Preparation method of lithium bis(oxalate)borate

A technology for lithium bis-oxalate borate and oxalic acid is applied in the field of preparation of lithium bis-oxalate borate, which can solve the problems of increased equipment and process costs, increased separation and purification costs, and various types of solvents involved, avoiding easy sublimation, simple reaction steps, and the like. Mild effect of preparation conditions

Active Publication Date: 2018-11-30
武汉海斯普林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that there are many synthesis steps, the cost of equipment and process increases, and there are many types of solvents involved, and the cost of separation and purification increases.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] This embodiment discloses a preparation method of lithium bisoxalate borate, comprising the following steps:

[0027] Add 900 g of acetonitrile, 1 mol of oxalic acid, 0.5 mol of boron trifluoride acetonitrile solution, and 0.5 mol of lithium fluoride into a 2L four-necked flask that has been fully dried and equipped with stirring, dropping funnel, and thermometer, at 15-25°C Stir for 10 minutes and mix evenly; then slowly add 0.5 mol of silicon tetrachloride to the mixed solution through the dropping funnel, control the reaction temperature at 0-30°C, and add the time for 0.5 hours. Gas is generated during the dropping process. After the dropwise addition, continue to stir for 3 hours. At this time, no gas will be generated, and the reaction is over. Distill under reduced pressure at 40-100°C and a vacuum of -0.1-0.1MPa to remove the solvent acetonitrile and hydrogen chloride and tetrafluoride in the solvent. Silica, 96.5 g of white solid product was obtained, the yield...

Embodiment 2

[0029] This embodiment discloses a preparation method of lithium bisoxalate borate, comprising the following steps:

[0030] Add 900 g of acetonitrile, 1 mol of oxalic acid, 0.5 mol of boron trifluoride acetonitrile solution, and 0.5 mol of lithium fluoride into a 2L four-necked flask that has been fully dried and equipped with stirring, dropping funnel, and thermometer, at 15-25°C Stir for 12 minutes, and mix well; then slowly add 0.5 mol of aluminum trichloride to the mixed solution through the dropping funnel, and the aluminum trichloride is dissolved in ether in advance, and the reaction temperature is controlled at 0-30°C, and the dropping time is 0.6 h, gas and milky white precipitates are formed during the dropwise addition. After the dropwise addition, continue to stir for 4 hours. At this time, no more gas is generated, and the reaction is over; the milky white precipitates are separated from the reaction solution by filtration. The reaction liquid was distilled off u...

Embodiment 3

[0032] This embodiment discloses a preparation method of lithium bisoxalate borate, comprising the following steps:

[0033] Add 1000 g of γ-butyrolactone, 1 mol of oxalic acid, 0.5 mol of boron trifluoride ether solution, and 0.5 mol of lithium fluoride into a fully dried four-necked flask with a volume of 2 L, equipped with stirring, dropping funnel, and thermometer. Stir at 15-25°C for 13 minutes, mix well; then slowly drop 0.5mol of silicon tetrachloride into the mixture through the dropping funnel, control the reaction temperature at 0-30°C, and add the time for 0.8h. Gas is generated. After the dropwise addition, continue to stir for 4 hours. At this time, no gas is generated, and the reaction is over; the solvent acetonitrile and the hydrogen chloride and silicon tetrafluoride to obtain 96.4 g of a white solid product with a yield of 99.5%.

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Abstract

The invention brings forward a preparation method of lithium bis(oxalate)borate. The synthesis process is almost performed in a solvent, thereby avoiding the defect that oxalic acid is easy to sublimate under the condition of a solid phase reaction. The preparation condition is mild, the reaction steps are simple, and yield is high. By-products in the whole synthesis process are gaseous or solid and are easy to separate from the product. The solvent can be recovered and recycled, thus being more economic and reducing the pollution to the environment.

Description

technical field [0001] The invention relates to the field of lithium ion battery electrolyte lithium salt synthesis, in particular to a preparation method of lithium bisoxalate borate. Background technique [0002] As an important part of lithium-ion batteries, electrolyte has a very important impact on battery performance. Lithium salts play the role of transporting ions and conducting current in lithium-ion batteries, and should meet high solubility, high conductivity, good chemical stability, wide electrochemical window and high aluminum corrosion Potential and other requirements; in addition, it should also have the advantages of easy preparation, environmental friendliness and low cost. [0003] Currently, the most commercially used electrolyte for Li-ion batteries is LiPF 6 , although the LiPF 6 The electrolyte has high conductivity and wide electrochemical window, but LiPF 6 It has poor thermal stability and is easy to decompose into phosphorus pentafluoride and l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 王文周宜海周永妍郭春花
Owner 武汉海斯普林科技发展有限公司
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