiting spring 52 and is clamped and matched with the clamping groove. A circular arc-shaped guide surface 58 is provided on the side wall of one end of the limiting block 51 passing out of the limiting groove 57 near the opening of the sliding groove 56.

[0079] Reference Figure 4 and Figure 5 The first moving block 53 is fixedly mounted on the outer wall of the limiting block 51 and is located in the limiting groove 57. The second moving block 54 is horizontally slidably mounted on the second gear 36 and contacts the first moving block 53. The side wall of the first moving block 53 and the second moving block 54 contacting each other is arranged in an inclined state. The first moving block 53 compresses the limiting spring 52 to move under the action of the second moving block 54. One end of the push rod 55 is fixedly connected to the end of the second moving block 54 away from the first moving block 53, and the other end of the push rod 55 extends out of the kettle body 1.

[0080] Reference Figure 4 and Figure 5 When the key shaft 37 is plugged into the connecting groove, the limit block 51 compresses the limit spring 52 and is located in the limit groove 57 as a whole. When the movable key shaft 37 is disengaged from the connecting groove, the key shaft 37 moves into the sliding groove 56, and the clamping groove on the key shaft 37 is connected with the limit groove 57. Then, under the action of the limit spring 52, the limit block 51 partially passes through the limit groove 57 and engages with the clamping groove, thereby limiting the position of the key shaft 37; when the key shaft 37 needs to be moved out, the push rod 55 drives the second moving block 54 to move. The second moving block 54 moves and drives the first moving block 53 to compress the limit spring 52 and move. The first moving block 53 moves and drives the limit block 51 to move into the limit groove 57 as a whole. It is convenient and quick.

[0081] Reference Figure 3 and Figure 4A manual rotating assembly 6 is provided on the kettle body 1, and the manual rotating assembly 6 is used to control the rotation of the transmission wheel 39 when the transmission motor 41 fails or loses power. The manual rotating assembly 6 includes a handwheel 61, a rotating wheel 62 and a transmission belt 63. The handwheel 61 is rotatably mounted on the outer wall of the kettle body 1. The rotating wheel 62 is rotatably arranged coaxially with the handwheel 61, and the rotating wheel 62 is located in the kettle body 1. The transmission belt 63 is sleeved on the rotating wheel 62 and the transmission wheel 39.

[0082] Reference Figure 3 and Figure 4 When the key shaft 37 is disengaged from the transmission wheel 39, the hand wheel 61 is rotated, the hand wheel 61 drives the rotating wheel 62 to rotate, the rotating wheel 62 drives the transmission belt 63 to rotate, the transmission belt 63 drives the transmission wheel 39 to rotate, the transmission wheel 39 drives the moving screw 33 to rotate, the moving screw 33 drives the switch plate 22 to move, thereby realizing the manual control of the movement of the switch plate 22 by rotating the hand wheel 61.

[0083] The working principle of Example 2 of the present application is:

[0084] The temperature sensor 24 senses the working environment temperature inside the kettle body 1. When the temperature sensed by the temperature sensor 24 is too high, the transmission motor 41 starts to drive the switch board 22 to open the heat dissipation pipe 21, and the heat dissipation pipe 21 dissipates heat and cools the inside of the kettle body 1. When the temperature inside the kettle body 1 is low, the transmission motor 41 drives the switch board 22 to close the heat dissipation pipe 21, so that the inside of the kettle body 1 is heated up under the action of the electric heating tube 11, thereby completing the automatic temperature adjustment work inside the kettle body 1, ensuring the stable and uniform temperature inside the kettle body 1, without the need for manual real-time monitoring and adjustment, reducing work intensity and improving work efficiency.

[0085] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A method for purifying diborane, characterized in that: include: S1. Preparation of crude diborane: sodium hydride is used as a starting material in a reactor, nitrogen is introduced to replace the air in the reactor, tetrahydrofuran is added, the mineral oil in the sodium hydride is cleaned, twice in total, trimethyl borate is added dropwise to the sodium hydride tetrahydrofuran mixture, the temperature is controlled to 68° C., a condensation reaction occurs, the fraction is condensed and all refluxed into the reactor, and the temperature is kept for 5 hours to obtain sodium trimethoxyborohydride, excess trimethyl borate is distilled off, boron trichloride tetrahydrofuran solution is added to the sodium trimethoxyborohydride tetrahydrofuran solution, the temperature is controlled, a double decomposition reaction occurs, and the reaction time is 5 to 10 hours to obtain crude diborane; S2. Low temperature pressure distillation: A packed tower filled with adsorbent is used to purify crude diborane containing low-boiling point and high-boiling point impurities by low temperature pressure distillation. The adsorbent is usually zeolite molecular sieve. The temperature of the reboiler is controlled between -90°C and -20°C. The pressure of the distillation system is 0.01MPa to 1.5MPa. S3, multi-stage purification treatment: using potassium borohydride to perform preliminary purification treatment at 20-40°C to obtain a first treated gas, further purifying the first treated gas using sodium hydroxide at 15-30°C to obtain a second treated gas, and adsorbing the second treated gas using 13X molecular sieve at -40 to -20°C to obtain a third treated gas; S4, gas-solid separation: performing gas-solid separation on the third treated gas at a temperature lower than the solidification point of diborane to obtain solid diborane; S5. Inert gas purging: In the method using excess diborane, the obtained product is purged with an inert gas (such as nitrogen or argon) to remove excess diborane; S6. Combined purification by continuous distillation and adsorption: The continuous distillation method and the combined adsorption purification method are used to remove low-boiling point and high-boiling point impurities through reboilers, packed towers, condensers and other equipment to improve the purity of diborane.

2. A diborane purification device for producing the diborane as claimed in claim 1, characterized in that: The invention comprises a kettle body (1) and an electric heating tube (11) arranged on the kettle body (1), wherein the kettle body (1) is provided with a temperature regulating device (2) for regulating the temperature in the kettle body (1), and the temperature regulating device (2) comprises: A heat dissipation pipe (21), the heat dissipation pipe (21) being arranged on the kettle body (1), the heat dissipation pipe (21) being provided with a fan, and the heat dissipation pipe (21) being used to discharge hot air in the kettle body (1); A switch plate (22), the switch plate (22) being horizontally slidably disposed on the kettle body (1), the switch plate (22) being located at the connection between the heat dissipation pipe (21) and the kettle body (1); A moving mechanism (23), wherein the moving mechanism (23) is arranged on the kettle body (1) and is used to control the movement of the switch plate (22); A temperature sensor (24) is arranged in the kettle body (1) and is electrically connected to the moving mechanism (23).

3. A diborane purification device according to claim 2, characterized in that: The moving mechanism (23) comprises: A movable slide rail (31), wherein the movable slide rail (31) is arranged on the kettle body (1), and the switch plate (22) is slidably arranged on the movable slide rail (31); A moving block (32), the moving block (32) being horizontally slidably disposed on the kettle body (1) and connected to the switch plate (22); A moving screw (33), the moving screw (33) is rotatably disposed on the kettle body (1) and is threadably connected to the moving block (32); A transmission component (34) is arranged on the kettle body (1), and the transmission component (34) receives the temperature signal of the temperature sensor (24) and controls the moving screw (33) to rotate.

4. A diborane purification device according to claim 3, characterized in that: The transmission assembly (34) comprises: A transmission motor (41), wherein the transmission motor (41) is arranged on the kettle body (1) and the output shaft is connected to the moving screw (33); A temperature control meter (42), the temperature control meter (42) being arranged on the kettle body (1) and being electrically connected to the temperature sensor (24); A high temperature relay (43) and a high temperature travel switch (44), wherein the high temperature relay (43) and the high temperature travel switch (44) are both arranged on the kettle body (1) and are electrically connected to the temperature control meter (42) and the positive rotation electrode of the transmission motor (41); A low temperature relay (45) and a low temperature travel switch (46), wherein the low temperature relay (45) and the low temperature travel switch (46) are both arranged on the kettle body (1) and are electrically connected to the temperature control meter (42) and the reverse electrode of the transmission motor (41).

5. A diborane purification device according to claim 2, characterized in that: The kettle body (1) is provided with a heating switch (12), and the heating switch (12) is electrically connected to the electric heating tube (11). When the switch plate (22) closes the heat dissipation tube (21), the switch plate (22) contacts the heating switch (12), and the heating switch (12) controls the electric heating tube (11) to be energized.

6. A diborane purification device according to claim 4, characterized in that: The output shaft of the transmission motor (41) is provided with a first gear (35); the kettle body (1) is rotatably provided with a second gear (36); the second gear (36) is meshed with the first gear (35); the movable screw rod (33) is provided with a transmission wheel (39); a key shaft (37) is slidably provided on the second gear (36); a connecting groove is provided on the transmission wheel (39); the key shaft (37) is plugged into the connecting groove; a limiting component (38) is provided on the second gear (36); the limiting component (38) limits the sliding position of the key shaft (37); and a manual rotating component (6) is provided on the kettle body (1); the manual rotating component (6) is used to control the rotation of the transmission wheel (39).

7. A diborane purification device according to claim 6, characterized in that: The limiting component (38) comprises: A limit block (51), the second gear (36) is provided with a sliding groove (56) for the key shaft (37) to slide horizontally, the inner side wall of the sliding groove (56) is provided with a limit groove (57) along the radial direction of the second gear (36), and the limit block (51) is slidably mounted on the limit groove (57); A limit spring (52), the limit spring (52) is arranged on the inner bottom wall of the limit groove (57) and connected to the limit block (51), a clamping groove is provided on the side wall of the key shaft (37), and the limit block (51) partially passes out of the limit groove (57) under the action of the limit spring (52) and is clamped and matched with the clamping groove; A first moving block (53), wherein the first moving block (53) is arranged on the limiting block (51); a second moving block (54), the second moving block (54) being horizontally slidably arranged on the second gear (36) and abutting against the first moving block (53), the side wall of one side of the first moving block (53) and the second moving block (54) abutting against each other being arranged in an inclined state, and the first moving block (53) being compressed by the limiting spring (52) to move under the action of the second moving block (54); A push rod (55), one end of which is arranged on the second moving block (54), and the other end of which extends out of the kettle body (1).

8. A diborane purification device according to claim 7, characterized in that: A movable spring (13) is arranged on the inner bottom wall of the sliding groove (56), and the movable spring (13) is connected to the key shaft (37). Under the action of the movable spring (13), the head of the key shaft (37) passes through the sliding groove (56) and is plugged into the connecting groove. A pull rod (14) is arranged on the key shaft (37), and one end of the pull rod (14) away from the key shaft (37) extends out of the kettle body (1).

9. A diborane purification device according to claim 6, characterized in that: The manual rotation assembly (6) comprises: A hand wheel (61), the hand wheel (61) being rotatably disposed on the kettle body (1); A rotating wheel (62), the rotating wheel (62) being coaxially rotatable with the hand wheel (61), and the rotating wheel (62) being located inside the kettle body (1); A transmission belt (63), wherein the transmission belt (63) is sleeved on the rotating wheel (62) and the transmission wheel (39).

10. A diborane purification device according to claim 7, characterized in that: An arc-shaped guide surface (58) is provided on a side wall of one end of the limiting block (51) that passes out of the limiting groove (57) and is close to the opening of the sliding groove (56).

Images