Preparation method for lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and lithium carbonate, which is applied in the direction of borates, boron oxide compounds, and educts, can solve the problems of reducing the purity of lithium tetrafluoroborate, increasing production costs, and affecting the dehydration effect, achieving huge environmental benefits and social benefits, increase output rate, and improve product quality

Active Publication Date: 2013-08-07
DO FLUORIDE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has easy-to-obtain raw materials, low cost, and low energy consumption in the production process; but the solids are melted and wrapped during the drying process, which affects the dehydration effect and reduces the purity of the synthesized lithium tetrafluoroborate, and due to the use of a large amount of organic solvents as The extraction agent has certain pollution to the environment and increases the production cost, so this method is not suitable for industrial production

Method used

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  • Preparation method for lithium tetrafluoroborate
  • Preparation method for lithium tetrafluoroborate
  • Preparation method for lithium tetrafluoroborate

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Embodiment 1

[0043] The preparation method of lithium tetrafluoroborate of the present embodiment, technological process is as follows figure 1 shown, including the following steps:

[0044] 1) Lithium carbonate is prepared into a slurry with a mass fraction of 5%, and CO is continuously fed under a pressure of 1MPa 2 , the reaction produces LiHCO 3 , the reaction solution was filtered to obtain LiHCO 3 solution; the accuracy of the filtration is: the removal rate of solid particles with a particle size of 1 μm or more is greater than 99.9%;

[0045] 2) The LiHCO obtained in step 1) 3 solution with anhydrous hydrofluoric acid in LiHCO 3 Mix with anhydrous hydrofluoric acid at a molar ratio of 1:4, and react at room temperature for 2.5 hours to obtain LiF 3HF solution;

[0046] 3) Mix the LiF·3HF solution obtained in step 2) with the boric acid solution with a mass fraction of 5% at a molar ratio of LiF·3HF to boric acid of 1:1, and react to obtain a lithium tetrafluoroborate solution;...

Embodiment 2

[0049] The preparation method of lithium tetrafluoroborate of the present embodiment, technological process is as follows figure 1 shown, including the following steps:

[0050] 1) Lithium carbonate is prepared into a slurry with a mass fraction of 10%, and CO is continuously fed under a pressure of 5MPa 2 , the reaction produces LiHCO 3 , the reaction solution was filtered to obtain LiHCO 3 solution; the accuracy of the filtration is: the removal rate of solid particles with a particle size of 1 μm or more is greater than 99.9%;

[0051] 2) The LiHCO obtained in step 1) 3 solution with anhydrous hydrofluoric acid in LiHCO 3 Mix with anhydrous hydrofluoric acid at a molar ratio of 1:5, and react at room temperature for 5 hours to obtain LiF 3HF solution;

[0052] 3) Mix the LiF·3HF solution obtained in step 2) with the boric acid solution with a mass fraction of 20% at a molar ratio of LiF·3HF to boric acid of 1.3:1, and react to obtain a lithium tetrafluoroborate solutio...

Embodiment 3

[0055] The preparation method of lithium tetrafluoroborate of the present embodiment, technological process is as follows figure 1 shown, including the following steps:

[0056] 1) Lithium carbonate is prepared into a slurry with a mass fraction of 0.5%, and CO is continuously fed under a pressure of 2MPa 2 , the reaction produces LiHCO 3 , the reaction solution was filtered to obtain LiHCO 3 solution; the accuracy of the filtration is: the removal rate of solid particles with a particle size of 1 μm or more is greater than 99.9%;

[0057] 2) The LiHCO obtained in step 1) 3 solution with anhydrous hydrofluoric acid in LiHCO 3 Mix with anhydrous hydrofluoric acid at a molar ratio of 1:4.5, and react at room temperature for 0.5h to obtain LiF 3HF solution;

[0058] 3) Mix the LiF·3HF solution obtained in step 2) with the boric acid solution with a mass fraction of 30% at a molar ratio of LiF·3HF to boric acid of 1.5:1, and react to obtain a lithium tetrafluoroborate solutio...

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Abstract

The invention discloses a preparation method for lithium tetrafluoroborate, and the method comprises the following steps: 1) preparing lithium carbonate or lithium hydroxide into slurry, continuously feeding into CO2 for reaction to generate LiHCO3, and filtering a reaction solution to obtain a LiHCO3 solution; 2) mixing the LiHCO3 solution obtained in step 1) with anhydrous hydrofluoric acid for reaction at a room temperature to obtain a LiF.3HF solution; 3) reacting the LiF.3HF solution obtained in step 2) with a boric acid solution to obtain a lithium tetrafluoroborate solution; and 4 ) concentrating the lithium tetrafluoroborate solution obtained in step 3), cooling the concentrated solution to give crystals, filtering and drying the crystals to obtain the lithium tetrafluoroborate. According to the preparation method of the present invention, the product quality is improved, the obtained product meets requirements of lithium-ion batteries either as a novel lithium salt or as a film-forming additive for lithium ion battery electrolyte; the raw materials adopted are readily available and inexpensive, the raw material utilization is high, thus improving productivity, reducing production costs, and being suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of lithium salts for lithium ion batteries, and in particular relates to a preparation method of lithium tetrafluoroborate. Background technique [0002] The molecular formula of lithium tetrafluoroborate is LiBF 4 , with a molecular weight of 93.74, it is mainly used as a new lithium salt and film-forming additive in lithium-ion batteries. 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 electr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0567C01B35/12
CPCY02E60/12Y02E60/10Y02P20/141
Inventor 刘海霞杨华春李世江侯红军薛旭金于贺华刘海庆尚钟声李霞李云峰
Owner DO FLUORIDE CHEM CO LTD
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