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A kind of preparation method of lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and lithium fluoride, applied in tetrafluoroboric acid, boron halide compounds, etc., can solve the problems of low purity and high production cost of lithium tetrafluoroborate, achieve good economic value and social value, and short reaction time , the effect of mild reaction conditions

Active Publication Date: 2017-02-01
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of lithium tetrafluoroborate, which solves the problems of low purity and high production cost of lithium tetrafluoroborate obtained by the existing preparation method

Method used

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  • A kind of preparation method of lithium tetrafluoroborate

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Embodiment 1

[0027] The preparation method of the lithium tetrafluoroborate of the present embodiment comprises the following steps:

[0028] 1) Put 20g of lithium fluoride into the reaction device, pass 500g of anhydrous hydrogen fluoride into the reaction device, shake and dissolve under normal temperature and pressure, and obtain lithium fluoride solution (mass fraction is 3.85%);

[0029] 2) Slowly inject 100 g of boron trifluoride gas into the lithium fluoride solution obtained in step 1), and the reaction time is 40 minutes to obtain a mixed solution; the mass fraction of lithium tetrafluoroborate in the obtained mixed solution is 22%;

[0030] 3) Put the mixed solution obtained in step 2) into a PTFE bottle under the protection of nitrogen, put the PTFE bottle containing the mixed solution into a freezing bath to cool down and crystallize, start from 5°C, and cool down at a rate of 2°C / h After reaching -40°C, the crystals were obtained by filtration, and the obtained crystals were b...

Embodiment 2

[0033] The preparation method of the lithium tetrafluoroborate of the present embodiment comprises the following steps:

[0034] 1) Put 40g of lithium fluoride into the reaction device, pass 800g of anhydrous hydrogen fluoride into the reaction device, shake and dissolve under normal temperature and pressure, and obtain a lithium fluoride solution (mass fraction is 4.76%);

[0035] 2) Slowly inject 150 g of boron trifluoride gas into the lithium fluoride solution obtained in step 1), and the reaction time is 40 minutes to obtain a mixed solution; the mass fraction of lithium tetrafluoroborate in the obtained mixed solution is 22%;

[0036] 3) Put the mixed solution obtained in step 2) into a PTFE bottle under the protection of nitrogen, put the PTFE bottle containing the mixed solution into a freezing bath to cool down and crystallize, start from 5°C, and cool down at a rate of 2°C / h After reaching -40°C, the crystals were obtained by filtration, and the obtained crystals were...

Embodiment 3

[0039] The preparation method of the lithium tetrafluoroborate of the present embodiment comprises the following steps:

[0040] 1) Put 70g of lithium fluoride into the reaction device, pass 930g of anhydrous hydrogen fluoride into the reaction device, shake and dissolve under normal temperature and pressure, and obtain a lithium fluoride solution (mass fraction is 7%);

[0041] 2) Slowly inject 300 g of boron trifluoride gas into the lithium fluoride solution obtained in step 1), and the reaction time is 30 minutes to obtain a mixed solution; the mass fraction of lithium tetrafluoroborate in the obtained mixed solution is 22%;

[0042] 3) Put the mixed solution obtained in step 2) into a PTFE bottle under the protection of nitrogen, put the PTFE bottle containing the mixed solution into a freezing bath to cool down and crystallize, start from 5°C, and cool down at a rate of 2°C / h After reaching -40°C, the crystals were obtained by filtration, and the obtained crystals were bl...

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Abstract

The invention discloses a preparation method of lithium tetrafluoroborate. The preparation method comprises the following steps of (1) dissolving lithium fluoride in anhydrous hydrogen fluoride at a normal temperature and normal pressure to obtain a lithium fluoride solution; (2) introducing a boron trifluoride gas into the lithium fluoride solution obtained by the step (1), and reacting for 30-60 min to obtain a mixed solution; and (3) cooling the mixed solution obtained by the step (2) for crystallization, filtering and drying to obtain lithium tetrafluoroborate. According to the preparation method of lithium tetrafluoroborate, boron trifluoride is an industrial grade raw material, is cheap and easily available; reaction conditions are mild; a reaction time is short; energy consumption is low; production cost is reduced; the obtained lithium tetrafluoroborate has good quality; a purity of the product reaches over 99.5%; and moisture content is controlled below 100 ppm. The lithium tetrafluoroborate completely meets production requirements of lithium ion batteries and has very good economic values and social values; and a synthetic process is simple, is convenient to operate and control and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of lithium tetrafluoroborate, and in particular relates to a preparation method of lithium tetrafluoroborate. Background technique [0002] For a long time, the depletion of fossil energy and environmental pollution have been the main problems faced by countries all over the world. As a green and clean energy explored and developed in the 21st century, lithium-ion batteries have been vigorously promoted and applied. With the continuous expansion of the application range of lithium-ion batteries, especially the rapid progress in the field of power batteries such as electric vehicles, the different requirements for the environment, temperature and safety factors have placed stringent requirements on the electrolyte system. [0003] Electrolyte is an indispensable part of the electrolyte of lithium-ion batteries and one of the determinants of the performance of lithium-ion batteries. Therefore, improving the e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06
CPCC01B35/063
Inventor 闫春生陈虎马广辉贾雪峰薛峰峰王永勤王艳君刘陈红
Owner DO FLUORIDE CHEM CO LTD
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