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Method for preparing lithium difluorophosphate

A technology of lithium difluorophosphate and lithium hexafluorophosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of difficult control of the reaction process, unfavorable production, numerous by-products, etc., and achieve fast and efficient purity and yield. Product The effect of excellent properties and great industrial value

Inactive Publication Date: 2017-11-24
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, lithium difluorophosphate is prepared by reacting lithium hexafluorophosphate with water. This method is not easy to control the reaction process, and there are many by-products, which is very unfavorable to production.
In addition, CN101847753A describes a method for preparing lithium difluorophosphate in an aprotic solvent by using lithium hexafluorophosphate and lithium carbonate, but only a non-aqueous solution of lithium difluorophosphate can be obtained by this method, and high-purity lithium difluorophosphate cannot be obtained , which is very unfavorable for the promotion of lithium difluorophosphate, and there are more or less organic impurities and lithium fluoride in the salt solution, and these impurities may have an adverse effect on the performance of the battery
[0004] In summary, the existing preparation method of lithium difluorophosphate has complex process and many by-products, which is very unfavorable for the industrialization and promotion of lithium difluorophosphate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) In an inert gas environment, add 600ml of dimethyl carbonate to a 1L glass reaction bottle, then add 2mol of lithium carbonate and 1mol of lithium hexafluorophosphate, and use mechanical stirring to stir the reaction materials evenly.

[0024] (2) Add the evenly stirred reaction materials into a 1L hydrothermal reaction kettle and seal it well.

[0025] (3) Put the hydrothermal reaction kettle in step (2) in an oven at 160°C for high temperature and high pressure solvothermal reaction.

[0026] (4) After reacting for 5 hours, the reaction was terminated, and the reaction solution was rotary evaporated at 75° C. to remove dimethyl carbonate to obtain a solid crude product of lithium difluorophosphate.

[0027] (5) Wash the solid crude product obtained in step (5) with 200ml of acetone, stir for two hours under mechanical stirring, and filter to remove the solid residue.

[0028] (6) The filtrate obtained in step (6) was dried to finally obtain 98.5 g of lithium difl...

Embodiment 2

[0030] (1) In an inert gas environment, add 600ml of dimethyl carbonate to a 1L glass reaction bottle, then add 2mol of lithium carbonate and 1mol of lithium hexafluorophosphate, and use mechanical stirring to stir the reaction materials evenly.

[0031] (2) Add the evenly stirred reaction materials into a 1L hydrothermal reaction kettle and seal it well.

[0032] (3) Put the hydrothermal reaction kettle in step (2) in an oven at 160°C for high temperature and high pressure solvothermal reaction.

[0033] (4) After reacting for 5 hours, the reaction was terminated, and the reaction solution was rotary evaporated at 75° C. to remove dimethyl carbonate to obtain a solid crude product of lithium difluorophosphate.

[0034] (5) Wash the solid crude product obtained in step (4) with 200ml of tetrahydrofuran, stir for two hours under the condition of mechanical stirring, and filter to remove the solid residue.

[0035] (6) The filtrate obtained in step (5) was dried to finally obta...

Embodiment 3

[0037] (1) In an inert gas environment, add 600ml of acetonitrile to a 1L glass reaction bottle, then add 2.2mol of lithium carbonate and 1mol of lithium hexafluorophosphate, and use mechanical stirring to stir the reaction materials evenly.

[0038] (2) Add the evenly stirred reaction materials into a 1L hydrothermal reaction kettle and seal it well.

[0039] (3) Put the hydrothermal reaction kettle in step (2) in an oven at 130°C to perform a high temperature and high pressure solvothermal reaction.

[0040] (4) The reaction was terminated after 6 hours of reaction, and the reaction liquid was rotary evaporated at 60° C. to remove acetonitrile to obtain a solid crude product of lithium difluorophosphate.

[0041] (5) Wash the crude solid product obtained in step (4) with 200ml of acetone, stir for two hours under mechanical stirring, and filter to remove the solid residue.

[0042] (6) The filtrate obtained in step (5) was dried to finally obtain 95.4 g of lithium difluorop...

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PUM

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Abstract

The invention discloses a method for preparing lithium difluorophosphate. The method comprises the following steps: dissolving lithium carbonate and lithium hexafluorophosphate in an aprotic solvent, uniformly mixing above substances and the solvent, filling a closed container with the obtained solution, carrying out a high-temperature and high-pressure reaction for a certain time, carrying out rotary evaporation to remove the solvent, and purifying the obtained reaction product through a washing process to obtain highly-pure lithium difluorophosphate. The method for preparing the lithium difluorophosphate through adopting a solvothermal technology has the advantages of realization of high-temperature rapid preparation of the lithium difluorophosphate, small dosage of the solvent, high easiness in purification, and very high purity of the target product.

Description

Technical field: [0001] The invention relates to a preparation technology of lithium difluorophosphate. Background technique: [0002] As a new type of mobile portable power supply, lithium-ion batteries have higher specific capacity and discharge voltage than traditional lead-acid batteries and alkaline batteries, and have less environmental pollution. At present, lithium-ion batteries are mainly used as portable mobile power sources, mobile phone batteries, and are widely used in electric vehicles, automobiles, etc. as power batteries. Due to the strong support of national policies and the accumulation of lithium-ion battery technology in recent years, the lithium-ion battery industry has achieved tremendous development, and will continue to develop due to policy encouragement and technological progress. However, there are still many defects in lithium-ion batteries at present. In the development of lithium salts, traditional lithium hexafluorophosphate cannot meet the us...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80
Inventor 孟跃中张黎明王拴紧肖敏陆景华罗自谦韩东梅
Owner SUN YAT SEN UNIV
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