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Preparation method of lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and fluorine gas, applied in tetrafluoroboric acid, boron halide compounds, etc., can solve the problem of difficulty in removing water from lithium tetrafluoroborate, and achieve low water content, high raw material utilization, and no three wastes. Effect

Inactive Publication Date: 2015-06-10
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a method for preparing lithium tetrafluoroborate with simple process operation, environmental friendliness and low water content in the obtained product, which solves the problem of difficult water removal in existing lithium tetrafluoroborate products

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0032] The preparation method of lithium tetrafluoroborate of this embodiment includes the following steps:

[0033] 1) At -10℃, according to H 3 BO 3 The molar ratio to HF is 1:4, boric acid is slowly added to hydrofluoric acid with a concentration of 10% by mass, and then stirring is continued for 2 hours to react to obtain a fluoroboric acid solution;

[0034] 2) According to the molar ratio of Li to B of 1.05:1, lithium carbonate was added to the fluoroboric acid solution obtained in step 1), and the reaction was stirred at 100°C for 0.5h to obtain a lithium tetrafluoroborate solution;

[0035] 3) Concentrate the lithium tetrafluoroborate solution obtained in step 2) at -0.05MPa and 90°C, concentrate to 1 / 8 of the original volume of the lithium tetrafluoroborate solution, and then lower it to room temperature and 20°C for crystallization and filtration. The obtained solid is lithium tetrafluoroborate crystal;

[0036] 4) The lithium tetrafluoroborate crystal obtained in step 3) wa...

Embodiment 2

[0039] The preparation method of lithium tetrafluoroborate of this embodiment includes the following steps:

[0040] 1) At -5℃, according to H 3 BO 3 The molar ratio of HF to HF is 1:5, boric acid is slowly added to hydrofluoric acid with a concentration of 40% by mass, and then stirring is continued and reacted for 1 hour to obtain a fluoroboric acid solution;

[0041] 2) According to the molar ratio of Li to B of 1.10:1, lithium hydroxide is added to the fluoroboric acid solution obtained in step 1), and the reaction is stirred at 90°C for 2 hours to obtain a lithium tetrafluoroborate solution;

[0042] 3) Concentrate the lithium tetrafluoroborate solution obtained in step 2) under the conditions of -0.09MPa and 50°C, concentrate to 1 / 6 of the original volume of the lithium tetrafluoroborate solution, and then reduce to room temperature 20°C for crystallization and filtration. The obtained solid is lithium tetrafluoroborate crystal;

[0043] 4) The lithium tetrafluoroborate crystals...

Embodiment 3

[0046] The preparation method of lithium tetrafluoroborate of this embodiment includes the following steps:

[0047] 1) At 0℃, according to H 3 BO 3 The molar ratio to HF is 1:6, boric acid is slowly added to hydrofluoric acid with a concentration of 30% by mass, and then stirring is continued and reacted for 3 hours to obtain a fluoroboric acid solution;

[0048] 2) According to the molar ratio of Li to B of 1.20:1, add lithium bicarbonate to the fluoroboric acid solution obtained in step 1), and stir and react at 80°C for 3 hours to obtain a lithium tetrafluoroborate solution;

[0049] 3) Concentrate the lithium tetrafluoroborate solution obtained in step 2) under the conditions of -0.06MPa and 80°C, concentrate to 1 / 7 of the original volume of the lithium tetrafluoroborate solution, and then reduce to room temperature 20°C for crystallization and filtration. The obtained solid is lithium tetrafluoroborate crystal;

[0050] 4) The lithium tetrafluoroborate crystals obtained in step ...

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Abstract

The invention discloses a preparation method of lithium tetrafluoroborate. The preparation method comprises the following steps: 1) adding boric acid into hydrofluoric acid and reacting to obtain a fluoboric acid solution; 2) adding a lithium compound into the fluoboric acid solution and reacting to obtain a lithium tetrafluoroborate solution; 3) concentrating the lithium tetrafluoroborate solution, cooling, crystallizing and filtering to obtain lithium tetrafluoroborate crystals; 4) drying the lithium tetrafluoroborate crystals to obtain a lithium tetrafluoroborate crude product; and 5) putting the lithium tetrafluoroborate crude product into a reactor, introducing fluorine gas or fluorine-nitrogen mixed gas and reacting to obtain lithium tetrafluoroborate. According to the preparation method of lithium tetrafluoroborate disclosed by the invention, the deficiencies of the existing preparation method are made up, the process is simple to operate, no organic solvent is introduced, and the obtained lithium tetrafluoroborate product is high in purity and low in water content; and the whole preparation process is strong in operability and high in utilization rate of raw materials, has no emission of three wastes, and is suitable for large-scale industrial production.

Description

Technical field [0001] The invention belongs to the technical field of electrolyte lithium salts for lithium ion batteries, and specifically relates to a method for preparing lithium tetrafluoroborate. Background technique [0002] Electrolyte solution is an important part of lithium-ion battery, which plays the role of transporting ions and conducting current between the positive and negative electrodes, and is an indispensable part of completing the electrochemical reaction. Choosing a suitable electrolyte is also the key to obtain a lithium ion battery with high energy density and power density, long cycle life and good safety performance. The performance of the electrolyte directly affects the optimization and improvement of the performance of the lithium ion battery. At present, the electrolyte of commercial lithium-ion batteries is mainly lithium hexafluorophosphate (LiBF 6 ). Because lithium hexafluorophosphate has good electrical conductivity, can form a stable solid ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/06
CPCC01B35/066
Inventor 李云峰侯红军杨华春闫春生马广辉薛峰峰贾雪枫王艳君王永勤张永明
Owner DO FLUORIDE CHEM CO LTD
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