Lithium treatment device for lithium bis (trifluoromethanesulfonate)

Abstract

The invention relates to the technical field of lithiation devices, and discloses a lithium bis (trifluoromethanesulfonate) lithiation device which comprises a main body shell, an inner container is fixedly connected to the interior of the main body shell, a protective shell is fixedly connected to the surface of the inner container, and a first mounting plate is fixedly connected to the top of the inner container; the first mounting plate is fixedly connected with a second mounting plate through bolts, the top of the second mounting plate is fixedly connected with a sealing cover, the top of the sealing cover is fixedly connected with a sealing cover feeding pipe, and the top of the feeding pipe is fixedly connected with a connecting flange. By arranging two symmetrical feeding pipes and hastelloy micro-through pipes, an HTFSI acid solution and a lithium bicarbonate aqueous solution are premixed and preliminarily neutralized before entering the reaction box, and then are sprayed into a DMC cold bath through a tangential spray head in a high-speed rotation manner, so that a cascade reaction mode of pre-reaction first and then secondary dilution is realized, the reaction heat release peak value is reduced, and the reaction efficiency is improved. Local overheating of the reaction kettle is avoided, and raw materials in the reaction kettle are more uniformly reacted and mixed.

Description

Technical Field

[0001] This invention relates to the field of lithiumization equipment technology, specifically to a lithiumization equipment for lithium bis(trifluoromethanesulfonate). Background Technology

[0002] A lithiation device is a specialized device for pre-intercalating or replenishing lithium into the negative or positive electrode of a lithium-ion battery. Its core function is to quantitatively introduce active lithium into the electrode through electrochemical, self-discharge, or thermal-driven methods to compensate for the irreversible capacity loss during the first cycle and improve energy density and cycle life.

[0003] Lithium bis(trifluoromethanesulfonate) (LiTFSI) is the core lithium salt for high-performance electrolytes. Its synthesis requires the instantaneous neutralization of HTFSI acid and lithium bicarbonate at the end. The traditional direct drop-addition method in the reactor results in concentrated exothermic and uneven mixing, which can easily lead to local overheating and by-product LiF, affecting purity and scale-up stability. Therefore, a lithiumization equipment that can premix and disperse rapidly is needed. Summary of the Invention

[0004] To solve the above-mentioned technical problems, the present invention provides a lithiumization device for lithium bis(trifluoromethanesulfonate), comprising a main body shell, an inner liner fixedly connected inside the main body shell, a protective shell fixedly connected to the surface of the inner liner, a mounting plate one fixedly connected to the top of the inner liner, a mounting plate two fixedly connected to the mounting plate one by bolts, a cover fixedly connected to the top of the mounting plate two, a cover feed pipe fixedly connected to the top of the cover, a connecting flange fixedly connected to the top of the feed pipe, a Hastelloy microtube fixedly connected to the output end of the feed pipe, a reaction chamber fixedly connected to the output end of the reaction chamber, a connecting pipe fixedly connected to the output end of the connecting pipe, and a tangential nozzle fixedly installed at the output end of the connecting pipe.

[0005] The above technical solution integrates a Hastelloy microtube, a reaction chamber, and a tangential nozzle into a three-layer concentric shell consisting of a main outer shell, an inner liner, and a protective shell, all sealed with the same cover. This allows the acid and alkali solutions to complete all steps of premixing, instantaneous neutralization, and swirling spraying within a closed path, avoiding localized overheating inside the reactor caused by traditional dripping methods. This enables the lithiumation reaction to proceed at low temperature, high speed, and high purity.

[0006] As a further improvement to the above scheme, the first mounting plate and the second mounting plate are concentric, and there are two feed pipes, which are symmetrically distributed around the top center of the Hastelloy microtube.

[0007] With the above technical solution, the connecting pipe penetrates through the cap and is inserted directly into the inner liner. After the mixture is mixed inside the reaction chamber, it can be quickly transported into the inner liner through the connecting pipe.

[0008] As a further improvement to the above solution, the output end of the connecting pipe penetrates the inner wall of the cap and the inner liner.

[0009] With the above technical solution, the two feed pipes are symmetrically arranged at the top center of the microchannel, ensuring that the two liquids enter the microchannel with equal stroke and resistance.

[0010] As a further improvement to the above solution, a fixing tube is fixedly connected to the top of the cover, a drive motor is fixedly installed on the top of the fixing tube, a rotating rod is fixedly connected to the output end of the drive motor, and a stirring blade is fixedly connected to the surface of the rotating rod.

[0011] The above technical solution involves starting the drive motor, which in turn drives the rotating rod to rotate. The rotation of the rotating rod then drives the stirring blade to rotate, ensuring that the raw materials entering the inner liner are mixed evenly inside the liner.

[0012] As a further improvement to the above solution, the bottom of the rotating rod penetrates through the inner wall of the cap and the inner liner.

[0013] Through the above technical solution, the bottom of the rotating rod extends into the lower part of the inner tank, which can perform secondary radial shearing on the rotating liquid flow sprayed from the tangential nozzle, destroy the laminar flow boundary, and further improve the uniformity.

[0014] As a further improvement to the above solution, a support platform is fixedly connected to the surface of the main body shell, and the bottom of the support platform is provided with mounting holes.

[0015] As a further improvement to the above solution, the number of support platforms is set to three, and the three support platforms are evenly distributed on the surface with respect to the top center of the main shell.

[0016] Through the above technical solution, the support platform and the mounting hole form a three-point ground support, which distributes the force evenly, avoids equipment shaking at high speeds, and ensures the coaxial accuracy of the microchannel and the nozzle.

[0017] Compared with the prior art, the beneficial effects of the present invention are: This invention achieves a step-by-step reaction mode of pre-reaction followed by secondary dilution by setting up two symmetrical feed pipes and Hastelloy micro-channels, so that the HTFSI acid solution and lithium bicarbonate aqueous solution are pre-mixed and initially neutralized before entering the reaction tank, and then sprayed into the DMC cold bath at high speed through a tangential nozzle. This reduces the peak value of the reaction exothermic peak, avoids local overheating of the reaction vessel, and makes the internal raw material reaction and mixing more uniform.

[0018] This invention utilizes a tangential nozzle and a stirring blade to create a circulating flow from the tangential jet and a radial shearing effect from the stirring blade, resulting in a dual turbulence that allows the pre-reaction liquid to be fully and uniformly mixed with a large amount of cold DMC in the reactor. This shortens the overall reaction time and improves production efficiency. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic cross-sectional view of the overall structure of the present invention; Figure 3 This is a schematic diagram of the overall connection structure of the Hastelloy microtube of the present invention; Figure 4 This is a schematic diagram of the overall connection structure of the rotating rod of the present invention.

[0020] In the diagram: 1. Main outer shell; 2. Inner liner; 3. Protective shell; 4. Mounting plate one; 5. Mounting plate two; 6. Cover; 7. Feed pipe; 8. Connecting flange; 9. Hastelloy micro-tube; 10. Reaction chamber; 11. Connecting pipe; 12. Tangential nozzle; 13. Fixed pipe; 14. Drive motor; 15. Rotating rod; 16. Stirring blade; 17. Support platform; 18. Mounting hole. Detailed Implementation

[0021] The present invention will now be further described in conjunction with the accompanying drawings and specific embodiments. It should be noted that, without conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments. Example

[0022] Please combine Figure 1-4 The lithiumization device for lithium bis(trifluoromethanesulfonate) salt according to this embodiment includes a main shell 1, an inner liner 2 fixedly connected inside the main shell 1, a protective shell 3 fixedly connected to the surface of the inner liner 2, a mounting plate 4 fixedly connected to the top of the inner liner 2, a mounting plate 5 fixedly connected to the mounting plate 4 by bolts, a cover 6 fixedly connected to the top of the mounting plate 5, a cover feed pipe 7 fixedly connected to the top of the cover 6, a connecting flange 8 fixedly connected to the top of the feed pipe 7, a Hastelloy microtube 9 fixedly connected to the output end of the feed pipe 7, a reaction chamber 10 fixedly connected to the output end of the reaction chamber 10, a connecting pipe 11 fixedly connected to the output end of the connecting pipe 11, and a tangential nozzle 12 fixedly installed at the output end of the connecting pipe 11.

[0023] In use, the inner liner is filled with desiccant DMC solvent. Then, the two feed pipes 7 are connected to the external conveying pipe and pump. The HTFSI acid solution and lithium bicarbonate aqueous solution are then fed into the feed pipes 7 respectively, and enter the Hastelloy micro-channel 9 through the output end of the feed pipe. After contacting the Hastelloy micro-channel 9, the solution enters the reaction chamber 10 for instantaneous reaction and then enters the connecting pipe 11. Finally, it is sprayed into the inner liner 2 through the tangential nozzle 12, thus pre-reacting the reaction solvent inside the reaction vessel.

[0024] Mounting plate 1 4 and mounting plate 2 5 are concentric. There are two feed pipes 7, which are symmetrically distributed around the top center of Hastelloy micro-tube 9, so that the inner liner 2 and the cover 6 can be stably positioned during installation.

[0025] The output end of the connecting pipe 11 penetrates the inner wall of the inner liner 2 of the cap 6, and the connecting pipe 11 directly delivers the pre-reacted solution into the interior of the inner liner 2.

[0026] A fixed tube 13 is fixedly connected to the top of the cap 6. A drive motor 14 is fixedly installed on the top of the fixed tube 13. A rotating rod 15 is fixedly connected to the output end of the drive motor 14. A stirring plate 16 is fixedly connected to the rotating rod 15.

[0027] In use, the output end of the drive motor 14 drives the rotating rod 15 to rotate, so that the stirring plate 16 mixes the solution inside the inner liner and shears the solution sprayed from the tangential nozzle 12, so that it is evenly distributed inside the inner liner 2.

[0028] The bottom of the rotating rod 15 penetrates the inner wall of the cover 6 and the inner liner 2.

[0029] A support platform 17 is fixedly connected to the surface of the main body shell 1, and a mounting hole 18 is provided at the bottom of the support platform 17.

[0030] There are three support platforms 17, which are symmetrically and evenly distributed on the surface of the main body shell 1 with respect to the top center.

[0031] The implementation principle of the lithium lithiation device for lithium bis(trifluoromethanesulfonate) salt in this embodiment is as follows: First, the inner liner is filled with desiccant DMC solvent. Then, two feed pipes 7 are connected to external conveying pipes and pumps. Subsequently, HTFSI acid solution and lithium bicarbonate aqueous solution are fed into the feed pipes 7 respectively, and enter the Hastelloy micro-channel 9 through the output end of the feed pipe. After contacting the Hastelloy micro-channel 9, the solution enters the reaction tank 10 for instantaneous reaction and then enters the connecting pipe 11. It is then sprayed into the inner liner 2 through the tangential nozzle 12. By pre-reacting the reaction solvent inside the reaction vessel and spraying it out through the nozzle, the mixing reaction can be carried out quickly during the reaction process, making the reaction more complete.

[0032] Start the drive motor 14. The output end of the drive motor 14 drives the rotating rod 15 to rotate. The rotation of the rotating rod 15 drives the stirring plate 16 to rotate, so that the raw materials entering the inner liner 2 can be mixed evenly inside the inner liner 2.

[0033] The above embodiments are merely preferred embodiments of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-substantial changes and substitutions made by those skilled in the art based on the present invention shall fall within the scope of protection claimed by the present invention.

Claims

1. A lithiumization device for lithium bis(trifluoromethanesulfonate) salt, characterized in that: The device includes a main shell (1), an inner liner (2) fixedly connected inside the main shell (1), a protective shell (3) fixedly connected to the surface of the inner liner (2), a mounting plate (4) fixedly connected to the top of the inner liner (2), a mounting plate (5) fixedly connected to the mounting plate (4) by bolts, a cover (6) fixedly connected to the top of the mounting plate (5), a feed pipe (7) fixedly connected to the top of the cover (6), a connecting flange (8) fixedly connected to the top of the feed pipe (7), a Hastelloy micro-tube (9) fixedly connected to the output end of the feed pipe (7), a reaction chamber (10) fixedly connected to the output end of the reaction chamber (10), a connecting pipe (11) fixedly connected to the output end of the connecting pipe (11), and a tangential nozzle (12) fixedly installed at the output end of the connecting pipe (11).

2. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 1, characterized in that: The mounting plate one (4) and the mounting plate two (5) are concentric. There are two feed pipes (7), which are symmetrically distributed around the top center of the Hastelloy microtube (9).

3. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 1, characterized in that: The output end of the connecting pipe (11) passes through the inner wall of the cap (6) and the inner liner (2).

4. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 1, characterized in that: The top of the cover (6) is fixedly connected to a fixing tube (13), and a drive motor (14) is fixedly installed on the top of the fixing tube (13). A rotating rod (15) is fixedly connected to the output end of the drive motor (14), and a stirring plate (16) is fixedly connected to the surface of the rotating rod (15).

5. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 4, characterized in that: The bottom of the rotating rod (15) penetrates the inner wall of the cap (6) and the inner liner (2).

6. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 1, characterized in that: A support platform (17) is fixedly connected to the surface of the main body shell (1), and an installation hole (18) is provided at the bottom of the support platform (17).

7. The lithiumization apparatus for lithium bis(trifluoromethanesulfonate) salt according to claim 6, characterized in that: The number of the support platform (17) is three, and the three support platforms (17) are evenly distributed on the surface with the top center of the main shell (1) symmetrical.

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