CN216378009U - Preparation device of lithium bis (oxalato) borate - Google Patents

Abstract

The utility model provides a device for preparing lithium bis (oxalato) borate, and belongs to the technical field of lithium battery electrolyte preparation devices. The device comprises a first reaction liquid tank, a second reaction liquid tank, a microchannel reactor, a chromatographic column and a molecular sieve filter column; a boron source, lithium hydroxide and an organic solvent are stored in the first reaction liquid tank; anhydrous oxalic acid and an organic solvent are stored in the second reaction liquid tank; the first reaction liquid tank and the second reaction liquid tank are respectively connected with a feed inlet of the microchannel reactor through pipelines; the discharge port of the microchannel reactor is connected with the chromatographic column through a pipeline; the discharge port of the chromatographic column is connected with the molecular sieve filter column through a pipeline; the discharge port of the molecular sieve filter column is connected with the feed port of the microchannel reactor through a pipeline. The device provided by the utility model can remove moisture in the reaction process and accelerate the reaction process.

Description

A kind of preparation device of lithium bis-oxalate borate

technical field

The utility model relates to the technical field of a lithium battery electrolyte preparation device, in particular to a preparation device for lithium bis-oxalate borate.

Background technique

Lithium borate complexes are a new class of electrolytes for lithium-ion batteries, of which LiBOB is the most representative. Lithium bis-oxalate borate is a kind of coordination chelate, the anion in the formed electrolyte is larger, the lattice energy is smaller, and more ions can be obtained in the solvent, thereby improving the conductivity of the electrolyte. Lithium bis(oxalate borate) (LiBOB) has good electrochemical stability and thermal stability, can react with specific solvents to form a stable SEI film, and can undergo multiple cycles without decay in energy. Compared with lithium hexafluorophosphate, it has higher thermal stability. , and the decomposed products B ₂ O ₃ and CO ₂ have little effect on battery performance and environment, and are a kind of electrolyte material with development potential in the lithium battery industry.

Currently, boron source, oxalic acid and lithium source are generally mixed to prepare lithium bis-oxalate borate, but water is generated during the reaction, which inhibits the progress of the reaction, and the reactivity of the three substances is poor, which requires high temperature and long time. The reaction can only generate lithium bis-oxalate borate, which is a great waste of energy.

Utility model content

In view of this, the utility model provides a preparation device of lithium bis-oxalate borate, which can remove water during the reaction process and accelerate the reaction process.

In order to achieve the above purpose, the utility model provides a preparation device for lithium bis-oxalate borate, comprising a first reaction liquid tank, a second reaction liquid tank, a microchannel reactor, a chromatography column and a molecular sieve filter column; A boron source, lithium hydroxide and an organic solvent are stored in the reaction liquid tank; anhydrous oxalic acid and an organic solvent are stored in the second reaction liquid tank; the first reaction liquid tank and the second reaction liquid tank are respectively connected with the The inlet of the microchannel reactor is connected; the outlet of the microchannel reactor is connected to the chromatography column through a pipeline; the outlet of the chromatography column is connected to the molecular sieve filter column through a pipeline; the molecular sieve filter column The outlet of the microchannel reactor is connected with the inlet of the microchannel reactor through a pipeline.

Preferably, on the pipeline connecting the first reaction tank and the microchannel reactor, the pipeline connecting the second reaction tank and the microchannel reactor, and the pipeline connecting the molecular sieve filter column and the microchannel reactor are respectively provided with peristalsis Pump.

Preferably, the column core of the chromatography column is an anhydrous inorganic salt, and sand cores are used for plugging at both ends of the column core.

Preferably, the type of molecular sieve used for the molecular sieve filter column is 3A, 4A, 5A, 10Z, 13Z or Y-type molecular sieve, and sand cores are used for plugging at both ends of the molecular sieve.

Preferably, the chromatographic column and the molecular sieve filter column are respectively provided with grinding mouths.

Preferably, the inner diameter of the microchannel reactor is 0.5-10 mm.

Preferably, a temperature sensor is provided on the microchannel reactor.

Preferably, valves are arranged on the pipeline connecting the microchannel reactor with the chromatographic column and on the pipeline connecting the chromatographic column and the molecular sieve filter column.

Preferably, a product tank is also included, and the product tank is connected to the molecular sieve filter column through a pipeline.

Compared with the prior art, the advantages and positive effects of the present utility model are:

The utility model provides a preparation device for lithium bis-oxalate borate. A microchannel reactor is connected to a chromatographic column, the materials can be efficiently and rapidly reacted in the microchannel reactor, and directly transferred to a chromatographic column after the reaction, dehydrated, and then The molecular sieve filter column further adsorbs the water generated in the process, and the outlet is connected to the feed of the microchannel reactor, and the dehydrated solution continues to flow back into the reactor to continue the reaction. In the reaction process, water is directly removed to accelerate the reaction. And finally a product of lithium bis-oxalate borate with sufficient reaction and less water content is obtained.

Description of drawings

The accompanying drawings described herein are used to provide further understanding of the present invention and constitute a part of the present application. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the attached image:

Fig. 1 is the structural representation of the preparation device of the lithium bis-oxalate borate of the present invention;

Fig. 2 is the structural representation of the chromatography column of the present invention;

Fig. 3 is the structural representation of the molecular sieve of the present utility model;

Among them: 1- first reaction liquid tank, 2- second reaction liquid tank, 3- micro-channel reactor, 4- chromatography column, 5- molecular sieve filter column, 6- peristaltic pump, 7- temperature sensor, 8- valve , 9-sand core, 10-inorganic salt, 11-grinding mouth, 12-molecular sieve membrane.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

The utility model provides a preparation device for lithium bis-oxalate borate, comprising a first reaction liquid tank 1, a second reaction liquid tank 2, a microchannel reactor 3, a chromatography column 4 and a molecular sieve filter column 5; A boron source, lithium hydroxide and an organic solvent are stored in the reaction liquid tank 1; anhydrous oxalic acid and an organic solvent are stored in the second reaction liquid tank 2; the first reaction liquid tank 1 and the second reaction liquid tank 2 are stored are respectively connected with the feed port of the microchannel reactor 3 through the pipeline; the discharge port of the microchannel reactor 3 is connected with the chromatographic column 4 through the pipeline; the discharge port of the chromatographic column 4 is filtered with the molecular sieve through the pipeline The column 5 is connected; the outlet of the molecular sieve filter column 5 is connected to the inlet of the microchannel reactor 3 through a pipeline.

During operation, the material in the first reaction liquid tank 1 and the material in the second reaction liquid tank 2 are respectively transferred into the microchannel reactor 3 for reaction, and the reacted product is dehydrated in the chromatographic column 4, and part of the moisture is adsorbed. In the chromatography column 4, the partially dehydrated material enters the molecular sieve filter column 5 for dehydration again, and the dehydrated material is recycled to the microchannel reactor 3 again, and the reaction is circulated in this way until the reaction ends.

In the present invention, in order to control the flow rate and facilitate transportation, it is preferable to use the pipeline connecting the first reaction tank 1 and the microchannel reactor 3, the pipeline connecting the second reaction tank 2 and the microchannel reactor 3, and the molecular sieve Peristaltic pumps 6 are respectively provided on the pipelines connecting the filter column 5 and the microchannel reactor 3 .

In the present invention, in order to absorb water, the column core of the chromatography column 4 is preferably anhydrous inorganic salt, and sand cores 9 are used for plugging at both ends of the column core.

In the present utility model, in order to fully dehydrate, the molecular sieves of the molecular sieve filter column 5 are 3A, 4A, 5A, 10Z, 13Z or Y-type molecular sieves, and sand cores 9 are used at both ends of the molecular sieve for plugging.

In the present invention, in order to facilitate the replacement of the column core or the molecular sieve, the chromatographic column 4 and the molecular sieve filter column 5 are preferably provided with grinding mouths 11, respectively, through which the chromatographic column 4 or the molecular sieve filtering column 5 can be cleaned. Disassemble and replace the cartridge or molecular sieve.

In the present invention, the inner diameter of the microchannel reactor 3 is preferably 0.5-10 mm.

In the present invention, in order to facilitate temperature regulation, the microchannel reactor 3 is preferably provided with a temperature sensor 7 .

In the present invention, in order to facilitate the control of materials, valves 8 are preferably arranged on the pipeline connecting the microchannel reactor 3 and the chromatographic column 4 and on the pipeline connecting the chromatographic column 4 and the molecular sieve filter column 5 .

In the present invention, in order to collect the product, it is preferable to further include a product tank 13, and the product tank 13 is connected with the molecular sieve filter column 5 through a pipeline.

The above is only the preferred embodiment of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made. These improvements and Retouching should also be regarded as the protection scope of the present invention.

Claims (9)

1. a preparation device for lithium bis-oxalate borate, is characterized in that, comprises the first reaction liquid tank, the second reaction liquid tank, microchannel reactor, chromatography column and molecular sieve filter column; Described first reaction liquid tank and The second reaction liquid tank is connected to the feed port of the microchannel reactor through pipelines respectively; the discharge opening of the microchannel reactor is connected to the chromatography column through pipelines; the discharge opening of the chromatography column is connected to the molecular sieve through pipelines The filter column is connected; the outlet of the molecular sieve filter column is connected with the inlet of the microchannel reactor through a pipeline. 2. preparation device according to claim 1 is characterized in that, on the pipeline that the first reaction tank is connected with the microchannel reactor, on the pipeline that the second reaction tank is connected with the microchannel reactor, and on the molecular sieve filter column Peristaltic pumps are respectively arranged on the pipelines connected with the microchannel reactor. 3 . The preparation device according to claim 1 , wherein the column core of the chromatography column is an anhydrous inorganic salt, and sand cores are used for plugging at both ends of the column core. 4 . 4. The preparation device according to claim 1, characterized in that, the molecular sieves for the molecular sieve filter column are 3A, 4A, 5A, 10Z, 13Z or Y-type molecular sieves, and sand cores are used for plugging at both ends of the molecular sieve. 5 . The preparation device according to claim 1 , wherein the chromatographic column and the molecular sieve filter column are respectively provided with grinding mouths. 6 . 6 . The preparation device according to claim 1 , wherein the inner diameter of the microchannel reactor is 0.5-10 mm. 7 . 7 . The preparation device according to claim 1 , wherein a temperature sensor is provided on the microchannel reactor. 8 . 8 . The preparation device according to claim 1 , wherein valves are arranged on the pipeline connecting the microchannel reactor with the chromatography column and on the pipeline connecting the chromatography column and the molecular sieve filter column. 9 . 9 . The preparation device according to claim 1 , further comprising a product tank connected to the molecular sieve filter column through a pipeline. 10 .

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