Preparation method of lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and lithium fluoride, which is applied in the direction of tetrafluoroboric acid, boron halide compounds, electrochemical generators, etc., can solve the problem of difficult control of solid dosing, difficult control of reaction process, strong corrosion and irritation and other issues, to achieve good economic value and social value, easy to operate and control, and easy to operate

Inactive Publication Date: 2019-01-25
东营石大胜华新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem is that anhydrous hydrogen fluoride is a highly reactive substance, which can react with various substances, and is highly toxic, corrosive and irritating.
The existing problems are: the boron trifluoride complex is used to add lithium fluoride to the reaction, and the solid additi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:

[0024] 1) Add 2400g of dimethyl carbonate to the reaction device in an airtight manner, and then put in 100g of lithium fluoride. The lithium fluoride is high-purity lithium fluoride with a high purity greater than 99.5%. Under normal temperature and pressure, start stirring at a speed of 10~40rpm, to obtain lithium fluoride suspension (mass fraction is 4%);

[0025] 2) Slowly inject 310 g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 80 minutes to obtain a reaction solution; the mass fraction of lithium tetrafluoroborate in the obtained reaction solution is 13.09%;

[0026] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentrator under the protection of nitrog...

Embodiment 2

[0030] Embodiment 2, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:

[0031] 1) Sealedly add 2500g of ethyl methyl carbonate to the reaction device, and then put in 220g of lithium fluoride. The lithium fluoride is high-purity lithium fluoride with a high purity greater than 99.5%. Under normal temperature and pressure, start stirring at a speed of 30rpm, get 8.09% lithium fluoride suspension;

[0032] 2) Slowly inject 590 g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 110 minutes to obtain a reaction liquid; the mass fraction of lithium tetrafluoroborate in the obtained reaction liquid is 24.12%;

[0033] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentrator under the protection of nitrogen.

[0034]4) Heat up the filtrate ...

Embodiment 3

[0037] Embodiment 3, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:

[0038] 1) Airtightly add 1350g of the mother liquor filtered in Example 1 into the reaction device, then add 1100g of dimethyl carbonate, and then add 180g of lithium fluoride, the lithium fluoride is high-purity lithium fluoride, and its high purity is greater than 99.5 %, under normal temperature and pressure, start stirring, and the rotating speed is 40rpm to obtain lithium fluoride suspension;

[0039] 2) Slowly inject 480g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 100min to obtain a reaction solution; the mass fraction of lithium tetrafluoroborate in the obtained reaction solution is 23.23%;

[0040] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentr...

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PUM

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Abstract

The invention relates to a preparation method of lithium tetrafluoroborate. According to the technical scheme, the preparation method comprises the following steps that 1, under the ambient temperature and pressure, lithium fluoride is added into an esters solvent to obtain a lithium fluoride turbid liquid; 2, boron trifluoride gas is introduced into the lithium fluoride turbid liquid, and reaction is carried out for 1-2 h to obtain a lithium tetrafluoroborate solution; 3, unreacted trace lithium fluoride of the solution obtained in step 2 is filtered through a microporus filter; 4, the liquidafter filtration in step 3 is completed is subjected to concentration and degassing; 5, the solution after concentration is completed in step 4 is subjected to cooling crystallization, filtration anddrying to obtain a lithium tetrafluoroborate finished product. The preparation method of the lithium tetrafluoroborate has the advantages that adopted boron trifluoride is an industrial grade raw material, and is low and easy to obtain; the lithium fluoride forms the turbid liquid in the esters solvent, so that reaction is easily carried out, the operation is simple and convenient, the safety isimproved, and the problems of the risk in reaction and preparation when hydrogen fluoride is adopted as a solvent, excessive amount of free acid of the product, high energy consumption of ultralow-temperature crystallization and the like are avoided.

Description

technical field [0001] The invention relates to a preparation technology of an electrolyte material for a lithium ion battery, in particular to a preparation method of lithium tetrafluoroborate. Background technique [0002] In recent years, as the country vigorously promotes new energy vehicles and restricts the use of traditional fuel vehicles, the demand for energy other than non-petrochemical energy has increased significantly. As a green and clean energy explored and developed in the 21st century, lithium-ion batteries are widely used in the automotive field. It has been vigorously promoted and applied. With the rapid development of the application of power lithium-ion batteries, the different requirements for the environment, temperature and safety factors have put forward strict requirements on the electrolyte system. [0003] Lithium salts used in lithium-ion battery electrolytes are generally divided into lithium perchlorate (LiClO4), lithium tetrafluoroborate (LiB...

Claims

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Application Information

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IPC IPC(8): C01B35/06H01M10/0563
CPCH01M10/0563C01B35/066C01P2006/80C01P2006/82Y02E60/10
Inventor 郭建军
Owner 东营石大胜华新能源有限公司
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