A preparation device and method for lithium bis(fluorosulfonyl)imide

Abstract

The invention discloses a preparation device and method for lithium bis(fluorosulfonyl)imide, belonging to the technical field of lithium bis(fluorosulfonyl)imide preparation. The invention comprises a base; a reactor, which is arranged at the center position above the base; a fixed plate of an annular structure is fixedly connected to the annular outer side surface of the reactor near the lower position; the lower end surface of the fixed plate is fixedly connected to the base through four pillars distributed in an annular manner and equidistantly; a cover plate is provided on the upper end cover of the reactor; three barrels are fixedly connected to the upper end surface of the cover plate near the outer edge position and equidistantly in an annular manner; a feed pipe at the bottom of the barrel runs through the reactor; raw materials are input into the reactor through the barrel to prepare lithium bis(fluorosulfonyl)imide; in the scheme, an arc notch is provided on the sub-gear, so that the amount of raw materials entering the hopper can be controlled, so as to avoid accumulation and agglomeration of raw materials caused by excessive input at one time; and the raw materials are fully stirred with a stirring paddle on the lower end surface of the sub-gear, so as to improve the effect of initial stirring and mixing of the raw materials.

Description

Technical Field

[0001] The invention relates to the technical field of lithium bis(fluorosulfonyl)imide preparation, and more specifically to a preparation device and method for lithium bis(fluorosulfonyl)imide. Background Art

[0002] Lithium bis(fluorosulfonyl)imide (Li[N(SO2F)2], abbreviated as LiFSI) is a very important lithium battery electrolyte additive. It has the advantages of high conductivity, good thermal stability, high electrochemical stability, good cycle performance and good safety performance. Compared with the most widely used LiPF6, it has many excellent properties and is a better choice for lithium battery electrolytes.

[0003] At present, lithium bis(fluorosulfonyl)imide is mainly prepared by aminosulfonic acid, chlorosulfonic acid and dichlorothionyl. In the process of preparing lithium bis(fluorosulfonyl)imide, the reaction process is too long, resulting in excessive waste, which is not conducive to the mass production of lithium bis(fluorosulfonyl)imide.

[0004] In response to the above problems, the existing patent announcement number: CN113716534B discloses a device and method for preparing lithium bis(fluorosulfonyl)imide, and provides a technical solution, which uses a driving motor to drive the second transmission wheel to rotate, and realizes the rotation of the first transmission wheel through a transmission belt. The rotation of the first transmission wheel can drive the hollow rod to rotate, thereby causing the stirring blade to rotate, thereby achieving the effect of preliminary stirring reaction.

[0005] However, since aminosulfonic acid has a crystalline structure, the raw materials are only initially stirred by the stirring blades on the hollow rod, which results in poor mixing effect of aminosulfonic acid, chlorosulfonic acid and dichlorothionyl, so that the raw materials are easily sticked into lumps. When the lumps of raw materials enter the bottom of the reactor through the discharge port, the gas ejected from the jet holes on the annular tube is difficult to drive the lumps of raw materials to roll, so that the lumps of raw materials fall to the bottom of the reactor before they are stirred and mixed, thereby reducing the mixing effect of the raw materials and further reducing the preparation quality of lithium bis(fluorosulfonyl)imide. Summary of the invention

[0006] The object of the present invention is to provide a preparation device and method for lithium bis(fluorosulfonyl)imide to solve the problems raised in the above background technology.

[0007] To solve the above problems, the present invention adopts the following technical solutions.

[0008] A preparation device for lithium bis(fluorosulfonyl)imide, comprising a base;

[0009] The reaction kettle is arranged at the center position above the base, and a fixing plate of an annular structure is fixedly connected to the annular outer side surface of the reaction kettle near the lower position, and the lower end surface of the fixing plate is fixedly connected to the base through four supporting pillars distributed in an annular manner at equal intervals;

[0010] The upper end cover of the reactor is provided with a cover plate, and three barrels are fixedly connected to the upper end surface of the cover plate near the outer edge at an annular equidistant position, and a feed pipe at the bottom of the barrel runs through the reactor, and the raw materials are fed into the reactor through the barrel to prepare lithium bis(fluorosulfonyl)imide;

[0011] The mixing mechanism is used to stir and mix the raw materials input into the reactor to prevent the raw materials from sticking together into a lump, and includes a motor fixed at the center of the upper end surface of the cover plate, the output shaft of the motor passes through the cover plate and is fixedly connected to the drive shaft, and three rotating stirring paddles are equidistantly arranged in a ring at a level with the upper end of the drive shaft.

[0012] Furthermore, a main gear is fixedly sleeved on the upper end of the annular outer surface of the drive shaft, and three sub-gears are equidistantly meshed in an outer ring of the main gear. The sub-gears are rotatably connected to the upper end surface of the cover plate through a rotating shaft, and the stirring paddles are rotatably connected to the center position of the lower end surface of the sub-gears, and arc-shaped grooves are provided on the upper end surfaces of the sub-gears near the outer edges.

[0013] Furthermore, a hopper with a funnel-shaped structure is fixedly connected to the inner wall of the reactor below the stirring paddle, the driving shaft passes through a material guide pipe at the center of the hopper, and a spiral blade is fixedly connected to the annular outer surface of the driving shaft located inside the material guide pipe, and the driving shaft is fixedly connected to two scrapers matching the inner wall of the hopper on the annular outer surface symmetrically along the radial direction of 180°.

[0014] Furthermore, the annular outer side surface of the drive shaft is located between the hopper and the bottom of the reactor, and three conical disks forming a "pagoda" shaped structure are vertically and equidistantly fixedly connected thereto; the inner wall of the reactor is fixedly connected with a slow flow plate corresponding to each conical disk; the slow flow plate is concave near the edge of the lower end of the conical disk, and a number of leakage holes are equidistantly provided in an annular shape at the bottom of the concave structure of the slow flow plate; the conical outer side surfaces of the conical disks are all annularly and equidistantly fixedly connected with protrusions with a triangular cross-section.

[0015] Furthermore, a volute is provided below the reactor, and the annular outer side surface of the volute is fixedly connected to four pillars through four fixing rods, and the lower end of the drive shaft passes through the interior of the volute and is fixedly connected to a turbine.

[0016] Furthermore, a sealing cover is provided on the annular outer surface of the drive shaft between the volute and the bottom of the reactor through a sealing bearing rotating sleeve, the upper end of the sealing cover is fixedly connected to the bottom of the reactor, and the sealing cover is connected to the annular outer surface of the volute through an air pipe.

[0017] Furthermore, a guide hole extending to the uppermost conical disk is provided at the center of the driving shaft in the sealing cover, an air inlet hole connected to the guide hole is provided on the annular outer surface of the driving shaft in the sealing cover, each of the conical disks has a cavity structure inside, and diversion holes connected to the conical disks at corresponding positions are respectively provided on the inner walls of the guide holes, and jet holes distributed in a spiral pattern are provided on the conical outer surface of each conical disk.

[0018] Furthermore, three U-shaped suction pipes are equidistantly arranged on the annular outer side surface of the reactor near the upper end, the upper end openings of the suction pipes are respectively connected to the reactor above the hopper, the lower end openings of the suction pipes are respectively connected to the reactor below the hopper, the center positions of the vertical parts of the suction pipes are respectively connected to the reactor through a branch pipe, the reactor is fixedly connected to an absorption box on the annular outer side surface below the suction pipe, and the lower horizontal part of the suction pipe is connected to the absorption box through a guide pipe.

[0019] Furthermore, a turntable with a circular ring structure is provided on the outer side of the material guide pipe at the center of the hopper, and the lower end surface of the turntable is fixedly connected to the drive shaft near the inner edge through three equidistantly distributed support rods, and the lower end surface of the turntable is provided with a track with a "hexagonal star" structure, and a movable rod with an "L"-shaped structure is slidably inserted inside the lower horizontal part of the suction pipe, one end of the movable rod located in the suction pipe is fixedly connected to a piston, and the other end of the movable rod is located in the track, and a fixing ring is fixedly connected to the lower end of the suction pipe, and the movable rod is slidably inserted in the fixing ring.

[0020] A method for preparing lithium bis(fluorosulfonyl)imide comprises the following steps:

[0021] S1: Load the raw materials into the barrel respectively, then start the motor to drive the drive shaft to rotate, thereby driving the main gear to rotate, and then driving the three sub-gears to rotate synchronously, so that the stirring paddle under the sub-gear rotates continuously, and the notch on the sub-gear can intermittently open the discharge pipe at the lower end of the barrel, so as to perform intermittent discharge, avoiding too much raw material being put in at one time to affect the mixing effect;

[0022] S2: The rotation of the drive shaft drives the turbine in the volute to rotate, so that the turbine generates centrifugal force to suck the outside air into the volute, and then inputs it into the sealing cover through the air pipe. The air entering the sealing cover enters the guide hole through the air inlet hole, and then enters the three conical disks through the diversion hole, and finally ejects through the jet hole on the conical disk, thereby driving the falling raw materials to tumble and mix, improving the mixing effect;

[0023] S3: The rotation of the drive shaft will also drive the turntable to rotate, thereby driving the piston to reciprocate inside the lower horizontal part of the intake pipe, and then the hydrogen chloride gas and hydrogen fluoride gas generated in the preparation process of lithium bis(fluorosulfonyl)imide in the reactor are sucked into the intake pipe, and then the hydrogen chloride gas and hydrogen fluoride gas are introduced into the absorption box to prevent atmospheric pollution.

[0024] Compared with the prior art, the advantages of the present invention are:

[0025] 1. This solution controls the amount of raw materials entering the hopper by opening an arc-shaped notch on the secondary gear, avoiding accumulation and agglomeration of raw materials caused by excessive input at one time. The stirring paddle on the lower end of the secondary gear is then used to fully stir the raw materials, thereby improving the effect of initial stirring and mixing of the raw materials.

[0026] 2. This solution drives the driving shaft to rotate through an electrical appliance to drive the sub-gear to rotate while driving the turbine in the volute to rotate, so that the turbine generates centrifugal force to suck the outside air into the volute, and then inputs it into the sealing cover through the air pipe. The air entering the sealing cover enters the guide hole through the air inlet hole, and then enters the three conical disks through the diversion hole, and finally is ejected through the jet hole on the conical disk, thereby driving the falling raw materials to tumble and mix, thereby improving the mixing effect, and then improving the quality of lithium bis(fluorosulfonyl)imide.

[0027] 3. In this solution, the driving shaft rotates and drives the piston to reciprocate inside the lower horizontal part of the intake pipe, thereby sucking the hydrogen chloride gas and hydrogen fluoride gas generated in the preparation process of lithium bis(fluorosulfonyl)imide in the reactor into the intake pipe, and then introducing the hydrogen chloride gas and hydrogen fluoride gas into the absorption box through the guide pipe for absorption treatment to prevent pollution of the atmosphere. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a front perspective view of the overall structure of the present invention;

[0029] Figure 2 It is a bottom-up stereoscopic diagram of the overall structure of the present invention;

[0030] Figure 3 For the present invention Figure 1 A half-section diagram of

[0031] Figure 4 For the present invention Figure 2 A half-section diagram of

[0032] Figure 5 For the present invention Figure 3 Half-section diagram of the middle hopper, conical plate and slow flow plate;

[0033] Figure 6 This is a schematic diagram of the connection relationship between the turntable and the drive shaft of the present invention;

[0034] Figure 7 For the present invention Figure 4 A in the enlarged view;

[0035] Figure 8 For the present invention Figure 5 Enlarged view of point B in .

[0036] Description of the numbers in the figure:

[0037] 1. Base; 11. Fixed plate; 12. Pillar; 2. Reactor; 21. Cover plate; 22. Cylinder; 3. Motor; 31. Drive shaft; 32. Main gear; 33. Sub gear; 34. Notch; 35. Agitator; 36. Scraper; 37. Hopper; 38. Spiral blade; 4. Turntable; 41. Track; 42. Suction pipe; 43. Branch pipe; 44. Guide pipe; 45. Absorption box; 46. Movable rod; 47. Fixed ring; 48. Piston; 49. Support rod; 5. Conical disk; 51. Bump; 52. Slow flow plate; 53. Leakage hole; 54. Inlet hole; 55. Guide hole; 56. Diverter hole; 57. Jet hole; 6. Volute; 61. Turbine; 62. Air pipe; 63. Sealing cover. DETAILED DESCRIPTION

[0038] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments, and all other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making creative work are within the scope of protection of the present invention.

[0039] See also Figure 1-Figure 5 , a preparation device for lithium bis(fluorosulfonyl)imide, comprising a base 1, a reactor 2 is arranged at the center position above the base 1, a fixed plate 11 of an annular structure is fixedly connected to the annular outer side surface of the reactor 2 near the lower position, the lower end surface of the fixed plate 11 is fixedly connected to the base 1 through four pillars 12 distributed in an annular manner, a cover plate 21 is arranged on the upper end cover of the reactor 2, three barrels 22 are fixedly connected in an annular manner near the outer edge of the upper end surface of the cover plate 21, a feed pipe at the bottom of the barrel 22 penetrates into the reactor 2, a mixing mechanism is arranged in the reactor 2, the mixing mechanism comprises a motor 3 fixed at the center position of the upper end surface of the cover plate 21, the output shaft of the motor 3 penetrates the cover plate 21 and is fixedly connected to a driving shaft 31, and three self-rotating stirring paddles 35 are arranged in an annular manner and equidistantly in a position flush with the upper end of the driving shaft 31;

[0040] A main gear 32 is fixedly sleeved on the upper end of the annular outer surface of the driving shaft 31, and three sub-gears 33 are meshed in an annular manner at equal intervals on the outer side of the main gear 32. The sub-gear 33 is rotatably connected to the upper end surface of the cover plate 21 through a rotating shaft, and the stirring paddles 35 are rotatably connected to the center position of the lower end surface of the sub-gear 33 respectively. The upper end surface of the sub-gear 33 is provided with arc-shaped notches 34 near the outer edge, and a funnel-shaped hopper 37 is fixedly connected to the inner wall of the reactor 2 below the stirring paddle 35. The driving shaft 31 passes through a material guide pipe at the center position of the hopper 37, and a spiral blade 38 is fixedly connected to the annular outer surface of the driving shaft 31 located inside the material guide pipe, and two scrapers 36 matching the inner wall of the hopper 37 are fixedly connected to the annular outer side surface of the driving shaft 31 symmetrically along the radial direction of 180°.

[0041] When the above scheme is implemented, the raw materials for preparing lithium bis(fluorosulfonyl)imide are placed in the barrel 22 respectively, and then the motor 3 is started to drive the drive shaft 31 to rotate, thereby driving the main gear 32 to rotate, and then driving the three sub-gears 33 to rotate in the hopper 37. Since the upper end surfaces of the three sub-gears 33 are provided with arc-shaped notches 34 near the outer edge, and the lower end openings of the three discharge pipes at the bottom of the barrel 22 are respectively fitted with the upper end surfaces of the sub-gears 33, when the notches 34 on the sub-gears 33 pass through the lower end openings of the discharge pipes at the bottom of the barrel 22, the raw materials in the barrel 22 can enter the hopper 37 through the notches 34, thereby forming an intermittent feeding effect. Since aminosulfonic acid is a crystalline structure, and chlorosulfonic acid and dichlorothionyl are liquid structures, excessive feeding at one time can easily cause aminosulfonic acid, chlorosulfonic acid and dichlorothionyl to stick to each other into a mass, and intermittent feeding. It can avoid that too much material is discharged at one time and the accumulation of raw materials affects the stirring and mixing. The rotation of the sub-gear 33 will drive the stirring paddle 35 to rotate continuously, and the driving shaft 31 is located on the annular outer surface of the hopper 37 and is vertically and equidistantly fixedly connected with a plurality of stirring blades that are staggered with the blades on the stirring paddle 35, so that the raw materials entering the hopper 37 can be fully stirred to avoid the raw materials from sticking together. During the rotation of the driving shaft 31, the scraper 36 is also driven to scrape off the raw materials attached to the inner wall of the hopper 37 and the inner wall of the reactor 2 to avoid the raw materials from adhering to the reactor 2 and the inner wall of the hopper 37 and affecting the mixing effect. The mixed raw materials are transported to the reactor 2 below the hopper 37 under the action of the spiral blades 38 for further mixing reaction. The spiral blades 38 can prevent the raw materials from clogging the material guide pipe at the center of the hopper 37.

[0042] As an embodiment of the present invention, Figure 3 , Figure 4 , Figure 5 as well as Figure 8As shown, the annular outer side surface of the drive shaft 31 is located between the hopper 37 and the bottom of the reactor 2, and three conical disks 5 forming a "pagoda" shaped structure are fixedly connected vertically and equidistantly. The inner wall of the reactor 2 corresponds to each conical disk 5 and is fixedly connected with a slow flow plate 52. The slow flow plate 52 is concave near the edge of the lower end of the conical disk 5, and a plurality of leakage holes 53 are equidistantly provided at the bottom of the concave structure of the slow flow plate 52. The conical outer side surfaces of the conical disks 5 are all annularly and equidistantly fixed with protrusions 51 with a triangular cross-section. A volute 6 is provided below the reactor 2, and the annular outer side surface of the volute 6 is fixedly connected to four pillars 12 by four fixing rods. The lower end of the drive shaft 31 passes through the interior of the volute 6 and is fixedly connected with a turbine 61. The volute 6 A sealing cover 63 is rotatably sleeved on the annular outer surface of the driving shaft 31 between the bottom of the reactor 2 through a sealing bearing, the upper end of the sealing cover 63 is fixedly connected to the bottom of the reactor 2, the sealing cover 63 is connected to the annular outer side surface of the volute 6 through an air pipe 62, a guide hole 55 extending to the position of the uppermost conical disk 5 is provided at the center of the driving shaft 31 in the sealing cover 63, an air inlet hole 54 connected to the guide hole 55 is provided on the annular outer surface of the driving shaft 31 in the sealing cover 63, each conical disk 5 has a cavity structure inside, and diverter holes 56 connected to the corresponding conical disk 5 are respectively provided on the inner wall of the guide hole 55, and each conical disk 5 is provided with jet holes 57 distributed in a spiral line on the conical outer surface.

[0043] When the above scheme is implemented, based on the above embodiment, the driving shaft 31 can simultaneously drive the turbine 61 in the volute 6 to rotate during its rotation, so that the turbine 61 generates centrifugal force, and then the outside air is sucked into the volute 6 through the air inlet at the center of the lower end surface of the volute 6. A filter is fixedly connected to the air inlet by screws, and the filter can prevent dust in the air from entering the reactor 2 and affecting the purity of lithium bis(fluorosulfonyl)imide. The air entering the volute 6 is continuously thrown onto the annular inner wall of the volute 6 under the centrifugal force of the turbine 61, so that Negative pressure is generated at the center of the turbine 61, so that the air is continuously pumped into the sealing cover 63 through the air pipe 62 under the action of the external atmospheric pressure. As the air continuously enters the sealing cover 63, the air enters the guide hole 55 inside the driving shaft 31 through the air inlet hole 54, and then flows into the three conical disks 5 through the diverter hole 56, and finally sprays upward through the jet hole 57. The raw materials flowing down through the hopper 37 first fall on the uppermost conical disk 5. During the rotation of the conical disk 5, the protrusion 51 on it will impact the raw materials, thereby throwing the raw materials away. The raw materials are then moved to the inner wall of the reactor 2, and then slide down along the inner wall of the reactor 2 to the concave surface of the uppermost slow flow plate 52. At the same time, the gas ejected from the gas jet hole 57 can drive the falling raw materials to roll, thereby improving the mixing effect. Under the blocking effect of the uppermost slow flow plate 52, the raw materials will first gradually accumulate on the concave surface of the uppermost slow flow plate 52, so that the uppermost conical disk 5 cooperates with the convex block 51 to fully stir and mix the raw materials. Since a plurality of groups of leakage holes 53 are equidistantly arranged at the bottom of the concave surface of the slow flow plate 52, the raw materials can leak downward. The speed of the raw materials entering the reactor 2 is greater than the speed of the raw materials leaking out, so that more and more raw materials are placed on the uppermost slow flow plate 52. Since there is a gap between the slow flow plate 52 and the drive shaft 31, the excess raw materials can flow downward through the gap. As the raw materials continue to flow down through the hopper 37, the raw materials are stirred and mixed by the conical disk 5 layer by layer until they flow to the bottom of the reactor 2. Since the conical disk 5 is in a "pagoda" shape from top to bottom, the stirring and mixing effect of the raw materials is improved layer by layer, and finally lithium bis(fluorosulfonyl)imide is generated, thereby improving the synthesis quality of lithium bis(fluorosulfonyl)imide.

[0044] As an embodiment of the present invention, Figure 3-Figure 7As shown, three U-shaped suction pipes 42 are equidistantly arranged on the annular outer side surface of the reactor 2 near the upper end, the upper end openings of the suction pipes 42 are respectively connected to the reactor 2 above the hopper 37, the lower end openings of the suction pipes 42 are respectively connected to the reactor 2 below the hopper 37, the center position of the vertical part of the suction pipe 42 is respectively connected to the reactor 2 through a branch pipe 43, the annular outer side surface of the reactor 2 below the suction pipe 42 is fixedly connected to an absorption box 45, the lower horizontal part of the suction pipe 42 is respectively connected to the absorption box 45 through a guide pipe 44, the center position of the hopper 37 A turntable 4 with a circular ring structure is provided on the outer side of the material guide pipe. The lower end surface of the turntable 4 is fixedly connected to the drive shaft 31 near the inner edge through three equidistant support rods 49. The lower end surface of the turntable 4 is provided with a track 41 with a "hexagonal star" structure. A movable rod 46 with an "L"-shaped structure is slidably inserted inside the lower horizontal part of the suction pipe 42. One end of the movable rod 46 located in the suction pipe 42 is fixedly connected to a piston 48, and the other end of the movable rod 46 is located in the track 41. A fixing ring 47 is fixedly connected to the lower end of the suction pipe 42, and the movable rod 46 is slidably inserted in the fixing ring 47.

[0045] When the above scheme is implemented, based on the above embodiment, since hydrogen fluoride gas is added as a reactant during the preparation of lithium bis(fluorosulfonyl)imide, hydrogen chloride gas is also produced, and excess hydrogen chloride gas and hydrogen fluoride gas will float above the hopper 37 and below the hopper 37. If they are not removed, long-term accumulation will cause corrosion to the reactor 2. Therefore, during the rotation of the drive shaft 31, the turntable 4 will be driven to rotate through the support rod 49. Under the action of the "hexagonal star" structure track 41, the movable rod 46 will reciprocate back and forth inside the lower horizontal part of the suction pipe 42. When the movable rod 46 drives When the piston 48 contracts inward, the one-way valve located on the outside of the guide pipe 44 at the lower horizontal part of the suction pipe 42 is opened, and the one-way valve in the guide pipe 44 is closed, so that the hydrogen chloride gas and hydrogen fluoride gas floating above the hopper 37 are sucked into the lower horizontal part of the suction pipe 42 through the upper horizontal part of the suction pipe 42 by suction force, and the hydrogen chloride gas and hydrogen fluoride gas floating on the lower side of the hopper 37 are sucked into the lower horizontal part of the suction pipe 42 through the branch pipe 43. When the movable rod 46 drives the piston 48 to expand outward, the one-way valve located on the outside of the guide pipe 44 at the lower horizontal part of the suction pipe 42 is closed, and the guide pipe 44 is closed. The one-way valve in the suction pipe 42 is opened, so that the sucked hydrogen chloride gas and hydrogen fluoride gas are pressed into the absorption box 45 through the guide pipe 44 by pressure. The absorption box 45 contains absorption liquid. The lower end of the guide pipe 44 is lower than the liquid level to prevent the hydrogen chloride gas and hydrogen fluoride gas from escaping from the absorption box 45 and polluting the atmosphere. The hydrogen chloride gas and hydrogen fluoride gas are absorbed by the absorption liquid, thereby preventing the hydrogen chloride gas and hydrogen fluoride gas from corroding the equipment and avoiding the direct discharge of the hydrogen chloride gas and hydrogen fluoride gas to pollute the atmosphere. When the suction pipe 42 sucks the hydrogen chloride gas and hydrogen fluoride gas, it also sucks part of the gas ejected through the jet hole 57. Air is contained in the mixed gas entering the absorption box 45, and the air is almost insoluble in the absorption liquid, and can be discharged through the exhaust pipe on the upper end face of the absorption box 45, thereby not affecting the continuous absorption capacity of the absorption liquid for hydrogen chloride gas and hydrogen fluoride gas. A ceramic ring block is fixedly sleeved on one end of the movable rod 46 located in the track 41 to reduce the wear between the movable rod 46 and the track 41. A fixing ring 47 is fixedly connected to the pipe opening position of the horizontal part on the lower side of the intake pipe 42 to ensure that the movable rod 46 can move stably in the intake pipe 42, while preventing the movable rod 46 and the lower end pipe opening of the intake pipe 42 from wearing.

[0046] A method for preparing lithium bis(fluorosulfonyl)imide comprises the following steps:

[0047] S1: The raw materials are loaded into the barrel 22 respectively, and then the motor 3 is started to drive the driving shaft 31 to rotate, thereby driving the main gear 32 to rotate, and then driving the three sub-gears 33 to rotate synchronously, so that the stirring paddle 35 under the sub-gear 33 rotates continuously, and the notch 34 on the sub-gear 33 can intermittently open the feeding pipe at the lower end of the barrel 22, so as to perform intermittent feeding, so as to avoid too much raw material being put in at one time to affect the mixing effect;

[0048] S2: The rotation of the drive shaft 31 drives the turbine 61 in the volute 6 to rotate, so that the turbine 61 generates centrifugal force to suck the outside air into the volute 6, and then inputs it into the sealing cover 63 through the air pipe 62. The air entering the sealing cover 63 enters the guide hole 55 through the air inlet hole 54, and then enters the three conical disks 5 through the diverter hole 56, and finally ejects through the jet hole 57 on the conical disk 5, thereby driving the falling raw materials to tumble and mix, thereby improving the mixing effect;

[0049] S3: During the rotation of the drive shaft 31, the turntable 4 is also driven to rotate, thereby driving the piston 48 to reciprocate inside the lower horizontal part of the intake pipe 42, and then the hydrogen chloride gas and hydrogen fluoride gas generated in the preparation process of lithium bis(fluorosulfonyl)imide in the reactor 2 are sucked into the intake pipe 42, and then the hydrogen chloride gas and hydrogen fluoride gas are introduced into the absorption box 45 to prevent pollution of the atmosphere.

[0050] Working principle: The raw materials for preparing lithium bis(fluorosulfonyl)imide are placed in the barrel 22 respectively, and then the motor 3 is started to drive the driving shaft 31 to rotate, thereby driving the three sub-gears 33 to rotate in the hopper 37, so that when the notch 34 on the sub-gear 33 passes through the lower end of the discharge pipe at the bottom of the barrel 22, the raw materials in the barrel 22 enter the hopper 37 through the notch 34, thereby forming an intermittent feeding effect. Intermittent feeding can avoid excessive feeding at one time causing raw material accumulation and affecting stirring and mixing. During the self-rotation of the sub-gear 33, the stirring paddle 35 will be driven to rotate continuously, and the driving shaft 31 is located at A plurality of groups of stirring blades interlaced with the blades on the stirring paddle 35 are vertically and equidistantly fixedly connected to the annular outer surface of the hopper 37, so that the raw materials entering the hopper 37 are fully stirred to prevent the raw materials from sticking together. During the rotation of the drive shaft 31, the scraper 36 is driven to scrape off the raw materials attached to the inner wall of the hopper 37 and the inner wall of the reactor 2 to prevent the raw materials from adhering to the reactor 2 and the inner wall of the hopper 37 and affecting the mixing effect. The mixed raw materials are transported to the reactor 2 below the hopper 37 under the action of the spiral blades 38 for further mixing reaction.

[0051] During the rotation of the driving shaft 31, the turbine 61 in the volute 6 can be driven to rotate at the same time, so that the turbine 61 generates centrifugal force, and then the outside air is sucked into the volute 6 through the air inlet at the center of the lower end surface of the volute 6. The air entering the volute 6 is continuously pumped into the sealing cover 63 through the air pipe 62. As the air continues to enter the sealing cover 63, the air will enter the guide hole 55 inside the driving shaft 31 through the air inlet hole 54, and then flow into the three conical disks 5 through the diverter hole 56 respectively, and finally sprayed upward through the jet hole 57. The raw materials flowing down through the hopper 37 first fall on the uppermost conical disk 5, and the conical disk 5 rotates. During the process, the protrusion 51 on it will impact the raw material, so that the raw material is thrown onto the inner wall of the reactor 2, and slides down along the inner wall of the reactor 2 to the concave surface of the uppermost slow flow plate 52. At the same time, the gas ejected from the gas jet hole 57 can drive the falling raw material to roll, thereby improving the mixing effect. As the raw material continues to flow down through the hopper 37, the raw material will be stirred and mixed by the conical disk 5 layer by layer until it flows to the bottom of the reactor 2. Since the conical disk 5 is a "pagoda"-shaped structure from top to bottom, the stirring and mixing effect of the raw material can be improved layer by layer, and finally lithium bis(fluorosulfonyl)imide is generated, thereby improving the synthesis quality of lithium bis(fluorosulfonyl)imide.

[0052] Since hydrogen fluoride gas is added as a reactant during the preparation of lithium bis(fluorosulfonyl)imide, hydrogen chloride gas is also produced. Excessive hydrogen chloride gas and hydrogen fluoride gas will float above and below the hopper 37. If they are not removed, long-term accumulation will cause corrosion to the reactor 2. Therefore, during the rotation of the drive shaft 31, the turntable 4 will be driven to rotate through the support rod 49. Under the action of the "hexagonal star" structure track 41, the movable rod 46 will reciprocate back and forth inside the lower horizontal part of the suction pipe 42. When the movable rod 46 drives the piston 48 to retract inward, the one-way valve located on the outside of the guide pipe 44 at the lower horizontal part of the suction pipe 42 is opened, and the one-way valve in the guide pipe 44 is closed, so that the hydrogen chloride gas and hydrogen fluoride gas floating above the hopper 37 are sucked into the lower horizontal part of the suction pipe 42 through the upper horizontal part of the suction pipe 42 by suction, and the floating hydrogen chloride gas and hydrogen fluoride gas at the lower side of the hopper 37 are sucked into the lower horizontal part of the suction pipe 42 through the branch pipe 43. Hydrogen chloride gas and hydrogen fluoride gas are sucked into the lower horizontal part of the intake pipe 42. When the movable rod 46 drives the piston 48 to expand outward, the one-way valve located on the outer side of the guide pipe 44 at the lower horizontal part of the intake pipe 42 is closed, and the one-way valve in the guide pipe 44 is opened, so that the sucked hydrogen chloride gas and hydrogen fluoride gas are pressed into the absorption box 45 through the guide pipe 44 by pressure, and the hydrogen chloride gas and hydrogen fluoride gas are absorbed by the absorption liquid, so as to prevent the hydrogen chloride gas and hydrogen fluoride gas from corroding the equipment, and at the same time, avoid direct discharge of hydrogen chloride gas and hydrogen fluoride gas to pollute the atmosphere. A ceramic annular block is fixedly sleeved at one end of the movable rod 46 located in the track 41 to reduce the wear between the movable rod 46 and the track 41. A fixed ring 47 is fixedly connected to the pipe mouth position of the lower horizontal part of the intake pipe 42 to ensure that the movable rod 46 can move stably in the intake pipe 42, and at the same time, prevent the movable rod 46 and the lower end pipe mouth of the intake pipe 42 from being worn.

[0053] The above is only a preferred specific implementation of the present invention; however, the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solution and its improved conception within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A preparation device for lithium bis(fluorosulfonyl)imide, characterized in that: comprising a base (1); A reaction kettle (2) is arranged at a central position above the base (1); a fixing plate (11) of an annular structure is fixedly connected to the annular outer side surface of the reaction kettle (2) near the lower position; the lower end surface of the fixing plate (11) is fixedly connected to the base (1) via four supporting columns (12) equidistantly distributed in an annular manner; The upper end cover of the reaction kettle (2) is provided with a cover plate (21), and three barrels (22) are fixedly connected to the upper end surface of the cover plate (21) at equal intervals in an annular manner near the outer edge thereof, and a feed pipe at the bottom of the barrel (22) penetrates into the interior of the reaction kettle (2), and raw materials are fed into the reaction kettle (2) through the barrel (22) to prepare lithium bis(fluorosulfonyl)imide; A mixing mechanism, used for stirring and mixing raw materials input into the reaction kettle (2) to prevent the raw materials from sticking together into a mass, comprising a motor (3) fixed at the center of the upper end surface of the cover plate (21), the output shaft of the motor (3) passing through the cover plate (21) and fixedly connected to a drive shaft (31), and three stirring paddles (35) capable of self-rotation are provided in an annular manner and equidistantly in a position flush with the upper end of the drive shaft (31); A main gear (32) is fixedly sleeved on the upper end of the annular outer surface of the drive shaft (31), and three auxiliary gears (33) are equidistantly meshed on the outer side of the main gear (32). The auxiliary gears (33) are rotatably connected to the upper end surface of the cover plate (21) via a rotating shaft, and the stirring paddles (35) are respectively rotatably connected to the center of the lower end surface of the auxiliary gears (33). The upper end surfaces of the auxiliary gears (33) are each provided with arc-shaped notches (34) near the outer edges; A hopper (37) with a funnel-shaped structure is fixedly connected to the inner wall of the reactor (2) below the stirring paddle (35); the driving shaft (31) passes through a material guide tube at the center of the hopper (37); a spiral blade (38) is fixedly connected to the annular outer surface of the driving shaft (31) located inside the material guide tube; and two scrapers (36) matching the inner wall of the hopper (37) are fixedly connected to the annular outer surface of the driving shaft (31) symmetrically at 180° in the radial direction; The annular outer side surface of the drive shaft (31) is located between the hopper (37) and the bottom of the reactor (2), and three conical disks (5) forming a "pagoda" structure are fixedly connected vertically and equidistantly. The inner wall of the reactor (2) is fixedly connected to a slow flow plate (52) corresponding to each conical disk (5). The slow flow plate (52) is concave near the lower edge of the conical disk (5), and a plurality of leak holes (53) are equidistantly provided at the bottom of the concave structure of the slow flow plate (52). The conical outer side surfaces of the conical disks (5) are all fixedly connected to protrusions (51) with a triangular cross-section at annular and equidistant intervals. A volute (6) is provided below the reactor (2), and the annular outer side surface of the volute (6) is fixedly connected to four pillars (12) via four fixing rods; the lower end of the drive shaft (31) passes through the interior of the volute (6) and is fixedly connected to a turbine (61); A sealing cover (63) is provided on the annular outer surface of the drive shaft (31) between the volute (6) and the bottom of the reactor (2) via a sealing bearing rotatable sleeve, the upper end of the sealing cover (63) is fixedly connected to the bottom of the reactor (2), and the sealing cover (63) is connected to the annular outer surface of the volute (6) via an air delivery pipe (62); A guide hole (55) extending to the position of the uppermost conical disk (5) is provided at the center of the drive shaft (31) located in the sealing cover (63); an air inlet hole (54) communicating with the guide hole (55) is provided on the annular outer surface of the drive shaft (31) located in the sealing cover (63); each of the conical disks (5) has a cavity structure inside, and a flow diversion hole (56) communicating with the conical disk (5) at a corresponding position is provided on the inner wall of the guide hole (55); and each of the conical disks (5) has a spirally distributed jet hole (57) provided on the conical outer surface.

2. The preparation equipment of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: Three U-shaped air intake pipes (42) are equidistantly arranged on the annular outer side surface of the reactor (2) near the upper end thereof; the upper end openings of the air intake pipes (42) are respectively connected to the reactor (2) above the hopper (37); the lower end openings of the air intake pipes (42) are respectively connected to the reactor (2) below the hopper (37); the central position of the vertical portion of the air intake pipe (42) is respectively connected to the reactor (2) via a branch pipe (43); an absorption box (45) is fixedly connected to the annular outer side surface of the reactor (2) below the air intake pipe (42); and the lower horizontal portion of the air intake pipe (42) is respectively connected to the absorption box (45) via a guide pipe (44).

3. The preparation equipment of lithium bis(fluorosulfonyl)imide according to claim 2, characterized in that: A rotating disk (4) with an annular structure is provided on the outside of the guide tube at the center of the hopper (37); the lower end surface of the rotating disk (4) is fixedly connected to the drive shaft (31) through three equally spaced support rods (49) near the inner edge; the lower end surface of the rotating disk (4) is provided with a track (41) with a "hexagonal star" structure; a movable rod (46) with an "L"-shaped structure is slidably inserted into the lower horizontal portion of the suction pipe (42); one end of the movable rod (46) located in the suction pipe (42) is fixedly connected to a piston (48); the other end of the movable rod (46) is located in the track (41); a fixed ring (47) is fixedly connected to the lower end of the suction pipe (42); and the movable rod (46) is slidably inserted into the fixed ring (47).

4. A method for preparing a lithium bis(fluorosulfonyl)imide device according to claim 3, characterized in that: The following steps are involved: S1: The raw materials are respectively loaded into the barrel (22), and then the motor (3) is started to drive the driving shaft (31) to rotate, thereby driving the main gear (32) to rotate, and then driving the three sub-gears (33) to rotate synchronously, so that the stirring paddle (35) below the sub-gear (33) rotates continuously, and the notch (34) on the sub-gear (33) can intermittently open the discharge pipe at the lower end of the barrel (22), so as to perform intermittent discharge, thereby avoiding too much raw material being added at one time and affecting the mixing effect; S2: The rotation of the drive shaft (31) drives the turbine (61) in the volute (6) to rotate, so that the turbine (61) generates centrifugal force to suck outside air into the volute (6), and then inputs the air into the sealing cover (63) through the air supply pipe (62). The air entering the sealing cover (63) enters the guide hole (55) through the air inlet hole (54), and then enters the three conical disks (5) through the flow distribution hole (56), and finally is ejected through the injection hole (57) on the conical disk (5), thereby driving the falling raw materials to tumble and mix, thereby improving the mixing effect; S3: The rotation of the drive shaft (31) also drives the turntable (4) to rotate, thereby driving the piston (48) to reciprocate inside the lower horizontal portion of the suction pipe (42), thereby sucking the hydrogen chloride gas and hydrogen fluoride gas generated in the preparation process of lithium bis(fluorosulfonyl)imide in the reaction kettle (2) into the suction pipe (42), and then introducing the hydrogen chloride gas and hydrogen fluoride gas into the absorption box (45) to prevent pollution of the atmosphere.

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