CN115518594A

CN115518594A - Preparation equipment and method of lithium bis (fluorosulfonyl) imide

Info

Publication number: CN115518594A
Application number: CN202211235981.9A
Authority: CN
Inventors: 陈建国; 刘鹏; 肖元春; 张海波
Original assignee: HUNAN HENGGUANG CHEMICAL CO Ltd
Current assignee: HUNAN HENGGUANG CHEMICAL CO Ltd
Priority date: 2022-10-10
Filing date: 2022-10-10
Publication date: 2022-12-27

Abstract

The invention discloses equipment and a method for preparing lithium bis (fluorosulfonyl) imide, belonging to the technical field of preparation of lithium bis (fluorosulfonyl) imide, and comprising a base; the reaction kettle is arranged at the center above the base, a fixed plate with an annular structure is fixedly connected to the annular outer side surface of the reaction kettle close to the lower position, and the lower end surface of the fixed plate is fixedly connected with the base through four support columns which are annularly and equidistantly distributed; reation kettle upper end cover is equipped with the apron, the apron up end is close to outer three feed cylinder of position annular equidistance fixedly connected with along, the unloading pipe of feed cylinder bottom runs through inside reation kettle, carry out the preparation of two fluorine sulfonyl imide lithium in with raw materials input reation kettle through the feed cylinder, this scheme is through offering the arc notch on the pinion, make the raw material volume that gets into in the hopper control, avoid once dropping into too much and cause the raw materials to pile up the conglomeration, the stirring rake of terminal surface carries out the intensive mixing to the raw materials under the pinion of deuterogamying, the effect that the preliminary stirring of raw materials mixes has been improved.

Description

Preparation equipment and method of lithium bis (fluorosulfonyl) imide

Technical Field

The invention relates to the technical field of preparation of lithium bis (fluorosulfonyl) imide, and in particular relates to equipment and a method for preparing lithium bis (fluorosulfonyl) imide.

Background

Lithium bis (fluorosulfonyl) imide (Li [ N (SO 2F) 2], abbreviated as LiFSI), is a very important lithium battery electrolyte additive, has the advantages of high conductivity, good thermal stability, high electrochemical stability, good cycle performance, good safety performance and the like, has various excellent performances compared with LiPF6 which is the most widely used currently, and is a more preferable object of lithium battery electrolytes.

At present, the lithium bis (fluorosulfonyl) imide is mainly prepared from sulfamic acid, chlorosulfonic acid and thionyl chloride, and in the process of preparing and producing the lithium bis (fluorosulfonyl) imide, excessive waste is caused due to overlong reaction flow, so that the mass production of the lithium bis (fluorosulfonyl) imide is not facilitated.

In view of the above problems, the prior patent publication No.: CN113716534B discloses a device and a method for preparing lithium bis (fluorosulfonyl) imide, which provides a technical solution, wherein a driving motor is used to drive a second driving wheel to rotate, and a driving belt is used to realize the rotation of a first driving wheel, and the rotation of the first driving wheel can drive a hollow rod to rotate, so that a stirring blade rotates, and an effect of preliminary stirring reaction is achieved.

However, because sulfamic acid is crystal structure, only lean on the stirring leaf on the hollow rod to carry out preliminary mixing to the raw materials, make sulfamic acid and chlorosulfonic acid and thionyl chloride's mixed effect relatively poor, thereby easy bonding becomes the bulk, when the raw materials of bulk pass through the leakage fluid dram and get into the reation kettle below, gas that fumarole spun on the ring channel is difficult to drive the bulk raw materials and roll, make the picture form raw materials not reach the stirring and mix and just fall to the reation kettle bottom, thereby reduce the mixed effect of raw materials, and then reduce the quality in preparation of lithium bis fluoro sulfonyl imide.

Disclosure of Invention

The invention aims to provide equipment and a method for preparing lithium bis (fluorosulfonyl) imide, so as to solve the problems in the background art.

In order to solve the above problems, the present invention adopts the following technical solutions.

A preparation device of lithium bis (fluorosulfonyl) imide comprises a base;

the reaction kettle is arranged at the central position above the base, a fixed plate with an annular structure is fixedly connected to the annular outer side surface of the reaction kettle at a position close to the lower position, and the lower end surface of the fixed plate is fixedly connected with the base through four pillars which are annularly and equidistantly distributed;

the upper end cover of the reaction kettle is provided with a cover plate, the upper end surface of the cover plate is fixedly connected with three charging barrels at equal intervals in a ring shape at a position close to the outer edge, a blanking pipe at the bottom of each charging barrel penetrates into the reaction kettle, and raw materials are input into the reaction kettle through the charging barrels to prepare the lithium bis (fluorosulfonyl) imide;

mixing mechanism for stir the mixture to the inside raw materials of input reation kettle, prevent that the raw materials from bonding into the bulk, including the motor of fixing terminal surface central point on the apron, the output shaft of motor runs through apron and fixedly connected with drive shaft, with drive shaft upper end parallel and level position annular equidistance is equipped with the stirring rake of three rotation that can take place.

Further, the fixed cover in drive shaft annular lateral surface upper end is equipped with the master gear, the meshing of master gear outside annular equidistance has three pinion, the pinion rotates with the apron up end through the pivot to be connected, the stirring rake rotates with pinion lower extreme surface central point respectively and is connected, the pinion up end is close to the notch that all seted up convex structure along the position outward.

Further, a hopper of a funnel-shaped structure is fixedly connected to the inner wall of the reaction kettle below the stirring paddle, the driving shaft penetrates through the material guide pipe arranged at the center of the hopper, the driving shaft is fixedly connected to the annular outer side surface inside the material guide pipe, and the driving shaft is symmetrically and fixedly connected to two scraping plates matched with the inner wall of the hopper along the radial direction by 180 degrees and located on the annular outer side surface.

Further, drive shaft annular lateral surface is located the three toper dish that constitutes "pagoda" shape structure of the vertical equidistance fixedly connected with in position between hopper and the reation kettle bottom, the reation kettle inner wall corresponds every toper dish equal fixedly connected with bradyseism board, the bradyseism board is close to toper dish lower extreme border position department and is recessed structure, and the bottom annular equidistance of the recessed structure of bradyseism board has seted up a plurality of small opening, the equal annular equidistance fixedly connected with cross-section of toper lateral surface of toper dish is the lug of triangle-shaped structure.

Furthermore, a volute is arranged below the reaction kettle, the annular outer side surface of the volute is fixedly connected with the four supporting columns through four fixing rods, and the lower end of the driving shaft penetrates into the volute and is fixedly connected with a turbine.

Further, the sealing cover is rotatably sleeved on the outer side surface of the annular driving shaft between the volute and the bottom of the reaction kettle through the sealing bearing, the upper end of the sealing cover is fixedly connected with the bottom of the reaction kettle, and the sealing cover is communicated with the outer side surface of the annular volute through a gas conveying pipe.

Further, be located drive shaft central point in the sealed cowling puts and sets up the water conservancy diversion hole that extends to the top conical disk position, the drive shaft is located and sets up the inlet port with water conservancy diversion hole intercommunication on the annular lateral surface in the sealed cowling, every conical disk is inside all to be the cavity structure, and sets up respectively on the water conservancy diversion downthehole wall with the reposition of redundant personnel hole that corresponds position conical disk intercommunication, every all set up the fumarole that is the helix and distributes on the conical lateral surface of conical disk.

Furthermore, the annular outer side surface of the reaction kettle is provided with three air suction pipes of U-shaped structures at the position close to the upper end in an annular equidistant manner, the upper end pipe orifices of the air suction pipes are respectively communicated with the reaction kettle above the hopper, the lower end pipe orifices of the air suction pipes are respectively communicated with the reaction kettle below the hopper, the central positions of the vertical parts of the air suction pipes are respectively communicated with the reaction through a branch pipe, the reaction kettle is fixedly connected with an absorption box on the annular outer side surface below the air suction pipes, and the lower horizontal parts of the air suction pipes are respectively communicated with the absorption box through a flow guide pipe.

Furthermore, the outside that the magazine was put to hopper central point puts the position is equipped with the carousel of ring column structure, the terminal surface is close to interior edge position and is connected with drive shaft fixed connection through three equidistance branch that distributes, the lower terminal surface of carousel is close to the track of seting up "hexagonal star" shape structure, the inside slip of the downside horizontal segment of breathing pipe is pegged graft and is had the movable rod of "L" shape structure, the movable rod is located the one end fixedly connected with piston in the breathing pipe, the other end of movable rod is located the track, the lower extreme mouth of pipe position fixedly connected with solid fixed ring of breathing pipe, and the movable rod slides and inserts and establish in the solid fixed ring.

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

s1: the raw materials are respectively loaded into the charging barrels, then the motor is started to drive the driving shaft to rotate, so that the main gear is driven to rotate, the three secondary gears are driven to synchronously rotate, the stirring paddles below the secondary gears continuously rotate, and the notches in the secondary gears can intermittently open the discharging pipe at the lower end of the charging barrels, so that intermittent discharging is carried out, and the phenomenon that the mixing effect is influenced due to excessive one-time investment of forgiveness is avoided;

s2: the driving shaft can drive the turbine in the volute to rotate in the rotating process, so that the turbine generates centrifugal force to suck outside air into the volute, the outside air is input into the sealing cover through the air conveying pipe, the air entering the sealing cover enters the flow guide holes through the air inlet holes, then enters the three conical discs through the flow distribution holes respectively, and finally is ejected out through the air injection holes in the conical discs, so that falling raw materials are driven to be rolled and mixed, and the mixing effect is improved;

s3: the rotatory in-process of drive shaft still can drive the carousel rotatory to drive the inside reciprocating motion of piston at the downside horizontal part of breathing pipe, and then inhale the breathing pipe with hydrogen chloride gas and the hydrogen fluoride gas that double fluorine sulfonyl imide lithium preparation process produced in the reation kettle, in introducing the absorption box with hydrogen chloride gas and hydrogen fluoride gas again, prevent the polluted atmosphere.

Compared with the prior art, the invention has the advantages that:

1. this scheme is through seting up the arc notch on the pinion for the raw materials volume that gets into in the hopper can be controlled, avoids once dropping into too much and causes the raw materials to pile up the caking, and the stirring rake of terminal surface carries out intensive mixing to the raw materials under the pinion of deuterogamying, has improved the effect that the preliminary stirring of raw materials was mixed.

2. This scheme drives the drive shaft rotation through electrical apparatus and drives the turbine rotation in the spiral case when driving pinion rotation for the turbine produces centrifugal force and inhales the spiral case with the outside air in, in the rethread gas-supply pipe input seal cover, the air that gets into the seal cover then gets into the water conservancy diversion hole through the inlet port, again through the reposition of redundant personnel hole respectively get into three conical disk in, the fumarole blowout on the conical disk at last, thereby the raw materials that drives the whereabouts roll the mixture, the mixing effect has been improved, and then the quality of the lithium bifluorosulfonylimide is improved.

3. The inside reciprocating motion of the downside horizontal segment of this scheme drive shaft rotation simultaneously drive piston at the breathing pipe, and then inhale the breathing pipe with hydrogen chloride gas and the hydrogen fluoride gas that the lithium bifluorosulfonimide preparation process produced in the reation kettle, absorb the processing in leading-in absorption box with hydrogen chloride gas and hydrogen fluoride gas through the honeycomb duct again, prevent the polluted atmosphere.

Drawings

FIG. 1 is a front perspective view of the overall structure of the present invention;

FIG. 2 is a bottom perspective view of the overall structure of the present invention;

FIG. 3 is a schematic half-section view of FIG. 1 in accordance with the present invention;

FIG. 4 is a schematic half-section view of FIG. 2 in accordance with the present invention;

FIG. 5 is a semi-sectional view of the hopper, the conical disc and the flow-slowing plate of FIG. 3 according to the present invention;

FIG. 6 is a schematic view of the connection between the turntable and the driving shaft according to the present invention;

FIG. 7 is an enlarged view taken at A of FIG. 4 in accordance with the present invention;

FIG. 8 is an enlarged view of the invention at B in FIG. 5.

The reference numbers in the figures illustrate:

1. a base; 11. a fixing plate; 12. a pillar; 2. a reaction kettle; 21. a cover plate; 22. a charging barrel; 3. a motor; 31. a drive shaft; 32. a main gear; 33. a pinion gear; 34. a notch; 35. a stirring paddle; 36. a squeegee; 37. a hopper; 38. a helical blade; 4. a turntable; 41. a track; 42. an air intake duct; 43. a branch pipe; 44. a flow guide pipe; 45. an absorption tank; 46. a movable rod; 47. a fixing ring; 48. a piston; 49. a strut; 5. a conical disk; 51. a bump; 52. a buffer plate; 53. a leak hole; 54. an air inlet; 55. a flow guide hole; 56. a shunt hole; 57. a gas injection hole; 6. a volute; 61. a turbine; 62. a gas delivery pipe; 63. and (6) sealing the cover.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.

Referring to fig. 1-5, a device for preparing lithium bis (fluorosulfonyl) imide, includes a base 1, a reaction vessel 2 is disposed at a central position above the base 1, a fixing plate 11 with an annular structure is fixedly connected to a position, close to a lower position, of an annular outer side surface of the reaction vessel 2, a lower end surface of the fixing plate 11 is fixedly connected to the base 1 through four pillars 12 distributed at equal intervals in an annular shape, an upper end cover of the reaction vessel 2 is provided with a cover plate 21, an upper end surface of the cover plate 21 is fixedly connected to three charging barrels 22 at equal intervals in an annular shape, a discharging pipe at a bottom of the charging barrel 22 penetrates into the reaction vessel 2, a mixing mechanism is disposed in the reaction vessel 2, the mixing mechanism includes a motor 3 fixed at a central position of the upper end surface of the cover plate 21, an output shaft of the motor 3 penetrates through the cover plate 21 and is fixedly connected to a driving shaft 31, and three stirring paddles 35 capable of rotating are annularly and equidistantly disposed at a position flush with an upper end of the driving shaft 31;

a main gear 32 is fixedly sleeved at the upper end of the annular outer side surface of the driving shaft 31, three pinions 33 are meshed with the outer side of the main gear 32 in an annular equidistant mode, the pinions 33 are rotatably connected with the upper end surface of the cover plate 21 through rotating shafts, the stirring paddles 35 are respectively rotatably connected with the central positions of the lower end surfaces of the pinions 33, notches 34 of circular arc structures are formed in the positions, close to the outer edge, of the upper end surface of the pinions 33, a hopper 37 of a funnel-shaped structure is fixedly connected to the inner wall of the reaction kettle 2 below the stirring paddles 35, the driving shaft 31 penetrates through a material guide pipe in the central position of the hopper 37, a spiral blade 38 is fixedly connected to the annular outer side surface of the driving shaft 31 inside the material guide pipe, and two scraping plates 36 matched with the inner wall of the hopper 37 are fixedly connected to the annular outer side surface of the driving shaft 31 along the radial direction 180-degree symmetry.

When the above embodiment is implemented, the raw materials for preparing lithium bis (fluorosulfonyl) imide are respectively placed in the charging barrels 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 further driving the three secondary gears 33 to rotate in the hopper 37, because the positions of the upper end surfaces of the three pinion gears 33 close to the outer edge are all provided with notches 34 with circular arc structures, and the lower end pipe orifices of the discharging pipes at the bottom of the three charging barrels 22 are respectively attached to the upper end surface of the pinion 33, so that when the notch 34 on the secondary gear 33 passes through the lower end nozzle of the blanking pipe at the bottom of the charging barrel 22, the material in the barrel 22 can enter the hopper 37 through the slot 34, thereby forming an intermittent feeding effect, because the sulfamic acid is in a crystal structure and the chlorosulfonic acid and the thionyl chloride are in liquid structures, the sulfamic acid, the chlorosulfonic acid and the thionyl chloride are easy to be bonded into a bulk shape due to excessive one-time blanking, the intermittent blanking can avoid the influence on stirring and mixing caused by the accumulation of raw materials due to excessive one-time blanking, the stirring paddle 35 can be driven to continuously rotate in the autorotation process of the pinion 33, and a plurality of groups of stirring blades which are staggered with the blades on the stirring paddle 35 are vertically and fixedly connected on the annular outer side surface of the driving shaft 31 in the hopper 37 at equal intervals, thereby make the raw materials that get into in the hopper 37 obtain intensive mixing, in order to avoid the raw materials conglobation that bonds, the rotatory in-process of drive shaft 31 drives scraper 36 simultaneously and scrapes adnexed raw materials on hopper 37 inner wall and reation kettle 2 inner wall, avoid the raw materials to be attached to on reation kettle 2 and the hopper 37 inner wall and influence the mixing effect, the raw materials through mixing is carried to the reation kettle 2 of hopper 37 below in further mixing reaction under helical blade 38's effect, helical blade 38 can prevent that the stock guide that the raw materials blockked up hopper 37 central point and put from taking place to block up.

As an embodiment of the present invention, as shown in fig. 3, 4, 5 and 8, three conical discs 5 forming a "pagoda" structure are fixedly connected vertically and equidistantly at a position between the hopper 37 and the bottom of the reaction vessel 2 on the annular outer side surface of the driving shaft 31, a baffle plate 52 is fixedly connected to the inner wall of the reaction vessel 2 corresponding to each conical disc 5, the position of the baffle plate 52 near the lower edge of the conical disc 5 is a concave structure, a plurality of leakage holes 53 are formed in the bottom of the concave structure of the baffle plate 52 at an annular equal distance, a protrusion 51 having a triangular cross section is fixedly connected to the conical outer side surface of the conical disc 5 at an annular equal distance, a volute 6 is arranged below the reaction vessel 2, the annular outer side surface of the volute 6 is fixedly connected to four pillars 12 through four fixing rods, the lower end of the driving shaft 31 penetrates into the volute 6 and is fixedly connected to a turbine 61, a sealing cover 63 is rotatably sleeved on the annular outer side surface of the driving shaft 31 between the volute 6 and the bottom of the reaction vessel 2 through a sealing bearing, the upper end of the sealing cover 63 is fixedly connected to the bottom of the reaction vessel 2, the sealing cover 63 is communicated with the outer side surface of the conical disc 5 on which a sealing hole 55, and a sealing hole 55 is formed in the conical disc 5, the conical hole 55, the conical hole is formed in the conical disc 5.

When the above embodiment is implemented, based on the above embodiment, the driving shaft 31 can simultaneously drive the turbine 61 in the volute 6 to rotate in the rotating process, 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 central position of the lower end surface of the volute 6, the filter screen is fixedly connected at the air inlet through screws, the filter screen can prevent dust in the air from entering the reaction kettle 2 to affect the purity of lithium bis (fluorosulfonyl imide) and 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 the central position of the turbine 61 generates negative pressure, so that the air is continuously pumped into the sealing cover 63 through the air pipe 62 under the action of the outside atmospheric pressure, and as the air continuously enters the sealing cover 63, the air enters the diversion holes 55 in the driving shaft 31 through the air inlet 54 and then respectively flows into the three conical disks 5 through the diversion holes 56, finally, the raw materials are upwards sprayed out through the gas holes 57, the raw materials flowing down through the hopper 37 firstly fall on the conical disc 5 on the uppermost layer, the conical disc 5 can drive the bumps 51 thereon to impact the raw materials in the rotating process, so that the raw materials are thrown to the inner wall of the reaction kettle 2 and slide along the inner wall of the reaction kettle 2 to the concave surface of the baffle plate 52 on the uppermost layer, meanwhile, the gas sprayed out of the gas holes 57 can drive the falling raw materials to roll, so as to improve the mixing effect, under the blocking effect of the baffle plate 52 on the uppermost layer, the raw materials can be gradually accumulated on the concave surface of the baffle plate 52 on the uppermost layer, so that the raw materials can be fully stirred and mixed by the conical disc 5 on the uppermost layer in cooperation with the bumps 51, as a plurality of groups of leakage holes 53 are formed in the bottom of the concave surface of the baffle plate 52 in an annular and equidistant manner, the raw materials can be leaked downwards, and as the speed of the raw materials is higher than the speed of leaking raw materials, make the raw materials on the topside current buffering board 52 more and more, because leave the space between current buffering board 52 and the drive shaft 31, thereby make too much raw materials can flow downwards through the space, along with the raw materials constantly flows down through hopper 37, the raw materials can the successive layer mix through the stirring of conical disk 5, until flow to reation kettle 2 bottom, because conical disk 5 is "pagoda" shape structure from top to bottom, thereby mix the effect and can promote by the successive layer to the stirring of raw materials, finally generate two fluorine sulfonyl imide lithium, promote two fluorine sulfonyl imide lithium synthetic quality.

As an embodiment of the present invention, as shown in fig. 3-7, three suction pipes 42 having a U-shaped structure are annularly and equidistantly arranged on an annular outer side surface of the reaction vessel 2 near an upper end position, upper end pipe orifices of the suction pipes 42 are respectively communicated with the reaction vessel 2 above the hopper 37, lower end pipe orifices of the suction pipes 42 are respectively communicated with the reaction vessel 2 below the hopper 37, a central position of a vertical portion of the suction pipes 42 is respectively communicated with the reaction via a branch pipe 43, the reaction vessel 2 is fixedly connected with an absorption box 45 on the annular outer side surface below the suction pipes 42, lower horizontal portions of the suction pipes 42 are respectively communicated with the absorption box 45 via a guide pipe 44, a turntable 4 having a circular ring structure is arranged on an outer side of a material guide pipe at a central position of the hopper 37, a lower end surface of the turntable 4 near an inner edge position is fixedly connected with the driving shaft 31 via three support rods 49 which are equidistantly distributed, a lower end surface of the turntable 4 is near a rail 41 which is provided with a "hexagon" star "structure", a movable rod 46 having an L "shape" is slidably inserted in the lower horizontal portion of the suction pipe 42, one end of the movable rod 46 is fixedly connected with a piston 48, the other end of the movable rod 46 is located in the rail 41, and a fixed ring 47 is inserted in the fixed ring 47.

In the above embodiment, according to the above embodiment, since hydrogen fluoride gas is added as a reactant and hydrogen chloride gas is generated during the preparation of lithium bis-fluorosulfonylimide, and excessive hydrogen chloride gas and hydrogen fluoride gas float above the hopper 37 and below the hopper 37, and if not removed, corrosion of the reaction vessel 2 occurs due to long-term accumulation, the rotating disk 4 is driven to rotate by the supporting rod 49 during the rotation of the driving shaft 31, the movable rod 46 reciprocates inside the lower horizontal portion of the air suction pipe 42 under the action of the orbit 41 having the hexagonal structure, when the movable rod 46 drives the piston 48 to contract inward, the check valve at the lower horizontal portion of the air suction pipe 42 is opened, the check valve inside the air suction pipe 44 is closed, so that hydrogen chloride gas and hydrogen fluoride gas floating above the hopper 37 are sucked into the lower horizontal portion of the air suction pipe 42 by suction force through the upper horizontal portion of the air suction pipe 42, the hydrogen chloride gas and hydrogen fluoride gas floating below the hopper 37 are sucked into the lower horizontal portion of the air suction pipe 42 through the branch pipe 43, and the check valve 44 is closed, thereby preventing the hydrogen chloride gas from sucking into the air suction pipe 44 and hydrogen fluoride gas through the check valve 44, and preventing the hydrogen fluoride gas from being sucked into the air suction pipe 44 and the hydrogen chloride absorption tank, and hydrogen fluoride absorption tank, the hydrogen chloride absorption tank is prevented from being contaminated by the hydrogen chloride absorption tank 44, meanwhile, the phenomenon that the atmosphere is polluted due to direct discharge of hydrogen chloride gas and hydrogen fluoride gas is avoided, the air sucking pipe 42 sucks partial air sprayed out through the air spraying holes 57 while sucking the hydrogen chloride gas and the hydrogen fluoride gas, air is contained in mixed gas entering the absorption box 45, the air is hardly dissolved in absorption liquid, the air can be discharged through an exhaust pipe on the upper end face of the absorption box 45, the continuous absorption capacity of the absorption liquid on the hydrogen chloride gas and the hydrogen fluoride gas is not influenced, an annular block made of ceramic materials is fixedly sleeved at one end of the movable rod 46 positioned in the rail 41, abrasion between the movable rod 46 and the rail 41 is reduced, the fixed ring 47 is fixedly connected at the position of the pipe orifice of the horizontal part on the lower side of the air sucking pipe 42, the movable rod 46 is guaranteed to stably move in the air sucking pipe 42, and meanwhile abrasion of the lower ends of the movable rod 46 and the air sucking pipe 42 is prevented.

s1: the raw materials are respectively loaded into the charging barrels 22, then the motor 3 is started to drive the driving shaft 31 to rotate, so as to drive the main gear 32 to rotate, further drive the three secondary gears 33 to synchronously rotate, so that the stirring paddles 35 below the secondary gears 33 continuously rotate, and the notches 34 on the secondary gears 33 can intermittently open the discharging pipe at the lower end of the charging barrels 22, so that intermittent discharging is carried out, and the phenomenon that the mixing effect is influenced by too much investment once is avoided;

s2: the driving shaft 31 drives the turbine 61 in the volute 6 to rotate in the rotating process, so that the turbine 61 generates centrifugal force to suck outside air into the volute 6, the outside air is input into the sealing cover 63 through the air pipe 62, the air entering the sealing cover 63 enters the diversion holes 55 through the air inlet 54, then enters the three conical discs 5 through the diversion holes 56, and finally is ejected out through the air ejecting holes 57 on the conical discs 5, so that falling raw materials are driven to be rolled and mixed, and the mixing effect is improved;

s3: the rotation of the driving shaft 31 also drives the rotation of the turntable 4, so as to drive the piston 48 to reciprocate in the horizontal portion of the lower side of the air suction pipe 42, further to suck the hydrogen chloride gas and the hydrogen fluoride gas generated in the preparation process of the lithium bis (fluorosulfonyl) imide in the reaction kettle 2 into the air suction pipe 42, and then to introduce the hydrogen chloride gas and the hydrogen fluoride gas into the absorption box 45, thereby preventing the atmosphere from being polluted.

The working principle is as follows: raw materials for preparing lithium bis (fluorosulfonyl) imide are respectively placed in a charging barrel 22, then a motor 3 is started to drive a driving shaft 31 to rotate, so that three secondary gears 33 are driven to rotate in a hopper 37, when a notch 34 on each secondary gear 33 passes through a lower end pipe orifice of a discharging pipe at the bottom of the charging barrel 22, the raw materials in the charging barrel 22 enter the hopper 37 through the notches 34, and an intermittent discharging effect is formed, the intermittent discharging can prevent the raw materials from being accumulated due to excessive discharging at one time and affecting stirring and mixing, the stirring paddles 35 can be driven to rotate continuously in the rotation process of the secondary gears 33, a plurality of groups of stirring blades which are mutually staggered with blades on the stirring paddles 35 are fixedly connected to the annular outer side surface of the driving shaft 31 in the hopper 37 at equal intervals, so that the raw materials entering the hopper 37 are fully stirred, the raw materials are prevented from being bonded into a mass, the driving scraper 36 is simultaneously driven to scrape the inner wall of the hopper 37 and the raw materials attached to the inner wall of the hopper 37 and the inner wall of the reaction kettle 2 in the reaction kettle 2 under the action of a spiral blade 38, and further mixing effect of the reaction kettle 37 is achieved;

the driving shaft 31 can drive the turbine 61 in the volute 6 to rotate simultaneously in the rotating process, so that the turbine 61 generates centrifugal force, outside air is sucked into the volute 6 through the air inlet at the central position of the lower end face of the volute 6, the air entering the volute 6 is continuously pumped into the sealing cover 63 through the air pipe 62, along with the continuous air entering the sealing cover 63, the air enters the diversion holes 55 in the driving shaft 31 through the air inlet holes 54, then respectively flows into the three conical disks 5 through the diversion holes 56, finally is upwards sprayed out through the air spraying holes 57, raw materials flowing down through the hopper 37 firstly fall on the conical disk 5 at the uppermost layer, the conical disc 5 can drive the convex block 51 thereon to impact the raw material in the rotating process, so that the raw material is thrown onto the inner wall of the reaction kettle 2, the raw material slides down to the concave surface of the uppermost current-slowing plate 52 along the inner wall of the reaction kettle 2, meanwhile, the gas sprayed out of the gas-spraying holes 57 can drive the falling raw material to roll, so that the mixing effect is improved, the raw material continuously flows down through the hopper 37, and can be stirred and mixed layer by layer through the conical disc 5 until the raw material flows to the bottom of the reaction kettle 2, and the stirring and mixing effect of the raw material can be improved layer by layer due to the fact that the conical disc 5 is of a pagoda-shaped structure from top to bottom, so that the lithium bis-fluorosulfonylimide is finally generated, and the synthesis quality of the lithium bis-fluorosulfonylimide is improved;

since the lithium bis (fluorosulfonyl imide) is added with hydrogen fluoride gas as a reactant during the preparation process and also generates hydrogen chloride gas, and the excessive hydrogen chloride gas and hydrogen fluoride gas will float above the hopper 37 and under the hopper 37, if not removed, corrosion will occur in the reaction vessel 2 due to long-term accumulation, the rotating disk 4 will be driven to rotate by the support rod 49 during the rotation of the driving shaft 31, the movable rod 46 will reciprocate back and forth inside the lower horizontal portion of the air suction pipe 42 under the action of the orbit 41 with the hexagonal star-shaped structure, when the movable rod 46 drives the piston 48 to contract inwards, the check valve at the lower horizontal portion of the air suction pipe 42 outside the air guide pipe 44 is opened, the check valve inside the air 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 portion of the air suction pipe 42 by the suction force through the upper horizontal portion of the air suction pipe 42, the hydrogen chloride gas and hydrogen fluoride gas floating at the lower horizontal portion of the hopper 37 are sucked into the lower horizontal portion of the air suction pipe 42 through the branch pipe 43, thereby preventing the hydrogen chloride gas and hydrogen fluoride gas from being sucked into the annular orbit 44 through the ceramic suction pipe, and the ceramic ring-shaped structure, thereby preventing the hydrogen chloride gas from being corroded by the ceramic ring-filled in the ceramic hydrogen chloride gas guide pipe 41 and the ceramic ring-filled in the ceramic ring-filled with the hydrogen fluoride gas, and hydrogen chloride gas, and hydrogen fluoride gas, and the ceramic hydrogen fluoride gas filled in the ceramic ring-filled tube 41, the fixed ring 47 is fixedly connected to the lower horizontal portion of the air intake pipe 42 at the nozzle position to ensure the stable movement of the movable rod 46 in the air intake pipe 42 and prevent the abrasion of the movable rod 46 and the lower nozzle of the air intake pipe 42.

The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims

1. A preparation equipment of lithium bis (fluorosulfonyl) imide is characterized in that: comprises a base (1);

the reaction kettle (2) is arranged at the central position above the base (1), a fixing plate (11) with an annular structure is fixedly connected to the annular outer side surface of the reaction kettle (2) at a position close to the lower position, and the lower end surface of the fixing plate (11) is fixedly connected with the base (1) through four pillars (12) which are annularly and equidistantly distributed;

a cover plate (21) is arranged on the upper end cover of the reaction kettle (2), three charging barrels (22) are fixedly connected to the upper end face of the cover plate (21) close to the outer edge at equal intervals in a circular mode, a discharging pipe at the bottom of each charging barrel (22) penetrates into the reaction kettle (2), and raw materials are input into the reaction kettle (2) through the charging barrels (22) to prepare the lithium bis (fluorosulfonyl) imide;

mixing mechanism for stir the mixture to the inside raw materials of input reation kettle (2), prevent that the raw materials from bonding into the massif, including fixing motor (3) of putting at apron (21) upper end face central point, the output shaft of motor (3) runs through apron (21) and fixedly connected with drive shaft (31), with drive shaft (31) upper end parallel and level position annular equidistance is equipped with three stirring rake (35) that can take place the rotation.

2. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the fixed cover in drive shaft (31) annular lateral surface upper end is equipped with master gear (32), the meshing of master gear (32) outside annular equidistance has three pinion (33), pinion (33) are connected through pivot and apron (21) up end rotation, stirring rake (35) are connected with pinion (33) down terminal surface central point respectively and are put the rotation, pinion (33) up end is close to outer notch (34) of all offering the arc structure along the position.

3. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 2, wherein: the stirring device is characterized in that a hopper (37) with a funnel-shaped structure is fixedly connected to the inner wall of the reaction kettle (2) below the stirring paddle (35), the driving shaft (31) penetrates through a material guide pipe arranged at the center of the hopper (37), the driving shaft (31) is fixedly connected with a spiral blade (38) on the annular outer side surface inside the material guide pipe, and the driving shaft (31) is symmetrically and fixedly connected with two scraping plates (36) matched with the inner wall of the hopper (37) along the radial direction 180 degrees on the annular outer side surface.

4. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 3, wherein: drive shaft (31) annular lateral surface is located the toper dish (5) of three constitution "pagoda" shape structure of the vertical equidistance fixedly connected with in position between hopper (37) and reation kettle (2) bottom, reation kettle (2) inner wall corresponds every toper dish (5) equal fixedly connected with slowly flow board (52), slowly flow board (52) are close to toper dish (5) lower extreme border position department and are recessed structure, and slowly flow board (52) recessed structure's bottom annular equidistance and seted up a plurality of small opening (53), the equal annular equidistance fixedly connected with cross-section of toper lateral surface of toper dish (5) is lug (51) of triangle-shaped structure.

5. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 4, wherein: a volute (6) is arranged below the reaction kettle (2), the annular outer side surface of the volute (6) is fixedly connected with four struts (12) through four fixing rods, and the lower end of the driving shaft (31) penetrates into the volute (6) and is fixedly connected with a turbine (61).

6. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 5, wherein: rotate the cover through sealed bearing and be equipped with sealed cowling (63) on drive shaft (31) annular lateral surface between spiral case (6) and reation kettle (2) bottom, the upper end and reation kettle (2) bottom fixed connection of sealed cowling (63), communicate through gas-supply pipe (62) between the annular lateral surface of sealed cowling (63) and spiral case (6).

7. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 6, wherein: lie in drive shaft (31) central point in seal cover (63) puts and sets up water conservancy diversion hole (55) that extend to topmost side conical disk (5) position, set up on drive shaft (31) the annular lateral surface that is located seal cover (63) inlet port (54) with water conservancy diversion hole (55) intercommunication, every conical disk (5) inside all is the cavity structure, and sets up on water conservancy diversion hole (55) inner wall respectively with flow distribution hole (56) that correspond position conical disk (5) intercommunication, every jet orifice (57) that are the helix and distribute are all seted up on conical disk (5) toper lateral surface.

8. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 3, wherein: reation kettle (2) annular lateral surface is close to upper end position annular equidistance and is equipped with breathing pipe (42) of three U-shaped structures, the upper end mouth of pipe of breathing pipe (42) communicates with reation kettle (2) of hopper (37) top position respectively, breathing pipe (42) lower extreme mouth of pipe communicates with reation kettle (2) of hopper (37) below respectively, the central point of breathing pipe (42) vertical portion puts respectively through a branch pipe (43) and reaction intercommunication, reation kettle (2) are located fixedly connected with absorption box (45) on the annular lateral surface of breathing pipe (42) below, the downside horizontal segment of breathing pipe (42) communicates with absorption box (45) through a honeycomb duct (44) respectively.

9. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 8, wherein: the outside of hopper (37) central point position passage is equipped with round annular structure's carousel (4), the terminal surface is close to interior edge position and passes through three equidistance branch (49) and drive shaft (31) fixed connection that distribute down of carousel (4), the terminal surface is close to track (41) of seting up "hexagonal star" shape structure down of carousel (4), the inside slip of the downside horizontal segment of breathing pipe (42) is pegged graft and is had movable rod (46) of "L" shape structure, movable rod (46) are located one end fixedly connected with piston (48) of breathing pipe (42), the other end of movable rod (46) is located track (41), the lower extreme mouth of pipe position fixedly connected with solid fixed ring (47) of breathing pipe (42), and movable rod (46) slip and insert and establish in solid fixed ring (47).

10. The method for manufacturing lithium bis (fluorosulfonyl) imide, which is applied to any one of claims 1 to 9, comprises the steps of: the method comprises the following steps:

s1: respectively loading raw materials into a charging barrel (22), then starting a motor (3) to drive a driving shaft (31) to rotate, thereby driving a main gear (32) to rotate, further driving three secondary gears (33) to synchronously rotate, so that a stirring paddle (35) below the secondary gears (33) continuously rotates, and notches (34) on the secondary gears (33) can intermittently open a discharging pipe at the lower end of the charging barrel (22), thereby carrying out intermittent discharging and avoiding the influence of excessive one-time feeding on a mixing effect;

s2: the turbine (61) in the volute (6) can be driven to rotate in the rotating process of the driving shaft (31), so that the turbine (61) generates centrifugal force to suck outside air into the volute (6), the outside air is input into the sealing cover (63) through the air conveying pipe (62), the air entering the sealing cover (63) enters the flow guide holes (55) through the air inlet holes (54), then respectively enters the three conical discs (5) through the flow distribution holes (56), and finally is ejected out through the air ejection holes (57) in the conical discs (5), so that falling raw materials are driven to be rolled and mixed, and the mixing effect is improved;

s3: the rotary disc (4) is driven to rotate in the rotating process of the driving shaft (31), so that the piston (48) is driven to reciprocate in the horizontal part of the lower side of the air suction pipe (42), hydrogen chloride gas and hydrogen fluoride gas generated in the preparation process of the lithium bis (fluorosulfonyl) imide in the reaction kettle (2) are sucked into the air suction pipe (42), and then the hydrogen chloride gas and the hydrogen fluoride gas are introduced into the absorption box (45) to prevent atmosphere pollution.