阅读说明：本技术 一种双氟磺酰亚胺锂的制备装置及方法 (Preparation device and method of lithium bis (fluorosulfonyl) imide ) 是由 林坤 王少波 马朝选 王亚峰 罗建志 董云海 李丹丹 王云飞 于 2021-08-27 设计创作，主要内容包括：本发明涉及一种双氟磺酰亚胺锂的制备装置及方法,属于双氟磺酰亚胺锂制备生产技术领域。所述装置包括反应釜、驱动机构和气动机构。所述装置利用驱动机构带动反应釜中的空心杆转动使搅拌叶转动,达到初步搅拌反应效果；反应釜中设计的结构可将反应釜中心处的液体能够向边缘流动,使液体充分反应；通过气动机构的气动动力组件将外界空气通过连接管注入空心杆内,然后进入气体喷出组件并喷出,能够喷动液体翻滚,进一步的提高了反应的效果。所述制备方法反应流程短,产生的废弃物少,所述装置能够将添加至反应釜内的原料进行充分的混合反应,大大的提高了原料的反应效果。(The invention relates to a device and a method for preparing lithium bis (fluorosulfonyl) imide, and belongs to the technical field of preparation and production of lithium bis (fluorosulfonyl) imide. The device comprises a reaction kettle, a driving mechanism and a pneumatic mechanism. The device utilizes a driving mechanism to drive a hollow rod in the reaction kettle to rotate so as to rotate the stirring blades, thereby achieving the effect of preliminary stirring reaction; the structure designed in the reaction kettle can enable the liquid in the center of the reaction kettle to flow towards the edge, so that the liquid can fully react; the pneumatic power assembly through the pneumatic mechanism injects the external air into the hollow rod through the connecting pipe, then enters the gas spraying assembly and is sprayed out, the sprayed liquid can roll, and the reaction effect is further improved. The preparation method has the advantages of short reaction flow and less generated waste, and the device can carry out full mixing reaction on the raw materials added into the reaction kettle, thereby greatly improving the reaction effect of the raw materials.)

1. A device for preparing lithium bis (fluorosulfonyl) imide is characterized in that: the device comprises a reaction kettle (1), a driving mechanism and a pneumatic mechanism;

the driving mechanism is positioned above the outer side of the top of the reaction kettle (1);

the pneumatic mechanism mainly comprises a pneumatic power assembly and a gas ejection assembly, the pneumatic power assembly is positioned above the outer side of the top of the reaction kettle (1), and the gas ejection assembly is positioned above the bottom in the reaction kettle (1);

a feeding hole (10) is formed in the top of the reaction kettle (1), a discharging hole (22) is formed in the lowest position of the bottom of the reaction kettle (1), and an outer half pipe for heating is arranged on the outer side of the reaction kettle (1);

a hollow rod (25) is arranged at the center position above the bottom in the reaction kettle (1), the bottom of the hollow rod (25) is connected with a gas ejection assembly of the driving mechanism, and the top of the hollow rod (25) penetrates through the interior of the reaction kettle (1), extends out of the reaction kettle (1) from the top of the reaction kettle (1) and is respectively connected with the driving mechanism and a pneumatic power assembly of the pneumatic mechanism;

a cavity is fixedly arranged at the upper part in the reaction kettle (1), a hollow rod (25) penetrates through the middle part of the cavity, two ends of the top of the cavity are connected with the inner wall of the reaction kettle (1), two liquid inlets (11) are symmetrically arranged at positions close to the hollow rod (25) in the center, and two liquid discharge ports (16) are symmetrically arranged at the connection part of the bottom of the cavity and the inner wall of the reaction kettle (1); two partition plates (12) are symmetrically arranged in the cavity below the inner side of the liquid inlet (11), the upper ends of the partition plates (12) are connected with the top of the cavity, the lower ends of the partition plates (12) are connected with the bottom of the cavity, the interior of the cavity is divided into a central area and a peripheral area, so that liquid flows into the peripheral area but cannot enter the central area, the peripheral area of the cavity is symmetrically provided with two spiral rods (15), the outer ends of the spiral rods (15) are connected with the inner wall of the reaction kettle (1), and the inner ends penetrate through the partition plates (12) and extend into the central area and are fixedly connected with first bevel gears (13); the hollow rod (25) penetrates through the central area of the cavity, a second bevel gear (14) is fixedly connected to the lower part of the central area of the cavity, and the second bevel gear (14) is meshed with the first bevel gear (13);

the hollow rod (25) is positioned in the reaction kettle (1) and is connected with a plurality of stirring blades (17) at the part outside the cavity body.

2. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the bottom of the reaction kettle (1) is funnel-shaped, and a plurality of support legs (21) are fixedly connected to the outer side of the bottom of the reaction kettle (1) and used for supporting the reaction kettle (1).

3. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the spiral rods (15) are composed of a rod body and spiral blades fixedly wound on the periphery of the rod body, and the spiral directions of the two spiral rods (15) are opposite.

4. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the bottom of the reaction kettle (1) is funnel-shaped, and the outer side of the bottom of the reaction kettle (1) is fixedly connected with a plurality of support legs (21) for supporting the reaction kettle (1);

the spiral rods (15) are composed of a rod body and spiral blades fixedly wound on the periphery of the rod body, and the spiral directions of the two spiral rods (15) are opposite.

5. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the driving mechanism comprises a first driving wheel (6), a second driving wheel (7), a driving motor (8) and a mounting plate (9); mounting panel (9) fixed connection is in reation kettle (1) top outside top, the lateral wall fixedly connected with driving motor (8) of mounting panel (9), the output shaft end and reation kettle (1) top of driving motor (8) are rotated and are connected, the output shaft cover of driving motor (8) is equipped with second drive wheel (7), it is equipped with first drive wheel (6) to stretch out on the lower part of reation kettle (1) top portion hollow rod (25), be connected through transmission belt transmission between first drive wheel (6) and second drive wheel (7).

6. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the pneumatic power assembly of the pneumatic mechanism comprises a bracket (18), an annular pipe (19), an annular sleeve (23) and a communicating pipe (24); annular tube (19) fixed connection is bottom top in reation kettle (1), and the top of annular tube (19) is equidistant to be provided with a plurality of fumarole (20), and hollow rod (25) bottom is connected with annular tube (19), and concrete connected mode is: an annular sleeve (23) is sleeved on the outer side of the hollow rod (25), a plurality of openings (26) are circumferentially and equidistantly arranged on the side wall of the bottom of the hollow rod (25), the openings (26) are positioned inside the annular sleeve (23), two communicating holes (27) are symmetrically arranged on the annular sleeve (23), two communicating pipes (24) matched with the communicating holes (27) are fixedly connected to the annular sleeve (23), and one ends, far away from the annular sleeve (23), of the communicating pipes (24) are communicated with the annular pipe (19); two brackets (18) for supporting the communicating pipes (24) are symmetrically arranged on the inner side of the bottom of the reaction kettle (1);

the gas spraying assembly of the pneumatic mechanism comprises a blower (2), a connecting pipe (3), a rotary joint (4) and a mounting rack (5); air-blower (2) are located the top outside top of reation kettle (1), and mounting bracket (5) are located reation kettle (1) top outside top and are close to the part that hollow rod (25) stretches out reation kettle (1) top, and fixed connection has rotary joint (4) on mounting bracket (5), and rotary joint (4) lower extreme and hollow rod (25) stretch out the top intercommunication of reation kettle (1) top part, and air-blower (2) are through connecting pipe (3) and rotary joint (4) upper end intercommunication.

7. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the driving mechanism comprises a first driving wheel (6), a second driving wheel (7), a driving motor (8) and a mounting plate (9); the mounting plate (9) is fixedly connected above the outer side of the top of the reaction kettle (1), the side wall of the mounting plate (9) is fixedly connected with a driving motor (8), the tail end of an output shaft of the driving motor (8) is rotatably connected with the top of the reaction kettle (1), an output shaft of the driving motor (8) is sleeved with a second driving wheel (7), a first driving wheel (6) is sleeved on the lower part of the hollow rod (25) extending out of the top of the reaction kettle (1), and the first driving wheel (6) is in transmission connection with the second driving wheel (7) through a transmission belt;

the pneumatic power assembly of the pneumatic mechanism comprises a bracket (18), an annular pipe (19), an annular sleeve (23) and a communicating pipe (24); annular tube (19) fixed connection is bottom top in reation kettle (1), and the top of annular tube (19) is equidistant to be provided with a plurality of fumarole (20), and hollow rod (25) bottom is connected with annular tube (19), and concrete connected mode is: an annular sleeve (23) is sleeved on the outer side of the hollow rod (25), a plurality of openings (26) are circumferentially and equidistantly arranged on the side wall of the bottom of the hollow rod (25), the openings (26) are positioned inside the annular sleeve (23), two communicating holes (27) are symmetrically arranged on the annular sleeve (23), two communicating pipes (24) matched with the communicating holes (27) are fixedly connected to the annular sleeve (23), and one ends, far away from the annular sleeve (23), of the communicating pipes (24) are communicated with the annular pipe (19); two brackets (18) for supporting the communicating pipes (24) are symmetrically arranged on the inner side of the bottom of the reaction kettle (1);

the gas spraying assembly of the pneumatic mechanism comprises a blower (2), a connecting pipe (3), a rotary joint (4) and a mounting rack (5); air-blower (2) are located the top outside top of reation kettle (1), and mounting bracket (5) are located reation kettle (1) top outside top and are close to the part that hollow rod (25) stretches out reation kettle (1) top, and fixed connection has rotary joint (4) on mounting bracket (5), and rotary joint (4) lower extreme and hollow rod (25) stretch out the top intercommunication of reation kettle (1) top part, and air-blower (2) are through connecting pipe (3) and rotary joint (4) upper end intercommunication.

8. The apparatus for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the bottom of the reaction kettle (1) is funnel-shaped, and the outer side of the bottom of the reaction kettle (1) is fixedly connected with a plurality of support legs (21) for supporting the reaction kettle (1);

the spiral rods (15) are composed of rod bodies and spiral blades fixedly wound on the peripheries of the rod bodies, and the spiral directions of the two spiral rods (15) are opposite;

the driving mechanism comprises a first driving wheel (6), a second driving wheel (7), a driving motor (8) and a mounting plate (9); the mounting plate (9) is fixedly connected above the outer side of the top of the reaction kettle (1), the side wall of the mounting plate (9) is fixedly connected with a driving motor (8), the tail end of an output shaft of the driving motor (8) is rotatably connected with the top of the reaction kettle (1), an output shaft of the driving motor (8) is sleeved with a second driving wheel (7), a first driving wheel (6) is sleeved on the lower part of the hollow rod (25) extending out of the top of the reaction kettle (1), and the first driving wheel (6) is in transmission connection with the second driving wheel (7) through a transmission belt;

the pneumatic power assembly of the pneumatic mechanism comprises a bracket (18), an annular pipe (19), an annular sleeve (23) and a communicating pipe (24); annular tube (19) fixed connection is bottom top in reation kettle (1), and the top of annular tube (19) is equidistant to be provided with a plurality of fumarole (20), and hollow rod (25) bottom is connected with annular tube (19), and concrete connected mode is: an annular sleeve (23) is sleeved on the outer side of the hollow rod (25), a plurality of openings (26) are circumferentially and equidistantly arranged on the side wall of the bottom of the hollow rod (25), the openings (26) are positioned inside the annular sleeve (23), two communicating holes (27) are symmetrically arranged on the annular sleeve (23), two communicating pipes (24) matched with the communicating holes (27) are fixedly connected to the annular sleeve (23), and one ends, far away from the annular sleeve (23), of the communicating pipes (24) are communicated with the annular pipe (19); two brackets (18) for supporting the communicating pipes (24) are symmetrically arranged on the inner side of the bottom of the reaction kettle (1);

the gas spraying assembly of the pneumatic mechanism comprises a blower (2), a connecting pipe (3), a rotary joint (4) and a mounting rack (5); air-blower (2) are located the top outside top of reation kettle (1), and mounting bracket (5) are located reation kettle (1) top outside top and are close to the part that hollow rod (25) stretches out reation kettle (1) top, and fixed connection has rotary joint (4) on mounting bracket (5), and rotary joint (4) lower extreme and hollow rod (25) stretch out the top intercommunication of reation kettle (1) top part, and air-blower (2) are through connecting pipe (3) and rotary joint (4) upper end intercommunication.

9. A preparation method of lithium bis (fluorosulfonyl) imide is characterized by comprising the following steps: the method is completed by adopting the device for preparing the lithium bis (fluorosulfonyl) imide as claimed in any one of claims 1 to 8, and comprises the following steps:

firstly, sulfamic acid, chlorosulfonic acid and thionyl chloride with the molar ratio of 0.8:1:1.8 are put into a reaction kettle (1), and the reaction kettle (1) is utilized to carry out temperature rise reaction to obtain an imide acid reaction solution;

secondly, after the reaction is finished, rectifying the reaction liquid, separating raw materials which do not finish the reaction, and collecting imine acid of the rectified fraction;

putting potassium fluoride and dimethyl carbonate into a reaction kettle (1), adding the obtained imide acid into the reaction kettle (1), wherein the molar ratio of the potassium fluoride to the imide acid is 1:3, the addition amount of the dimethyl carbonate is 2.5 times of that of the potassium fluoride, carrying out heating reaction after the imide acid is completely added until the pH value is 7, and then cooling and filtering to obtain a dimethyl carbonate solution;

adding anhydrous lithium chloride and dimethyl carbonate with the molar ratio of 1:5 into the reaction kettle (1), and adding the dimethyl carbonate solution obtained in the step (c) for reaction to obtain a crude product of lithium bis (fluorosulfonyl) imide;

fifthly, concentrating, evaporating, crystallizing and drying the crude product of the lithium bis (fluorosulfonyl) imide to obtain a finished product of the lithium bis (fluorosulfonyl) imide.

10. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 9, wherein: the temperature rise in the step I is 80-150 ℃, and the heating time is 50 h;

the addition of the imide acid in the step (III) and the addition of the dimethyl carbonate solution in the step (IV) are both in a dripping mode, and the dripping time of the imide acid in the step (III) is 8-10 h;

the reaction temperature in the step IV is 45-65 ℃ and the reaction time is 3-5 h.

Technical Field

The invention relates to a device and a method for preparing lithium bis (fluorosulfonyl) imide, and belongs to the technical field of preparation and production of lithium bis (fluorosulfonyl) imide.

Background

In the prior art, lithium ion batteries are widely used in electronic products, electric vehicles, and energy storage devices due to their high energy density. Therefore, lithium ion battery products are generally required to have excellent performance such as high capacity, long life, high power factor, and safety. Specifically, the electrolytes with different compositions in the lithium ion battery cause differences in performance of the lithium ion battery to a great extent, and particularly, the problems of the lithium ion battery, such as service life and self-discharge, are significantly affected by high and low temperature use environments, decomposition and side reactions of the electrolytes. Therefore, in the prior art, various additives are tried to be added into the electrolyte to improve the above-mentioned problems of the battery.

The lithium bis (fluorosulfonyl) imide has the characteristics of high temperature resistance, excellent low-temperature performance, good stability in water, environment friendliness and the like, is widely applied to the electrolyte of a lithium ion battery, can effectively reduce the high and low temperature resistance of a Solid Electrolyte Interface (SEI) layer formed on the surface of an electrode at low temperature, and reduces the capacity loss of the lithium ion battery in the placing process, so that a high-capacity battery is provided, and the electrochemical performance of the battery is improved.

At present, in the process of preparing and producing the lithium bis (fluorosulfonyl) imide, excessive wastes are caused due to too long reaction flow, and the mass production of the lithium bis (fluorosulfonyl) imide is not facilitated.

Disclosure of Invention

In order to overcome the defects in the prior art, the invention aims to provide a device and a method for preparing lithium bis (fluorosulfonyl) imide.

In order to achieve the purpose of the invention, the following technical scheme is provided.

A device for preparing lithium bis (fluorosulfonyl) imide comprises a reaction kettle, a driving mechanism and a pneumatic mechanism.

The driving mechanism is positioned above the outer side of the top of the reaction kettle.

The pneumatic mechanism mainly comprises a pneumatic power assembly and a gas spraying assembly, wherein the pneumatic power assembly is positioned above the outer side of the top of the reaction kettle, and the gas spraying assembly is positioned above the bottom in the reaction kettle.

The reaction kettle is characterized in that a feeding hole is formed in the top of the reaction kettle, a discharging hole is formed in the lowest position of the bottom of the reaction kettle, and an outer half pipe for heating is arranged on the outer side of the reaction kettle.

The top of the hollow rod penetrates through the inside of the reaction kettle, extends out of the reaction kettle from the top of the reaction kettle and is respectively connected with the driving mechanism and a pneumatic power assembly of the pneumatic mechanism.

A cavity is fixedly arranged at the upper part in the reaction kettle, a hollow rod penetrates through the middle part of the cavity, two ends of the top of the cavity are connected with the inner wall of the reaction kettle, two liquid inlets are symmetrically arranged at the positions close to the hollow rod in the center, and two liquid outlets are symmetrically arranged at the connecting part of the bottom of the cavity and the inner wall of the reaction kettle; two partition plates are symmetrically arranged in the cavity below the inner side of the liquid inlet, the upper ends of the partition plates are connected with the top of the cavity, the lower ends of the partition plates are connected with the bottom of the cavity, the interior of the cavity is divided into a central area and a peripheral area, so that liquid flows into the peripheral area but cannot enter the central area, the peripheral area of the cavity is symmetrically provided with two spiral rods, the outer ends of the spiral rods are connected with the inner wall of the reaction kettle, and the inner ends of the spiral rods penetrate through the partition plates and extend into the central area and are fixedly connected with a first bevel gear; the hollow rod penetrates through the central area of the cavity, and a second bevel gear is fixedly connected to the lower portion of the central area of the cavity and meshed with the first bevel gear.

The hollow rod is positioned in the reaction kettle, and the part outside the cavity body is connected with a plurality of stirring blades.

Preferably, the bottom of the reaction kettle is funnel-shaped, and a plurality of support legs are fixedly connected to the outer side of the bottom of the reaction kettle and used for supporting the reaction kettle.

Preferably, the screw rods are composed of a rod body and a helical blade fixedly wound on the periphery of the rod body, and the helical directions of the two screw rods are opposite.

Preferably, the driving mechanism comprises a first driving wheel, a second driving wheel, a driving motor and a mounting plate. Mounting panel fixed connection is in reation kettle top outside top, and mounting panel lateral wall fixedly connected with driving motor, driving motor output shaft end rotate with the reation kettle top and be connected, and driving motor output shaft cover is equipped with the second drive wheel, and the cover is equipped with first drive wheel on the lower part that hollow pole stretches out reation kettle top part, is connected through the transmission of drive belt between first drive wheel and the second drive wheel.

Preferably, the pneumatic power assembly of the pneumatic mechanism comprises a bracket, an annular pipe, an annular sleeve and a communicating pipe. Annular tube fixed connection is bottom top in reation kettle, and the top equidistant of annular tube is provided with a plurality of fumarole, and hollow rod bottom and annular union coupling, concrete connected mode are: the hollow rod outside cover is equipped with annular cover, and hollow rod bottom lateral wall circumference is equidistant to be provided with a plurality of opening, and the opening is located inside annular cover, and the annular is sheathe the symmetry and is provided with two intercommunicating pores, and two fixedly connected with communicating pipes with intercommunicating pore matched with are sheathe in to the annular, and the one end and the annular pipe intercommunication of annular cover are kept away from to communicating pipe. Two brackets for supporting the communicating pipe are symmetrically arranged on the inner side of the bottom of the reaction kettle.

Preferably, the gas ejection assembly of the pneumatic mechanism includes a blower, a connection pipe, a rotary joint, and a mounting bracket. The air-blower is located reation kettle top outside top, and the mounting bracket is located the part that the adjacent hollow pole in reation kettle top outside top stretches out the reation kettle top, and fixed connection has rotary joint on the mounting bracket, and the rotary joint lower extreme and the top intercommunication that the hollow pole stretches out reation kettle top part, air-blower pass through connecting pipe and rotary joint upper end intercommunication.

The preparation device of the lithium bis (fluorosulfonyl) imide provided by the invention works:

utilize actuating mechanism to drive hollow rod and rotate to make the stirring leaf rotate, reach the effect of preliminary stirring reaction. Specifically speaking, actuating mechanism's driving motor orders about the second drive wheel and rotates, realizes the rotation of first drive wheel through the drive belt, and first drive wheel rotates and drives hollow rod and rotate to make the stirring leaf rotate, reach preliminary stirring reaction's effect.

Hollow rod rotates and drives second bevel gear and rotate, because second bevel gear and first bevel gear meshing to realize the rotation of two hob, under the promotion of hob, can pass through the leakage fluid dram discharge with the liquid that gets into from the inlet, make the liquid of reation kettle center department can flow to the edge, so that the abundant reaction of liquid.

The pneumatic power assembly through the pneumatic mechanism injects the external air into the hollow rod through the connecting pipe, then enters the gas spraying assembly and is sprayed out, the sprayed liquid can roll, and the reaction effect is further improved. Specifically speaking, through opening the air-blower, utilize the air-blower to pass through the connecting pipe with the outside air and pour into hollow pole in, get into the annular ring through the opening afterwards in, get into the inside of annular pipe through intercommunicating pore and communicating pipe again, it is jet-propelled through the fumarole at last, can spout liquid and roll, further improvement the effect of reaction.

The invention also provides a preparation method of the lithium bis (fluorosulfonyl) imide, which is completed by adopting the preparation device of the lithium bis (fluorosulfonyl) imide, and comprises the following steps:

adding sulfamic acid, chlorosulfonic acid and thionyl chloride with the molar ratio of 0.8:1:1.8 into a reaction kettle, and performing temperature rise reaction by using the reaction kettle to obtain an imide acid reaction solution.

② after the reaction, rectifying the reaction liquid, separating the raw material which does not finish the reaction, and collecting the imine acid of the rectified fraction.

Thirdly, putting potassium fluoride and dimethyl carbonate into a reaction kettle, adding the obtained imide acid into the reaction kettle in the second step, wherein the molar ratio of the potassium fluoride to the imide acid is 1:3, the addition amount of the dimethyl carbonate is 2.5 times of that of the potassium fluoride, carrying out heating reaction after the imide acid is completely added until the pH value is 7, and then cooling and filtering to obtain a dimethyl carbonate solution.

Adding anhydrous lithium chloride and dimethyl carbonate with the molar ratio of 1:5 into the reaction kettle, and adding the dimethyl carbonate solution obtained in the step III to react to obtain crude product lithium bis (fluorosulfonyl) imide.

Fifthly, concentrating, evaporating, crystallizing and drying the crude product of the lithium bis (fluorosulfonyl) imide to obtain a finished product of the lithium bis (fluorosulfonyl) imide.

Preferably, the temperature rise in the first step is 80-150 ℃, and the heating time is 50 h.

Preferably, the addition of the imide acid in the step (c) and the addition of the dimethyl carbonate solution in the step (r) are both in a dropwise adding mode, and the dropwise adding time of the imide acid in the step (c) is 8-10 hours.

The reaction temperature in the step (iv) is preferably 45-65 ℃, and the reaction time is 3-5 h.

Advantageous effects

1. The invention provides a device for preparing lithium bis (fluorosulfonyl) imide, which utilizes a driving mechanism to drive a hollow rod to rotate, so that a stirring blade rotates, and the effect of preliminary stirring reaction is achieved. Specifically speaking, actuating mechanism's driving motor orders about the second drive wheel and rotates, realizes the rotation of first drive wheel through the drive belt, and first drive wheel rotates and drives hollow rod and rotate to make the stirring leaf rotate, reach preliminary stirring reaction's effect.

2. The invention provides a preparation device of lithium bis (fluorosulfonyl) imide, which utilizes the rotation of a hollow rod to drive a second bevel gear to rotate, and the second bevel gear is meshed with a first bevel gear, so that the rotation of two spiral rods is realized, and liquid entering from a liquid inlet can be discharged through a liquid discharge port under the pushing of the spiral rods, so that the liquid in the center of a reaction kettle can flow to the edge, and the full reaction of the liquid is facilitated.

3. The invention provides a device for preparing lithium bis (fluorosulfonyl) imide, which utilizes a pneumatic power assembly of a pneumatic mechanism to inject outside air into a hollow rod through a connecting pipe, then the outside air enters a gas spraying assembly and is sprayed out, so that sprayed liquid can roll over, and the reaction effect is further improved. Specifically speaking, through opening the air-blower, utilize the air-blower to pass through the connecting pipe with the outside air and pour into hollow pole in, get into the annular ring through the opening afterwards in, get into the inside of annular pipe through intercommunicating pore and communicating pipe again, it is jet-propelled through the fumarole at last, can spout liquid and roll, further improvement the effect of reaction.

4. The invention provides a device and a method for preparing lithium bis (fluorosulfonyl) imide, which have the advantages of short reaction flow and less generated waste, and can be used for fully mixing and reacting raw materials added into a reaction kettle, so that the reaction effect of the raw materials is greatly improved.

Drawings

Fig. 1 is a schematic structural diagram of a device for preparing lithium bis (fluorosulfonyl) imide in example 1.

Fig. 2 is a sectional view taken along line a-a in fig. 1.

FIG. 3 is a schematic top view of a ring-shaped tube in the apparatus for preparing lithium bis (fluorosulfonyl) imide in example 1.

Fig. 4 is a perspective view of a mounting plate in the apparatus for preparing lithium bis (fluorosulfonyl) imide in example 1.

The device comprises a reaction kettle 1, a blower 2, a connecting pipe 3, a rotary joint 4, a mounting rack 5, a first transmission wheel 6, a second transmission wheel 7, a driving motor 8, a mounting plate 9, a feeding port 10, a liquid inlet 11, a partition plate 12, a first bevel gear 13, a second bevel gear 14, a screw rod 15, a liquid outlet 16, a stirring blade 17, a support 18, a ring pipe 19, an air jet hole 20, a supporting leg 21, a discharging port 22, an annular sleeve 23, a communicating pipe 24, a hollow rod 25, an opening 26 and a communicating hole 27.

Detailed Description

The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.

Example 1

A device for preparing lithium bis (fluorosulfonyl) imide comprises a reaction kettle 1, a driving mechanism and a pneumatic mechanism.

The driving mechanism is positioned above the outer side of the top of the reaction kettle 1.

The pneumatic mechanism mainly comprises a pneumatic power assembly and a gas spraying assembly, wherein the pneumatic power assembly is positioned above the outer side of the top of the reaction kettle 1, and the gas spraying assembly is positioned above the bottom in the reaction kettle 1.

A feeding hole 10 is formed in the top of the reaction kettle 1, a discharging hole 22 is formed in the lowest position of the bottom of the reaction kettle 1, and an outer half pipe for heating is arranged on the outer side of the reaction kettle 1.

A hollow rod 25 is arranged at the center of the upper part of the bottom in the reaction kettle 1, the bottom of the hollow rod 25 is connected with a gas ejection assembly of a driving mechanism, and the top of the hollow rod 25 penetrates through the inside of the reaction kettle 1, extends out of the reaction kettle 1 from the top of the reaction kettle 1 and is respectively connected with a pneumatic power assembly of the driving mechanism and a pneumatic mechanism.

A cavity is fixedly arranged at the upper part in the reaction kettle 1, a hollow rod 25 penetrates through the middle part of the cavity, two ends of the top of the cavity are connected with the inner wall of the reaction kettle 1, two liquid inlets 11 are symmetrically arranged at the positions, close to the hollow rod 25, of the center of the cavity, and two liquid outlets 16 are symmetrically arranged at the connecting part of the bottom of the cavity and the inner wall of the reaction kettle 1; two partition plates 12 are symmetrically arranged in the cavity below the inner side of the liquid inlet 11, the upper ends of the partition plates 12 are connected with the top of the cavity, the lower ends of the partition plates 12 are connected with the bottom of the cavity, the interior of the cavity is divided into a central area and a peripheral area, so that liquid flows into the peripheral area but cannot enter the central area, the peripheral area of the cavity is symmetrically provided with two spiral rods 15, the outer ends of the spiral rods 15 are connected with the inner wall of the reaction kettle 1, and the inner ends of the spiral rods penetrate through the partition plates 12 and extend into the central area and are fixedly connected with a first bevel gear 13; the hollow rod 25 penetrates through the central region of the cavity, and a second bevel gear 14 is fixedly connected to the lower part of the central region of the cavity, and the second bevel gear 14 is meshed with the first bevel gear 13.

The hollow rod 25 is positioned in the reaction kettle 1, and a plurality of stirring blades 17 are connected and arranged on the part outside the cavity.

The bottom of the reaction kettle 1 is funnel-shaped, and a plurality of support legs 21 are fixedly connected to the outer side of the bottom of the reaction kettle 1 and used for supporting the reaction kettle 1.

The screw rods 15 are composed of a rod body and spiral blades fixedly wound on the periphery of the rod body, and the spiral directions of the two screw rods 15 are opposite.

The driving mechanism comprises a first driving wheel 6, a second driving wheel 7, a driving motor 8 and a mounting plate 9. The mounting plate 9 is composed of two triangular support plates and a rectangular plate, and the two triangular support plates are symmetrically arranged on the side wall of the rectangular plate, so that the supporting effect is achieved. Mounting panel 9 fixed connection is in 1 top outside top of reation kettle top, and the lateral wall fixedly connected with driving motor 8 of mounting panel 9, and driving motor 8's output shaft end rotates with reation kettle 1 top to be connected, and driving motor 8's output shaft cover is equipped with second drive wheel 7, and hollow rod 25 stretches out and is equipped with first drive wheel 6 on the lower part of reation kettle 1 top part, is connected through transmission belt transmission between first drive wheel 6 and the second drive wheel 7.

The pneumatic power assembly of the pneumatic mechanism comprises a bracket 18, an annular pipe 19, an annular sleeve 23 and a communicating pipe 24. Annular tube 19 fixed connection is bottom top in reation kettle 1, and annular tube 19's top is equidistant to be provided with a plurality of fumarole 20, and hollow rod 25 bottom is connected with annular tube 19, and concrete connection mode is: the outer side of the hollow rod 25 is sleeved with an annular sleeve 23, a plurality of openings 26 are formed in the circumferential direction of the side wall of the bottom of the hollow rod 25 at equal intervals, the openings 26 are located inside the annular sleeve 23, the annular sleeve 23 is rotatably connected with the hollow rod 25, dynamic sealing treatment is conducted through a rotary sealing ring, two communicating holes 27 are symmetrically formed in the annular sleeve 23, two communicating pipes 24 matched with the communicating holes 27 are fixedly connected to the annular sleeve 23, and one end, away from the annular sleeve 23, of each communicating pipe 24 is communicated with the annular pipe 19. Two brackets 18 for supporting the communicating tubes 24 are symmetrically arranged on the inner side of the bottom of the reaction kettle 1.

The gas ejection assembly of the pneumatic mechanism includes a blower 2, a connection pipe 3, a rotary joint 4, and a mounting bracket 5. Air-blower 2 is located 1 top outside top of reation kettle, and mounting bracket 5 is located the part that the adjacent hollow rod 25 in 1 top outside top of reation kettle stretches out 1 top of reation kettle, and mounting bracket 5 is the type of falling L structure, fixedly connected with rotary joint 4 on mounting bracket 5, and the top intercommunication that the 4 lower extremes of rotary joint and hollow rod 25 stretch out 1 top of reation kettle, and air-blower 2 is through connecting pipe 3 and 4 upper end intercommunications of rotary joint.

When the device is in operation:

the driving motor 8 is used for driving the second driving wheel 7 to rotate, the first driving wheel 6 is driven to rotate through a driving belt, the hollow rod 25 can be driven to rotate through the rotation of the first driving wheel 6, and therefore the stirring blades 17 are driven to rotate, and the effect of preliminary stirring reaction is achieved;

the hollow rod 25 rotates to drive the second bevel gear 14 to rotate, and the second bevel gear 14 is meshed with the first bevel gear 13, so that the two spiral rods 15 rotate, and liquid entering from the liquid inlet 11 can be discharged through the liquid outlet 16 under the pushing action of the spiral rods 15, so that the liquid in the center of the reaction kettle 1 can flow to the edge, and the liquid can be fully reacted;

the blower 2 is turned on, outside air can be injected into the hollow rod 25 through the connecting pipe 3 by the blower 2, then enters the annular sleeve 23 through the opening 26, enters the annular pipe 19 through the communicating hole 27 and the communicating pipe 24, and finally is sprayed through the spraying holes 20, so that the sprayed liquid rolls over, and the reaction effect is further improved.

Example 2

A method for preparing lithium bis (fluorosulfonyl) imide, which is performed by the apparatus for preparing lithium bis (fluorosulfonyl) imide described in embodiment 1, and which comprises the following steps:

adding sulfamic acid, chlorosulfonic acid and thionyl chloride with the molar ratio of 0.8:1:1.8 into a reaction kettle 1, and performing heating reaction by using the reaction kettle 1 at the temperature of 80 ℃ for 50 hours to obtain an imide acid reaction solution.

② after the reaction, rectifying the reaction liquid, separating the raw material which does not finish the reaction, and collecting the imine acid of the rectified fraction.

Thirdly, putting potassium fluoride and dimethyl carbonate into a reaction kettle 1, then adding dropwise the potassium fluoride and dimethyl carbonate into the reaction kettle 1 to obtain the imide acid, wherein the dropwise adding time is 8 hours, the molar ratio of the potassium fluoride to the imide acid is 1:3, the addition amount of the dimethyl carbonate is 2.5 times of that of the potassium fluoride, after the imide acid is completely added, the heating reaction is carried out until the pH value is 7, and then, the temperature is reduced and the dimethyl carbonate solution is obtained after filtration.

Adding anhydrous lithium chloride and dimethyl carbonate with the molar ratio of 1:5 into a reaction kettle 1, dropwise adding the dimethyl carbonate solution obtained in the step III, reacting at the reaction temperature of 45 ℃ for 3 hours to obtain crude product lithium bis (fluorosulfonyl) imide.

Fifthly, concentrating, evaporating, crystallizing and drying the crude product of the lithium bis (fluorosulfonyl) imide to obtain a finished product of the lithium bis (fluorosulfonyl) imide, wherein the yield is 70%.

The lithium bis (fluorosulfonyl) imide product prepared in this example was tested as follows:

(1) detecting by using a 400M nuclear magnetic resonance spectrometer of Bruker company, and determining that the purity of the product is 99.9% according to the proportion of the integral area of the product to the integral areas of other impurities; wherein, the moisture content is less than or equal to 1ppm, and a Karl Fischer moisture meter is used for detection; the content of chloride ions is less than or equal to 1ppm, and ultraviolet-visible spectrum colorimetric analysis is used for detection; the content of fluorine ions is less than or equal to 1ppm, and a fluorine ion electrode is used for detection; the potassium ion content is less than or equal to 1ppm and is detected by using inductively coupled plasma mass spectrometry.

Example 3

A method for preparing lithium bis (fluorosulfonyl) imide, which is performed by the apparatus for preparing lithium bis (fluorosulfonyl) imide described in embodiment 1, and which comprises the following steps:

adding sulfamic acid, chlorosulfonic acid and thionyl chloride with the molar ratio of 0.8:1:1.8 into a reaction kettle 1, and performing temperature rise reaction by using the reaction kettle 1 at the temperature of 120 ℃ for 50 hours to obtain an imide acid reaction solution.

② after the reaction, rectifying the reaction liquid, separating the raw material which does not finish the reaction, and collecting the imine acid of the rectified fraction.

Thirdly, putting potassium fluoride and dimethyl carbonate into a reaction kettle 1, then adding dropwise the potassium fluoride and dimethyl carbonate into the reaction kettle 1 to obtain the imide acid, wherein the dropwise adding time is 9 hours, the molar ratio of the potassium fluoride to the imide acid is 1:3, the addition amount of the dimethyl carbonate is 2.5 times of that of the potassium fluoride, after the imide acid is completely added, the heating reaction is carried out until the pH value is 7, and then, the temperature is reduced and the dimethyl carbonate solution is obtained after filtration.

Adding anhydrous lithium chloride and dimethyl carbonate with the molar ratio of 1:5 into a reaction kettle 1, dropwise adding the dimethyl carbonate solution obtained in the step III, reacting at the reaction temperature of 60 ℃ for 4 hours to obtain crude product lithium bis (fluorosulfonyl) imide.

Fifthly, concentrating, evaporating, crystallizing and drying the crude product of the lithium bis (fluorosulfonyl) imide to obtain the finished product of the lithium bis (fluorosulfonyl) imide, wherein the yield is 78%.

The lithium bis (fluorosulfonyl) imide product prepared in this example was tested as follows:

(1) detecting by using a 400M nuclear magnetic resonance spectrometer of Bruker company, and determining that the purity of the product is 99.9% according to the proportion of the integral area of the product to the integral areas of other impurities; wherein, the moisture content is less than or equal to 1ppm, and a Karl Fischer moisture meter is used for detection; the content of chloride ions is less than or equal to 1ppm, and ultraviolet-visible spectrum colorimetric analysis is used for detection; the content of fluorine ions is less than or equal to 1ppm, and a fluorine ion electrode is used for detection; the potassium ion content is less than or equal to 1ppm and is detected by using inductively coupled plasma mass spectrometry.

Example 4

A method for preparing lithium bis (fluorosulfonyl) imide, which is performed by the apparatus for preparing lithium bis (fluorosulfonyl) imide described in embodiment 1, and which comprises the following steps:

adding sulfamic acid, chlorosulfonic acid and thionyl chloride with the molar ratio of 0.8:1:1.8 into a reaction kettle 1, and performing heating reaction by using the reaction kettle 1 at the temperature of 150 ℃ for 50 hours to obtain an imide acid reaction solution.

② after the reaction, rectifying the reaction liquid, separating the raw material which does not finish the reaction, and collecting the imine acid of the rectified fraction.

Thirdly, putting potassium fluoride and dimethyl carbonate into a reaction kettle 1, then adding dropwise the potassium fluoride and dimethyl carbonate into the reaction kettle 1 to obtain the imide acid, wherein the dropwise adding time is 10 hours, the molar ratio of the potassium fluoride to the imide acid is 1:3, the addition amount of the dimethyl carbonate is 2.5 times of that of the potassium fluoride, after the imide acid is completely added, the heating reaction is carried out until the pH value is 7, and then, the temperature is reduced and the dimethyl carbonate solution is obtained after filtration.

Adding anhydrous lithium chloride and dimethyl carbonate with the molar ratio of 1:5 into a reaction kettle 1, dropwise adding the dimethyl carbonate solution obtained in the step III, reacting at the reaction temperature of 65 ℃ for 5 hours to obtain crude product lithium bis (fluorosulfonyl) imide.

Fifthly, concentrating, evaporating, crystallizing and drying the crude product of the lithium bis (fluorosulfonyl) imide to obtain a finished product of the lithium bis (fluorosulfonyl) imide, wherein the yield is 73%.

The lithium bis (fluorosulfonyl) imide product prepared in this example was tested as follows:

(1) detecting by using a 400M nuclear magnetic resonance spectrometer of Bruker company, and determining that the purity of the product is 99.9% according to the proportion of the integral area of the product to the integral areas of other impurities; wherein, the moisture content is less than or equal to 1ppm, and a Karl Fischer moisture meter is used for detection; the content of chloride ions is less than or equal to 1ppm, and ultraviolet-visible spectrum colorimetric analysis is used for detection; the content of fluorine ions is less than or equal to 1ppm, and a fluorine ion electrode is used for detection; the potassium ion content is less than or equal to 1ppm and is detected by using inductively coupled plasma mass spectrometry.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.