Synthesis device of lithium difluoro (oxalato) borate
By using boron trifluoride raw material gas in the synthetic kettle and reacting with organic solvents of lithium oxalate, the problem of high impurity introduction and operation risks in the preparation process of lithium difluoroxalate difluoroxalate in the prior art is solved, and the effect of simplifying synthesis and reducing costs is achieved.
Patent Information
- Application Number
- CN202421714462.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-19
- Publication Date
- 2025-07-25
- Estimated Expiration
- 2034-07-19
AI Technical Summary
The existing preparation methods for lithium difluoroxalate borate are prone to introduce impurities, have high operating risks, and are costly, making it difficult to control the proportion of raw materials.
Boron trifluoride raw material gas is used to react with organic solvent dissolved with lithium oxalate in the synthetic kettle, and synthesize it through the pipeline connected to the synthetic kettle to avoid the use of additives and dangerous materials hydrogen fluoride, ensuring the stability of pipeline transportation and the simplicity of reaction.
The simplified synthesis process is achieved, reducing the risk of impurity introduction, improving the safety and control of operations, and reducing costs.
Smart Images
Figure CN223144708U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the field of preparation of lithium ion battery electrolytes, and particularly relates to a synthesis device for lithium difluorooxalate borate. Background Art
[0002] Lithium difluorooxalate borate is mainly used as an additive for non-aqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors, and is applied to the field of lithium salt for lithium ion battery electrolytes. Combining the advantages of lithium bis(oxalato)borate and lithium tetrafluoroborate, it has good high and low temperature performance, high conductivity and good thermal stability. As a new type of lithium salt, it can be used as a film-forming additive in lithium ion battery electrolytes or replace lithium hexafluorophosphate as a conductive salt.
[0003] At present, the preparation methods of this additive mainly include the following: 1. Lithium tetrafluoroborate and anhydrous oxalic acid react under the action of an organic solvent and a reaction assistant silicon tetrachloride to produce a lithium difluorooxalate borate product. This method is prone to introducing new impurities, has a high residual chlorine ion content, and generates a large amount of strong acidic gas during the reaction, and the tail gas treatment is cumbersome. The raw material lithium tetrafluoroborate is expensive, resulting in high costs; 2. Lithium difluorooxalate borate and lithium tetrafluoroborate are produced by reacting lithium oxalate with boron trifluoride complex, and then the product is obtained through repeated recrystallization purification and separation. It is difficult to control the proportion of each raw material in this method as both lithium oxalate and boron trifluoride complex are solids; 3. A hydrogen fluoride solution of lithium fluoride reacts with boron trichloride and oxalic acid at a certain temperature to obtain a hydrogen fluoride solution containing lithium difluorooxalate borate and lithium tetrafluoroborate. After removing the solvent, a solid mixture of lithium difluorooxalate borate and lithium tetrafluoroborate is obtained, and then lithium difluorooxalate borate is obtained through separation and purification. It is difficult to control the proportion of each raw material used in this method, and there are risks in operating with hydrogen fluoride during the preparation process.
[0004] Therefore, the applicant hopes to propose a new synthesis device for lithium difluorooxalate borate to solve the above technical problems. Summary of the Invention
[0005] In view of this, the purpose of the utility model is to provide a synthesis device for lithium difluorooxalate borate, which does not require the addition of additives, does not need to use dangerous hydrogen fluoride materials, and uses boron trifluoride raw material gas. The continuous pipeline transportation is easier to control, making the synthesis process simple and easy, without introducing other impurities, and greatly reducing the operation risk.
[0006] The technical solution adopted by the utility model is as follows:
[0007] A synthesis device for lithium difluorooxalate borate includes a synthesis kettle, wherein the synthesis kettle is respectively connected to an organic solvent feed pipeline, a solid lithium oxalate feeder, at least one boron trifluoride raw material gas feed pipeline, and a synthesis liquid discharge pipeline.
[0008] Preferably, the upper end of the synthesis kettle is connected to a first feed pipeline for boron trifluoride as a raw material gas, and the lower end of the synthesis kettle is connected to a second feed pipeline for boron trifluoride as a raw material gas.
[0009] Preferably, the first feed pipeline for boron trifluoride as a raw material gas includes a first branch pipeline A of the feed pipeline for boron trifluoride as a raw material gas and a first branch pipeline B of the feed pipeline for boron trifluoride as a raw material gas; wherein, the input ends of the first branch pipeline A of the feed pipeline for boron trifluoride as a raw material gas and the first branch pipeline B of the feed pipeline for boron trifluoride as a raw material gas are connected in parallel to the first feed pipeline for boron trifluoride as a raw material gas, and the output ends of the first branch pipeline A of the feed pipeline for boron trifluoride as a raw material gas and the first branch pipeline B of the feed pipeline for boron trifluoride as a raw material gas respectively penetrate through the upper end of the synthesis kettle and then extend to the lower end inside the synthesis kettle.
[0010] Preferably, a raw material gas feed port for plug-in connection with the second feed pipeline for boron trifluoride as a raw material gas is provided on the side wall of the lower end of the synthesis kettle, and after the second feed pipeline for boron trifluoride as a raw material gas is inserted into the raw material gas feed port, it extends into the interior of the synthesis kettle.
[0011] Preferably, the extending direction of the first feed pipeline for boron trifluoride as a raw material gas inside the synthesis kettle and the extending direction of the second feed pipeline for boron trifluoride as a raw material gas inside the synthesis kettle are non-parallel.
[0012] Preferably, the extending direction of the first feed pipeline for boron trifluoride as a raw material gas inside the synthesis kettle and the extending direction of the second feed pipeline for boron trifluoride as a raw material gas inside the synthesis kettle are perpendicular.
[0013] Preferably, a thermal circulation interlayer is provided on the outer periphery of the synthesis kettle, wherein the upper end and the lower end of the thermal circulation interlayer are respectively connected to a cold and hot medium discharge pipeline and a cold and hot medium feed pipeline.
[0014] Preferably, a nitrogen pipeline and a sampling port are respectively connected to the upper end of the synthesis kettle.
[0015] Preferably, a stirring device is provided inside the synthesis kettle.
[0016] Preferably, the organic solvent feed pipeline and the solid lithium oxalate feeder are respectively connected to the upper end of the synthesis kettle, and the synthetic liquid discharge pipeline is connected to the bottom of the synthesis kettle.
[0017] It should be noted that the lithium difluorooxalate borate synthesis liquid output through the synthetic liquid discharge pipeline can be obtained as a finished product of lithium difluorooxalate borate after subsequent well-known crystallization, filtration and washing, and drying. These subsequent treatment processes are common knowledge for those skilled in the art, and the present application will not specifically elaborate on them here.
[0018] The utility model provides a novel synthetic device for lithium difluoro(oxalato)borate, which comprises a synthesis kettle composed of an organic solvent feed pipeline, a solid lithium oxalate feeder, at least one raw material gas boron trifluoride feed pipeline and a synthetic liquid discharge pipeline. Based on the synthesis reaction of boron trifluoride gas and the organic solvent dissolved with lithium oxalate in the synthesis kettle, the product lithium difluoro(oxalato)borate and the by-product lithium tetrafluoroborate are obtained. Compared with the existing process, no additives are needed, dangerous hydrogen fluoride materials do not have to be used, and boron trifluoride raw material gas is used, and continuous pipeline transportation is easier to control, so that the synthesis process becomes simple and easy, no other impurities are introduced, and the operation risk is greatly reduced. Brief Description of the Drawings
[0019] Figure 1 It is a schematic structural diagram of the synthetic device for lithium difluoro(oxalato)borate under the specific embodiment of the utility model.
[0020] Reference numerals: synthesis kettle 1, raw material gas inlet 1a, organic solvent feed pipeline 2, solid lithium oxalate feeder 3, sampling port 4, vent pipeline 5, second raw material gas boron trifluoride feed pipeline 6, first raw material gas boron trifluoride feed pipeline 7, first raw material gas boron trifluoride feed pipeline branch A 7a, first raw material gas boron trifluoride feed pipeline branch B 7b, synthetic liquid discharge pipeline 8, cooling and heating medium feed pipeline 9, cooling and heating medium discharge pipeline 10, nitrogen pipeline 11. Detailed Embodiment
[0021] This embodiment provides a synthetic device for lithium difluoro(oxalato)borate, which comprises a synthesis kettle. Among them, the synthesis kettle is respectively connected with an organic solvent feed pipeline, a solid lithium oxalate feeder, at least one raw material gas boron trifluoride feed pipeline and a synthetic liquid discharge pipeline.
[0022] In order to enable those skilled in the art to better understand the technical solutions in the present utility model, the following will clearly and completely describe the technical solutions in the embodiments of the present utility model with reference to the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all of the embodiments. Based on the embodiments in the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present utility model.
[0023] Please refer to Figure 1As shown, a synthesis device for lithium difluorooxalate borate includes a synthesis kettle 1. Among them, the synthesis kettle 1 is respectively connected to an organic solvent feed pipeline 2, a solid lithium oxalate feeder 3, at least one raw material gas boron trifluoride feed pipeline, and a synthesis liquid discharge pipeline 8. Preferably, in this embodiment, the upper end of the synthesis kettle 1 is also respectively connected to a nitrogen gas pipeline 11 (for displacing the air inside the synthesis kettle 1, where the vent pipeline 5 is used to discharge the air) and a sampling port 4 (for sampling). The organic solvent feed pipeline 2 and the solid lithium oxalate feeder 3 are respectively connected to the upper end of the synthesis kettle 1, and the synthesis liquid discharge pipeline 8 is connected to the bottom of the synthesis kettle 1. Preferably, in order to facilitate the full mixing of raw materials, in this embodiment, a stirring device is also provided inside the synthesis kettle 1.
[0024] Preferably, in order to enable the raw material gas boron trifluoride to better participate in the reaction inside the synthesis kettle 1 and improve the synthesis efficiency, in this embodiment, the upper end of the synthesis kettle 1 is connected to a first raw material gas boron trifluoride feed pipeline 7, and the lower end of the synthesis kettle 1 is connected to a second raw material gas boron trifluoride feed pipeline 6. Further preferably, in this embodiment, the extending direction of the first raw material gas boron trifluoride feed pipeline 7 inside the synthesis kettle 1 and the extending direction of the second raw material gas boron trifluoride feed pipeline 6 inside the synthesis kettle 1 are non-parallel. Specifically preferably, the extending direction of the first raw material gas boron trifluoride feed pipeline 7 inside the synthesis kettle 1 is the axial direction of the synthesis kettle 1, and the extending direction of the second raw material gas boron trifluoride feed pipeline 6 inside the synthesis kettle 1 is perpendicular to the axial direction of the synthesis kettle 1.
[0025] Further specifically preferably, in this embodiment, the first raw material gas boron trifluoride feed pipeline 7 includes a first raw material gas boron trifluoride feed pipeline branch A7a and a first raw material gas boron trifluoride feed pipeline branch B7b. Among them, the input ends of the first raw material gas boron trifluoride feed pipeline branch A7a and the first raw material gas boron trifluoride feed pipeline branch B7b are connected in parallel to the first raw material gas boron trifluoride feed pipeline 7, and the output ends of the first raw material gas boron trifluoride feed pipeline branch A7a and the first raw material gas boron trifluoride feed pipeline branch B7b respectively penetrate the upper end of the synthesis kettle 1 and then extend to the lower end inside the synthesis kettle 1. A raw material gas inlet 1a for inserting and connecting with the second raw material gas boron trifluoride feed pipeline 6 is provided on the side wall of the lower end of the synthesis kettle 1, and the second raw material gas boron trifluoride feed pipeline 6 extends into the synthesis kettle 1 after being inserted into the raw material gas inlet 1a.
[0026] In actual implementation and application, boron trifluoride of the raw material gas is inserted into the bottom (i.e., the lower end inside) of the synthesis kettle 1 through the input end of the first branch line A7a of the boron trifluoride feed pipeline for the raw material gas and the first branch line B7b of the boron trifluoride feed pipeline for the raw material gas respectively. The second boron trifluoride feed pipeline 6 for the raw material gas enters the inside of the synthesis kettle 1 from the lower side wall of the synthesis kettle 1, ensuring that the boron trifluoride of the raw material gas fully reacts with lithium oxalate dissolved in the solvent in the synthesis kettle 1;
[0027] Preferably, in order to control the temperature environment required for the synthesis reaction, in this embodiment, a thermal circulation jacket is provided on the outer periphery of the synthesis kettle 1. Among them, the upper end and the lower end of the thermal circulation jacket are respectively connected with a cold and hot medium discharge pipeline 10 and a cold and hot medium feed pipeline 9.
[0028] During actual operation, after opening the nitrogen pipeline 11 to displace the air in the synthesis kettle 1, an organic solvent is quantitatively transported into the synthesis kettle 1 at one time through the organic solvent feed pipeline 2, and then the motor of the stirring device in the synthesis kettle 1 is started for stirring; then a certain amount of raw material solid lithium oxalate is added through the solid lithium oxalate feeder 3 and stirred and mixed evenly in the synthesis kettle 1; the required reaction temperature is controlled, and the boron trifluoride of the raw material gas is continuously and stably transported into the synthesis kettle 1 through the first boron trifluoride feed pipeline 7 for the raw material gas and the second boron trifluoride feed pipeline 6 for the raw material gas. After the synthesis reaction is completed, the synthesis liquid is transferred through the synthesis liquid discharge pipeline 8, then filtered through a filter, and then enters subsequent processes such as crystallization, filtration and washing, and drying to obtain the required pure lithium difluorooxalate borate.
[0029] For those skilled in the art, it is obvious that the present utility model is not limited to the details of the above-described exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic characteristics of the present utility model. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present utility model is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present utility model. Any reference signs in the claims should not be regarded as limiting the claimed rights.
[0030] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A synthesis device for lithium difluorooxalate borate, characterized in that, It includes a synthesis kettle (1), wherein the synthesis kettle (1) is respectively connected to an organic solvent feed pipeline (2), a solid lithium oxalate feeder (3), at least one raw material gas boron trifluoride feed pipeline, and a synthesis liquid discharge pipeline (8).
2. The synthesis device of lithium difluorooxalate borate according to claim 1, wherein, The upper end of the synthesis kettle (1) is connected to a first raw material gas boron trifluoride feed pipeline (7), and the lower end of the synthesis kettle (1) is connected to a second raw material gas boron trifluoride feed pipeline (6).
3. The synthesis device of lithium difluorooxalate borate according to claim 2, characterized in that, The first raw material gas boron trifluoride feed pipeline (7) includes a first raw material gas boron trifluoride feed pipeline branch A (7a) and a first raw material gas boron trifluoride feed pipeline branch B (7b); wherein, The input end of the first raw material gas boron trifluoride feed pipeline branch A (7a) and the input end of the first raw material gas boron trifluoride feed pipeline branch B (7b) are connected in parallel to the first raw material gas boron trifluoride feed pipeline (7), and the output end of the first raw material gas boron trifluoride feed pipeline branch A (7a) and the output end of the first raw material gas boron trifluoride feed pipeline branch B (7b) respectively penetrate the upper end of the synthesis kettle (1) and then extend to the lower end inside the synthesis kettle (1).
4. The synthesis device of lithium difluorooxalate borate according to claim 2 or 3, characterized in that, A raw material gas inlet (1a) for insertion connection with the second raw material gas boron trifluoride feed pipeline (6) is provided on the side wall at the lower end of the synthesis kettle (1), and the second raw material gas boron trifluoride feed pipeline (6) extends into the synthesis kettle (1) after being inserted into the raw material gas inlet (1a).
5. The synthesis device of lithium difluoro(oxalato)borate according to claim 2, wherein The extending direction of the first raw material gas boron trifluoride feed pipeline (7) inside the synthesis kettle (1) is non-parallel to the extending direction of the second raw material gas boron trifluoride feed pipeline (6) inside the synthesis kettle (1).
6. The synthesis device of lithium difluoro(oxalato)borate according to claim 5, characterized in that, The extending direction of the first raw material gas boron trifluoride feed pipeline (7) inside the synthesis kettle (1) is perpendicular to the extending direction of the second raw material gas boron trifluoride feed pipeline (6) inside the synthesis kettle (1).
7. The synthesis device of lithium difluoro(oxalato)borate according to claim 1, wherein A thermal circulation jacket is provided on the outer periphery of the synthesis kettle (1), wherein the upper end and the lower end of the thermal circulation jacket are respectively connected to a cooling and heating medium discharge pipeline (10) and a cooling and heating medium feed pipeline (9).
8. The synthesis device of lithium difluoro(oxalato)borate according to claim 1, wherein The upper end of the synthesis kettle (1) is also respectively connected to a nitrogen pipeline (11) and a sampling port (4).
9. The synthesis device of lithium difluoro(oxalato)borate according to claim 1, characterized in that, A stirring device is provided inside the synthesis kettle (1).
10. The synthesis apparatus of lithium difluoro(oxalato)borate according to claim 1 or 2, characterized in that, The organic solvent feed pipeline (2) and the solid lithium oxalate feeder (3) are respectively connected to the upper end of the synthesis kettle (1), and the synthesis liquid discharge pipeline (8) is connected to the bottom of the synthesis kettle (1).