A continuous reaction apparatus and preparation method for preparing bis(fluorosulfonyl)imide

Abstract

This invention discloses a continuous reaction apparatus and method for preparing bis(fluorosulfonyl)imide, comprising an annular support platform and a support column. A preparation chamber is installed on the inner side of the annular support platform, and a top cover is installed on the top of the preparation chamber. A distillation chamber is installed at the bottom of the outer side of the top cover, and a first solenoid valve is installed at the bottom of the distillation chamber. A third solenoid valve is installed at the center of the bottom of the preparation chamber. A servo motor is installed on the top of the top cover. The invention uses a rotating rod to drive four sets of auxiliary stirring paddles in conjunction with a second stirring paddle to simultaneously stir the mixture, further improving the heating and stirring effect of the reaction apparatus on the raw material mixture. Simultaneously, a vacuum pump is controlled to extract air from the outer chamber, forcing the water vapor generated during distillation in the distillation chamber to enter the heating chamber through the air inlet. The water vapor flows upward along the guide spiral of the spiral guide plate, heating the inner bottom of the preparation chamber during its flow, thus improving thermal energy utilization efficiency.

Description

Technical Field

[0001] This invention relates to the field of bis(fluorosulfonyl)imide preparation technology, specifically to a continuous reaction apparatus and preparation method for bis(fluorosulfonyl)imide. Background Technology

[0002] Difluorosulfonylimide is the main raw material for preparing lithium difluorosulfonylimide. It has a boiling point of 170℃ and a melting point of 17℃. Lithium difluorosulfonylimide is a new type of lithium salt with many advantages such as high conductivity, high thermal stability, hydrolysis resistance, and suppression of battery gas expansion. In terms of performance, it can specifically solve common technical problems in the current lithium-ion battery industry, such as short cycle life (especially at high temperatures) and safety hazards. It has good application prospects and market demand.

[0003] Currently, the preparation of bis(fluorosulfonyl)imide often requires heating, stirring, and distillation of the raw material mixture. Each process requires separate processing time, making it impossible to synchronize these processes and improve the efficiency of the reaction device in preparing bis(fluorosulfonyl)imide. Furthermore, it is impossible to preheat and initially stir the raw material mixture with low energy consumption before bis(fluorosulfonyl)imide preparation, thus preventing further reduction in the subsequent heating and stirring time. At the same time, the heating and stirring effect of the raw material mixture during heating and stirring cannot be further improved to ensure the gas-liquid separation efficiency of the raw material during the preparation of bis(fluorosulfonyl)imide. Summary of the Invention

[0004] The purpose of this invention is to provide a continuous reaction apparatus and preparation method for preparing bis(fluorosulfonyl)imide, so as to solve the related problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a continuous reaction apparatus for preparing bis(fluorosulfonyl)imide, comprising an annular support platform and a support column, a preparation chamber installed on the inner side of the annular support platform, and an upper cover installed on the top of the preparation chamber, a distillation chamber installed at the bottom of the outer side of the upper cover, a first solenoid valve installed at the bottom of the distillation chamber, a third solenoid valve installed at the center of the bottom of the preparation chamber, a servo motor installed on the top of the upper cover, and a rotating rod installed at the output end of the servo motor, the rotating rod extending to the inner bottom of the preparation chamber, a first isolation tube installed at the middle position inside the upper cover, and a spiral heat-conducting tube wound around the outer side of the first isolation tube, the top end of the spiral heat-conducting tube extending to the outer side of the upper cover, the bottom end of the spiral heat-conducting tube extending to the interior of the preparation chamber, a feeding pipe installed on the top of the upper cover, and a second solenoid valve installed at the bottom of the upper cover;

[0006] An outer chamber is installed at the top of the outer side of the preparation chamber. A spiral conveying pipe is installed inside the outer chamber and is wound around the outside of the preparation chamber. The top of the spiral conveying pipe is connected to the top of the inside of the preparation chamber, and the bottom of the spiral conveying pipe extends to the outside of the outer chamber. An air pump is installed at the top of the annular support platform, and the input end of the air pump is connected to the top of the inside of the outer chamber. A preheating component is installed at the top of the inside of the preparation chamber, and a stirring component is installed at the bottom of the inside of the preparation chamber. An auxiliary heating component is installed at the top of the inside of the distillation chamber. An annular insulation layer is installed on the outside of the distillation chamber. A first annular electric heating plate is installed at the bottom of the outside of the distillation chamber. A drive motor is installed at an angle at the middle position of the outside of the annular insulation layer, and the output end of the drive motor extends into the inside of the distillation chamber and is equipped with a first stirring paddle. A control panel is installed at the bottom of the outside of a set of support columns.

[0007] Preferably, the stirring assembly includes a circular partition, a rotating shaft, a universal joint, an auxiliary stirring paddle, a second stirring paddle, a drive gear, a transmission gear, a driven gear, and a second annular electric heating plate. A circular partition is installed at the center of the preparation chamber, and four sets of rotating shafts are evenly arranged at the top edge of the circular partition. An auxiliary stirring paddle is installed at the bottom end of each rotating shaft via a universal joint. The bottom end of the outer side of the rotating shaft passes through the circular partition and is fitted with a second stirring paddle. A drive gear is installed at the center of the outer side of the rotating shaft. Four sets of transmission gears meshing with the drive gear are evenly arranged at the non-center position of the top of the circular partition. Driven gears meshing with the transmission gears are installed at the top ends of the four sets of rotating shafts. A second annular electric heating plate is installed at the bottom of the outer side of the preparation chamber.

[0008] Preferably, the preheating assembly includes a preheating chamber, a second isolation tube, a rotating frame, a stirring rod, and a fourth solenoid valve. The preheating chamber is located at the top of the preparation chamber. The second isolation tube is installed at the center of the bottom of the preheating chamber and is sleeved on the outside of the rotating rod. Four sets of rotating frames are evenly installed at the middle of the outside of the rotating rod. Stirring rods are evenly installed at the bottom of the rotating frames. Three sets of fourth solenoid valves are evenly installed at the edge of the bottom of the preheating chamber.

[0009] Preferably, the auxiliary heating assembly includes a heating chamber, an air inlet, a spiral guide plate, a through hole, and a connecting conduit. The heating chamber is installed at the middle position inside the distillation chamber, and a spiral guide plate adapted to the bottom of the preparation chamber is installed inside the heating chamber. Air inlets are evenly distributed at non-center positions at the bottom of the heating chamber. A through hole is provided at the center position of the bottom of the heating chamber. A connecting conduit is installed at the top of one side of the heating chamber, and the top of the connecting conduit communicates with the inner bottom of the outer chamber.

[0010] Preferably, a first bearing is installed at the bottom of the outer side of the auxiliary stirring paddle, and the outer side of the first bearing is fixedly connected to a non-central position at the bottom of the distillation chamber.

[0011] Preferably, a second bearing is installed at the center of the top of the circular partition, and a third bearing is installed at the inner top and inner bottom of the first isolation tube, and the inner sides of the third bearing and the second bearing are fixedly connected to the outer side of the rotating rod.

[0012] Preferably, the thickness of the bottom of the preheating chamber gradually increases from the edge to the center, and a fourth bearing is installed at the center of the bottom of the preheating chamber, with the inner side of the fourth bearing fixedly connected to the outer side of the rotating rod.

[0013] Preferably, the bottom of the top cover and the top of the preparation chamber are symmetrically equipped with first flanges, and several sets of first fixing bolts are provided on both sets of first flanges.

[0014] Preferably, a second flange is installed at the middle position on the outer side of the preparation chamber, and the second flange is provided with several sets of second fixing bolts that are fixedly connected to the top of the annular support platform.

[0015] Preferably, a method for preparing a continuous reaction apparatus for preparing bis(fluorosulfonyl)imide comprises the following steps:

[0016] 1. The two raw materials are conveyed into the preheating chamber and the upper cover through the spiral conveyor pipe and the feeding pipe respectively. Then the raw materials inside the upper cover also flow into the preheating chamber through the second solenoid valve.

[0017] 2. The servo motor is controlled to drive the rotating rod to rotate clockwise at a uniform speed. The rotating rod also drives the rotating frame and the stirring rod to perform preliminary stirring of the mixed raw materials inside the preheating chamber.

[0018] Third, the rotating rod, through the drive gear, transmission gear and driven gear, drives four sets of auxiliary stirring paddles to work with the second stirring paddle to perform secondary stirring of the mixed raw materials at the bottom of the preparation chamber. During the process, the second annular electric heating plate is controlled to heat the mixed raw materials at the bottom of the preparation chamber. The mixed raw materials at the bottom of the preparation chamber are separated into gas and liquid, and the separated gas is discharged into the external environment through the spiral heat conduction pipe.

[0019] Fourth, open the third solenoid valve to discharge the remaining liquid raw material at the bottom of the preparation chamber into the interior of the distillation chamber, and then control the first annular electric heating plate to heat the liquid raw material inside the distillation chamber and distill it.

[0020] 5. Control the drive motor to drive the first stirring paddle to stir the liquid raw material inside the distillation chamber;

[0021] 6. Next, control the air pump to draw air from the outer chamber. The water vapor generated during distillation in the distillation chamber enters the heating chamber through the air inlet and is finally discharged into the external environment through the output of the air pump. After the liquid raw material in the distillation chamber is distilled, open the first solenoid valve to discharge the distilled difluorosulfonamide.

[0022] Compared with the prior art, the present invention provides a continuous reaction apparatus and preparation method for preparing bis(fluorosulfonyl)imide, which has the following beneficial effects:

[0023] 1. In this invention, after hydrogen fluoride and bis(chlorosulfonyl)imide are fed into the bottom of the preparation chamber, a servo motor is controlled to drive a rotating rod to rotate. The rotating rod drives a stirring assembly to heat and stir the raw material mixture at the bottom of the preparation chamber, causing gas-liquid separation in the raw material mixture. The spiral heat pipe discharges the gas, and the remaining mixture enters the distillation chamber through a third solenoid valve and is heated by a first annular electric heating plate. Then, a drive motor is controlled to drive a first stirring paddle to stir and distill the mixture inside the distillation chamber. At the same time, hydrogen fluoride and bis(chlorosulfonyl)imide are added to the inside of the rotating rod and heated and stirred. By allowing the two processing steps to proceed simultaneously, the reaction device can continuously process bis(chlorosulfonyl)imide, thereby improving the efficiency of the reaction device in preparing bis(chlorosulfonyl)imide.

[0024] 2. In this invention, two raw materials are conveyed into the preheating chamber and the upper cover through a spiral conveying pipe and a feeding pipe, respectively. During the process, water vapor generated by distillation inside the distillation chamber is conveyed into the outer chamber through a connecting pipe. The water vapor preheats the raw materials inside the spiral conveying pipe. Meanwhile, the water vapor generated by heating and stirring at the bottom of the preparation chamber preheats the raw materials passing through the upper cover through the spiral heat conduction pipe. Then, it enters the preheating chamber through the second solenoid valve. After the two raw materials are mixed together inside the preheating chamber, when the servo motor drives the rotating rod to rotate, the rotating rod also drives the rotating frame and stirring rod to stir the mixed raw materials inside the preheating chamber. The water vapor passing through the outer chamber can also heat the mixed raw materials inside the preheating chamber, thereby further improving the utilization efficiency of thermal energy of the reaction device. After preheating and stirring the mixed raw materials, the subsequent heating and stirring time of the raw material mixture can be further reduced.

[0025] 3. In this invention, when the rotating rod drives the second stirring paddle to stir the raw material mixture inside the preparation chamber, the rotating rod, through the transmission of the drive gear, transmission gear, and driven gear, drives four sets of auxiliary stirring paddles to work in conjunction with the second stirring paddle to stir simultaneously. During the process, the second annular electric heating plate is controlled to heat the mixture, thereby further improving the heating and stirring effect of the reaction device on the raw material mixture. At the same time, the vacuum pump is controlled to extract air from the outer chamber, forcing the water vapor generated by distillation in the distillation chamber to enter the heating chamber through the air inlet. The water vapor flows upward along the guide spiral of the spiral guide plate, heating the inner bottom of the preparation chamber during the flow of water vapor. While improving the thermal energy utilization efficiency, the stirring components can further improve the heating and stirring effect of the reaction device on the difluorosulfonyl imide raw material. Attached Figure Description

[0026] Figure 1 This is the front view of the present invention;

[0027] Figure 2 This is a front sectional view of the present invention;

[0028] Figure 3 This is a front sectional view of the top cover of the present invention;

[0029] Figure 4 This is a front sectional view of the preparation chamber of the present invention;

[0030] Figure 5 This is a front sectional view of the distillation chamber of the present invention;

[0031] Figure 6 This is a front view schematic diagram of the preparation chamber of the present invention;

[0032] Figure 7 This is a three-dimensional schematic diagram of the preparation chamber of the present invention;

[0033] Figure 8 This is a front view schematic diagram of the distillation chamber of the present invention;

[0034] Figure 9 This is a top view of the circular partition of the present invention.

[0035] In the diagram: 1. Top cover; 2. Preparation chamber; 3. Vacuum pump; 4. Distillation chamber; 5. Annular support platform; 6. Preheating assembly; 601. Preheating chamber; 602. Second isolation tube; 603. Rotating frame; 604. Stirring rod; 605. Fourth solenoid valve; 7. Stirring assembly; 701. Circular partition; 702. Rotating shaft; 703. Universal joint; 704. Auxiliary stirring paddle; 705. Second stirring paddle; 706. Drive gear; 707. Transmission gear; 708. Driven gear; 709. Second annular electric heating plate; 8. Auxiliary... 801. Heating chamber; 802. Air inlet; 803. Spiral guide plate; 804. Through hole; 805. Connecting conduit; 9. Rotating rod; 10. Drive motor; 11. Support column; 12. First solenoid valve; 13. Control panel; 14. Annular insulation layer; 15. Second solenoid valve; 16. Outer chamber; 17. Spiral conveying pipe; 18. Feeding pipe; 19. Servo motor; 20. Spiral heat conduction pipe; 21. Third solenoid valve; 22. First stirring paddle; 23. First annular electric heating plate; 24. First isolation pipe. Detailed Implementation

[0036] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] Please see Figure 1-9 The present invention provides a technical solution: a continuous reaction apparatus for preparing bis(fluorosulfonyl)imide, comprising an annular support platform 5 and a support column 11. A preparation chamber 2 is installed on the inner side of the annular support platform 5, and an upper cover 1 is installed on the top of the preparation chamber 2. A distillation chamber 4 is installed on the bottom of the outer side of the upper cover 1. A first solenoid valve 12 is installed on the bottom of the distillation chamber 4. A third solenoid valve 21 is installed at the center of the bottom of the preparation chamber 2. A servo motor 19 is installed on the top of the upper cover 1, and a rotating rod 9 is installed at the output end of the servo motor 19. The rotating rod 9 extends to the inner bottom of the preparation chamber 2. A first isolation tube 24 is installed at the middle position inside the upper cover 1, and a spiral heat-conducting tube 20 is wound around the outer side of the first isolation tube 24. The top end of the spiral heat-conducting tube 20 extends to the outer side of the upper cover 1, and the bottom end of the spiral heat-conducting tube 20 extends to the interior of the preparation chamber 2. A feed pipe 18 is installed on the top of the upper cover 1, and a second solenoid valve 15 is installed at the bottom of the upper cover 1.

[0038] An outer chamber 16 is installed at the top of the outer side of the preparation chamber 2. A spiral conveying pipe 17 is installed inside the outer chamber 16 and is wound around the outside of the preparation chamber 2. The top of the spiral conveying pipe 17 is connected to the top of the inside of the preparation chamber 2, and the bottom of the spiral conveying pipe 17 extends to the outside of the outer chamber 16. An air pump 3 is installed at the top of the annular support platform 5, and the input end of the air pump 3 is connected to the top of the inside of the outer chamber 16. A preheating component 6 is installed at the top of the inside of the preparation chamber 2, and a stirring component 7 is installed at the bottom of the inside of the preparation chamber 2. An auxiliary heating component 8 is installed at the top of the inside of the distillation chamber 4. An annular insulation layer 14 is installed on the outside of the distillation chamber 4. A first annular electric heating plate 23 is installed at the bottom of the outside of the distillation chamber 4. A drive motor 10 is installed at an angle at the middle position of the outside of the annular insulation layer 14, and the output end of the drive motor 10 extends into the inside of the distillation chamber 4 and is equipped with a first stirring paddle 22. A control panel 13 is installed at the bottom of the outside of a set of support columns 11.

[0039] Furthermore, the stirring assembly 7 includes a circular partition 701, a rotating shaft 702, a universal joint 703, an auxiliary stirring paddle 704, a second stirring paddle 705, a drive gear 706, a transmission gear 707, a driven gear 708, and a second annular electric heating plate 709. A circular partition 701 is installed at the center of the preparation chamber 2, and four sets of rotating shafts 702 are evenly arranged at the top edge of the circular partition 701. The bottom end of each rotating shaft 702 is fitted with an auxiliary stirring paddle 704 via a universal joint 703. A stirring paddle 704 is installed at the bottom of the outer side of the rotating rod 9, which passes through the circular partition 701 and is fitted with a second stirring paddle 705. A drive gear 706 is installed at the middle position of the outer side of the rotating rod 9. Four sets of transmission gears 707 that mesh with the drive gear 706 are evenly arranged at the non-center position of the top of the circular partition 701. Driven gears 708 that mesh with the transmission gears 707 are installed at the top of the outer side of the four sets of rotating shafts 702. A second annular electric heating plate 709 is installed at the bottom of the outer side of the preparation chamber 2.

[0040] Furthermore, the preheating component 6 includes a preheating chamber 601, a second isolation tube 602, a rotating frame 603, a stirring rod 604, and a fourth solenoid valve 605. The preheating chamber 601 is located at the top of the preparation chamber 2. The second isolation tube 602 is installed at the center of the bottom of the preheating chamber 601 and is sleeved on the outside of the rotating rod 9. Four sets of rotating frames 603 are evenly installed at the middle of the outside of the rotating rod 9. The stirring rod 604 is evenly installed at the bottom of the rotating frame 603. Three sets of fourth solenoid valves 605 are evenly installed at the edge of the bottom of the preheating chamber 601.

[0041] Furthermore, the auxiliary heating component 8 includes a heating chamber 801, an air inlet 802, a spiral guide plate 803, a through hole 804, and a connecting conduit 805. The heating chamber 801 is installed in the middle of the interior of the distillation chamber 4, and a spiral guide plate 803 adapted to the bottom of the preparation chamber 2 is installed inside the heating chamber 801. Air inlets 802 are evenly distributed at non-center positions at the bottom of the heating chamber 801, and a through hole 804 is distributed at the center of the bottom of the heating chamber 801. A connecting conduit 805 is installed at the top of one side of the heating chamber 801, and the top of the connecting conduit 805 communicates with the inner bottom of the outer chamber 16.

[0042] Furthermore, a first bearing is installed at the bottom of the outer side of the auxiliary stirring paddle 704, and the outer side of the first bearing is fixedly connected to the bottom non-center position inside the distillation chamber 4, which helps to ensure the stability of the auxiliary stirring paddle 704 when it is tilted.

[0043] Furthermore, a second bearing is installed at the center of the top of the circular partition 701, and a third bearing is installed at the inner top and inner bottom of the first isolation tube 24. The inner sides of the third bearing and the second bearing are fixedly connected to the outer side of the rotating rod 9, which helps to ensure the stability of the rotating rod 9 during rotation.

[0044] Furthermore, the thickness of the bottom of the preheating chamber 601 gradually increases from the edge to the center. A fourth bearing is installed at the center of the bottom of the preheating chamber 601, and the inner side of the fourth bearing is fixedly connected to the outer side of the rotating rod 9, so that the mixed raw materials inside the preheating chamber 601 can be completely discharged into the bottom of the preparation chamber 2 through three sets of fourth solenoid valves 605.

[0045] Furthermore, the bottom of the top cover 1 and the top of the preparation chamber 2 are symmetrically installed with first flanges, and several sets of first fixing bolts are provided on the two sets of first flanges. The top cover 1 and the preparation chamber 2 can be separated by unscrewing the first fixing bolts.

[0046] Furthermore, a second flange is installed at the middle position on the outer side of the preparation chamber 2, and several sets of second fixing bolts are provided on the second flange to be fixedly connected to the top of the annular support platform 5. The preparation chamber 2 can be disassembled from the inside of the annular support platform 5 by unscrewing the second fixing bolts.

[0047] Furthermore, a method for preparing a continuous reaction apparatus for preparing bis(fluorosulfonyl)imide includes the following steps:

[0048] First, the two raw materials are conveyed into the preheating chamber 601 and the upper cover 1 through the spiral conveyor pipe 17 and the feeding pipe 18 respectively. Then, the raw materials inside the upper cover 1 also flow into the preheating chamber 601 through the second solenoid valve 15.

[0049] 2. The servo motor 19 drives the rotating rod 9 to rotate clockwise at a uniform speed. The rotating rod 9 also drives the rotating frame 603 and the stirring rod 604 to perform preliminary stirring of the mixed raw materials inside the preheating chamber 601.

[0050] Third, the rotating rod 9, through the drive gear 706, transmission gear 707 and driven gear 708, drives four sets of auxiliary stirring paddles 704 to work with the second stirring paddle 705 to perform secondary stirring of the mixed raw materials at the bottom of the preparation chamber 2. During the process, the second annular electric heating plate 709 is controlled to heat the mixed raw materials at the bottom of the preparation chamber 2. The mixed raw materials at the bottom of the preparation chamber 2 are separated into gas and liquid, and the separated gas is discharged into the external environment through the spiral heat conduction pipe 20.

[0051] Fourth, the third solenoid valve 21 is then opened to discharge the remaining liquid raw material at the bottom of the preparation chamber 2 into the interior of the distillation chamber 4. Then, the first annular electric heating plate 23 is controlled to heat the liquid raw material inside the distillation chamber 4 and distill it.

[0052] 5. Control the drive motor 10 to drive the first stirring paddle 22 to stir the liquid raw material inside the distillation chamber 4;

[0053] 6. Next, the air pump 3 is controlled to extract air from the outer chamber 16. The water vapor generated by distillation in the distillation chamber 4 enters the heating chamber 801 through the air inlet 802 and is finally discharged into the external environment through the output end of the air pump 3. After the liquid raw material in the distillation chamber 4 is distilled, the first solenoid valve 12 is opened to discharge the distilled difluorosulfonamide.

[0054] Example 1, such as Figure 1-8 As shown, by unscrewing several sets of first fixing bolts, the two sets of first flanges are disconnected, thereby disconnecting the top cover 1 and the preparation chamber 2. After opening the top cover 1, the parts inside the preheating chamber 601 can be inspected and maintained. When it is necessary to remove the entire preparation chamber 2 from the device, several sets of second fixing bolts are unscrewed to disconnect the preparation chamber 2 from the annular support platform 5. Then, the preparation chamber 2 together with the top cover 1 can be lifted and removed from the device.

[0055] Example 2, as Figure 2-4 and Figure 9As shown, when the servo motor 19 drives the rotating rod 9 to rotate clockwise, the rotating rod 9 simultaneously drives four sets of transmission gears 707 to rotate counterclockwise through the drive gear 706. The transmission gears 707 then drive the driven gear 708 connected to them to rotate clockwise. The rotating shaft 702, in conjunction with the universal joint 703, drives the auxiliary stirring paddle 704 to rotate clockwise. Since the drive gear 706 is larger than the driven gear 708, the rotational speed of the auxiliary stirring paddle 704 is greater than that of the second stirring paddle 705. At this time, the four sets of auxiliary stirring paddles 704, in conjunction with the second stirring paddle 705, can greatly improve the stirring effect of the device on the mixed raw materials at the bottom of the preparation chamber 2.

[0056] Working Principle: Before use, connect the device to the power supply. First, the two raw materials are conveyed into the preheating chamber 601 and the upper cover 1 through the spiral conveyor pipe 17 and the feeding pipe 18, respectively. Then, the raw materials inside the upper cover 1 also flow into the preheating chamber 601 through the second solenoid valve 15. The servo motor 19 is controlled by the control panel 13 to drive the rotating rod 9 to rotate clockwise at a uniform speed. The rotating rod 9 also drives the rotating frame 603 and the stirring rod 604 to perform preliminary stirring of the mixed raw materials inside the preheating chamber 601. The rotating rod 9, through the drive gear 706, transmission gear 707 and driven gear 708, drives the four sets of auxiliary stirring paddles 704 to work with the second stirring paddle 705 to perform secondary stirring of the mixed raw materials at the bottom of the preparation chamber 2. During the process, the second annular electric heating plate 709 is controlled to heat the mixed raw materials at the bottom of the preparation chamber 2. The mixed raw materials at the bottom of the preparation chamber 2 undergo gas-liquid separation. The separated gas is discharged into the external environment through the spiral heat conduction pipe 20. During the process, the high temperature gas preheats the raw materials passing through the upper cover 1. Then, the third solenoid valve 21 is opened to discharge the remaining liquid raw material at the bottom of the preparation chamber 2 into the interior of the distillation chamber 4. Next, the first annular electric heating plate 23 is controlled to heat the liquid raw material inside the distillation chamber 4 and distill it. At the same time, the drive motor 10 is controlled to drive the first stirring paddle 22 to stir the liquid raw material inside the distillation chamber 4. Then, the vacuum pump 3 is controlled to evacuate air from the interior of the outer chamber 16. The water vapor generated during distillation in the distillation chamber 4 enters the interior of the heating chamber 801 through the air inlet 802. The water vapor flows upward along the guide spiral of the spiral guide plate 803. During the flow of water vapor, the bottom of the preparation chamber 2 is heated. Then, the water vapor enters the bottom of the outer chamber 16 through the connecting conduit 805. Subsequently, the water vapor flows upward around the outer spiral of the preparation chamber 2 along the guide spiral conveyor pipe 17. Finally, it is discharged into the external environment through the output end of the vacuum pump 3. After the liquid raw material inside the distillation chamber 4 is distilled, the first solenoid valve 12 is opened to discharge the distilled difluorosulfonamide.

[0057] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0058] All electrical components mentioned in this article are connected to an external main controller and 220V AC mains power, and the main controller can be a conventional known device such as a computer that can control it.

[0059] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A continuous reaction apparatus for preparing bis(fluorosulfonyl)imide, comprising an annular support platform (5) and a support column (11), characterized in that: The inner side of the annular support platform (5) is equipped with a preparation chamber (2), and the top of the preparation chamber (2) is equipped with an upper cover (1). The bottom of the outer side of the upper cover (1) is equipped with a distillation chamber (4). The bottom of the distillation chamber (4) is equipped with a first solenoid valve (12). The center of the bottom of the preparation chamber (2) is equipped with a third solenoid valve (21). The top of the upper cover (1) is equipped with a servo motor (19), and the output end of the servo motor (19) is equipped with a rotating rod (9). 9) Extending to the inner bottom of the preparation chamber (2), a first isolation tube (24) is installed in the middle position inside the upper cover (1), and a spiral heat-conducting tube (20) is wound around the outside of the first isolation tube (24). The top end of the spiral heat-conducting tube (20) extends to the outside of the upper cover (1), and the bottom end of the spiral heat-conducting tube (20) extends to the inside of the preparation chamber (2). A feeding tube (18) is installed on the top of the upper cover (1), and a second solenoid valve (15) is installed on the bottom of the upper cover (1). An outer chamber (16) is installed at the top of the outer side of the preparation chamber (2). A spiral conveying pipe (17) is provided inside the outer chamber (16), and the spiral conveying pipe (17) is wound around the outside of the preparation chamber (2). The top of the spiral conveying pipe (17) is connected to the top of the inside of the preparation chamber (2). The bottom of the spiral conveying pipe (17) extends to the outside of the outer chamber (16). An air pump (3) is installed at the top of the annular support platform (5), and the input end of the air pump (3) is connected to the top of the inside of the outer chamber (16). A preheating component (6) is provided at the top of the inside of the preparation chamber (2). A stirring assembly (7) is provided at the bottom of the preparation chamber (2), an auxiliary heating assembly (8) is provided at the top of the distillation chamber (4), an annular insulation layer (14) is installed on the outside of the distillation chamber (4), a first annular electric heating plate (23) is installed at the bottom of the outside of the distillation chamber (4), a drive motor (10) is installed at an angle at the middle position of the outside of the annular insulation layer (14), and the output end of the drive motor (10) extends into the inside of the distillation chamber (4) and is equipped with a first stirring paddle (22). A control panel (13) is installed at the bottom of the outside of a set of support columns (11). The stirring assembly (7) includes a circular partition (701), a rotating shaft (702), a universal joint (703), an auxiliary stirring paddle (704), a second stirring paddle (705), a drive gear (706), a transmission gear (707), a driven gear (708), and a second annular electric heating plate (709). The circular partition (701) is installed in the middle of the preparation chamber (2), and four sets of rotating shafts (702) are evenly arranged at the top edge of the circular partition (701). The bottom end of the rotating shaft (702) is equipped with an auxiliary stirring paddle through the universal joint (703). (704), the bottom end of the outer side of the rotating rod (9) passes through the circular partition (701) and is equipped with a second stirring paddle (705). A drive gear (706) is installed at the middle position of the outer side of the rotating rod (9). Four sets of transmission gears (707) that mesh with the drive gear (706) are evenly arranged at the non-center position of the top of the circular partition (701). Driven gears (708) that mesh with the transmission gears (707) are installed at the top of the outer side of the four sets of rotating shafts (702). A second annular electric heating plate (709) is installed at the bottom of the outer side of the preparation chamber (2). The auxiliary stirring paddle (704) is equipped with a first bearing at the bottom of its outer side, and the outer side of the first bearing is fixedly connected to the bottom of the distillation chamber (4) at a non-central position. A second bearing is installed at the center of the top of the circular partition (701), and a third bearing is installed at the inner top and inner bottom of the first isolation tube (24). The inner sides of the third bearing and the second bearing are fixedly connected to the outer side of the rotating rod (9).

2. The continuous reaction apparatus for preparing bis(fluorosulfonyl)imide according to claim 1, characterized in that: The preheating assembly (6) includes a preheating chamber (601), a second isolation tube (602), a rotating frame (603), a stirring rod (604), and a fourth solenoid valve (605). The preheating chamber (601) is located at the top of the preparation chamber (2). The second isolation tube (602) is installed at the center of the bottom of the preheating chamber (601), and the second isolation tube (602) is sleeved on the outside of the rotating rod (9). Four sets of rotating frames (603) are evenly installed at the middle of the outside of the rotating rod (9). The stirring rod (604) is evenly installed at the bottom of the rotating frame (603). Three sets of fourth solenoid valves (605) are evenly installed at the edge of the bottom of the preheating chamber (601).

3. The continuous reaction apparatus for preparing bis(fluorosulfonyl)imide according to claim 2, characterized in that: The auxiliary heating assembly (8) includes a heating chamber (801), an air inlet (802), a spiral guide plate (803), a through hole (804), and a connecting conduit (805). The heating chamber (801) is installed in the middle of the interior of the distillation chamber (4), and a spiral guide plate (803) adapted to the bottom of the preparation chamber (2) is installed inside the heating chamber (801). The air inlet (802) is evenly opened at the non-center position of the bottom of the heating chamber (801), and a through hole (804) is opened at the center position of the bottom of the heating chamber (801). A connecting conduit (805) is installed at the top of one side of the heating chamber (801), and the top of the connecting conduit (805) is connected to the inner bottom of the outer chamber (16).

4. The continuous reaction apparatus for preparing bis(fluorosulfonyl)imide according to claim 3, characterized in that: The thickness of the bottom of the preheating chamber (601) gradually increases from the edge to the center. A fourth bearing is installed at the center of the bottom of the preheating chamber (601), and the inner side of the fourth bearing is fixedly connected to the outer side of the rotating rod (9).

5. The continuous reaction apparatus for preparing bis(fluorosulfonyl)imide according to claim 1, characterized in that: The bottom of the top cover (1) and the top of the preparation chamber (2) are symmetrically equipped with first flanges, and several sets of first fixing bolts are provided on the two sets of first flanges.

6. The continuous reaction apparatus for preparing bis(fluorosulfonyl)imide according to claim 1, characterized in that: A second flange is installed at the middle position outside the preparation chamber (2), and several sets of second fixing bolts are provided on the second flange to be fixedly connected to the top of the annular support platform (5).

7. A method for preparing bis(fluorosulfonyl)imide, comprising using the continuous reaction apparatus for preparing bis(fluorosulfonyl)imide as described in claim 4, wherein the preparation method comprises the following steps: First, the two raw materials are conveyed into the preheating chamber (601) and the upper cover (1) respectively through the spiral conveying pipe (17) and the feeding pipe (18). Then, the raw materials inside the upper cover (1) also flow into the preheating chamber (601) through the second solenoid valve (15).

2. Control the servo motor (19) to drive the rotating rod (9) to rotate clockwise at a uniform speed. The rotating rod (9) also drives the rotating frame (603) and the stirring rod (604) to perform preliminary stirring of the mixed raw materials inside the preheating chamber (601). Third, the rotating rod (9) drives the four sets of auxiliary stirring paddles (704) to work with the second stirring paddle (705) to perform secondary stirring of the mixed raw materials at the bottom of the preparation chamber (2) through the transmission of the driving gear (706), the transmission gear (707) and the driven gear (708). During the process, the second annular electric heating plate (709) is controlled to heat the mixed raw materials at the bottom of the preparation chamber (2) to separate the gas and liquid. The separated gas is discharged into the external environment through the spiral heat pipe (20). Fourth, open the third solenoid valve (21) to discharge the remaining liquid raw material at the bottom of the preparation chamber (2) into the interior of the distillation chamber (4), and then control the first annular electric heating plate (23) to heat the liquid raw material inside the distillation chamber (4) and distill it.

5. Control the drive motor (10) to drive the first stirring paddle (22) to stir the liquid raw material inside the distillation chamber (4); 6. Next, control the air pump (3) to evacuate the air inside the outer chamber (16). The water vapor generated by distillation inside the distillation chamber (4) enters the heating chamber (801) through the air inlet (802) and is finally discharged to the external environment through the output end of the air pump (3). After the liquid raw material inside the distillation chamber (4) is distilled, open the first solenoid valve (12) to discharge the distilled difluorosulfonamide.

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