Preparation method of lithium difluorophosphate

A technology of lithium difluorophosphate and lithium carbonate, applied in chemical instruments and methods, lithium halides, phosphorus compounds, etc., can solve problems such as difficult separation and purification, complicated process, and numerous by-products, and achieve good economic value and social Value, easy promotion and application, and simple process

Inactive Publication Date: 2017-06-13
东营石大胜华新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of lithium difluorophosphate usually adopts the following method: for example, using P 2 o 3 f 4 with metal salt or NH 3 Reaction to prepare difluorophosphate, this method has many by-products, it is difficult to achieve separation and purification; difluorophosphate is prepared by the reaction of difluorophosphoric acid and metal chloride, some chlorine ions will remain in the product, affecting battery performance; Using LiPF 6 Lithium difluorophosphate is obtained by mixing with LiCl and then passing water vapor. This method has cheap raw materials, but the reaction is not easy to control, and there are many by-products, which are difficult to purify and are not suitable for large-scale production; LiPF is used 6 Reaction with water to prepare lithium difluorophosphate, the reaction is not easy to control, will produce LiPO 4 F and other impurities that affect battery performance, and are not easy to purify, it is difficult to obtain high-purity products
The difluorophosphate prepared by this method is a solution, which is not very convenient for the promotion and application of difluorophosphate, and there are fluoride salts that are slightly soluble in solvents in the difluorophosphate solution, which may be harmful to the use of it in lithium batteries. Negative impact
[0004] It can be seen from the above that there are various defects in the existing preparation method, or the process is complicated, the cost is high, it is difficult to industrialize production, or the yield is low, there are many by-products, it is not easy to purify, and the prepared difluorophosphate has low purity, which affects the product performance.

Method used

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  • Preparation method of lithium difluorophosphate
  • Preparation method of lithium difluorophosphate
  • Preparation method of lithium difluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1)LiPO 2 f 2 Synthesis of DEC: In a glove box environment, add 600mL of DEC to a 1L PFA container, and at the same time turn on the magnetic stirrer to make the stirring bar in the PFA container start to work, the stirring speed is 250r / min, and then add 1mol of lithium carbonate to make It forms a suspension.

[0054] (2) Turn on the high and low temperature circulation device, heat the PFA container, control the temperature at 62°C, and start adding 0.5mol LiPF slowly 6 , The feeding time is 10 minutes, the reaction temperature is observed during the feeding process, and the temperature is controlled below 68°C. After the feeding is completed, use the high and low temperature circulation device to raise the temperature in the PFA container to 72-73°C, and continue to stir and react for 2 hours. Observe that there is gas overflow, and the liquid is a suspension.

[0055] (3) The resulting suspension is filtered through a pressurized closed filter with a pore size ...

Embodiment 2

[0059] (1)LiPO 2 f 2 Synthesis of DEC: In a glove box environment, add 600mL of DEC to a 1L PFA container, and at the same time turn on the magnetic stirrer to make the stirring bar in the PFA container start to work, the stirring speed is 250r / min, and then add 1.2mol of lithium carbonate, to form a suspension.

[0060] (2) Turn on the high and low temperature circulation device, heat the PFA container, control the temperature at 55-65°C, and start adding 0.5mol LiPF slowly 6 , The feeding time is 10 minutes, the reaction temperature is observed during the feeding process, and the temperature is controlled below 68°C. After the feeding is completed, use the high and low temperature circulation device to raise the temperature in the PFA container to 72-73°C, and continue to stir and react for 2 hours.

[0061] (3) The resulting suspension is filtered through a pressurized closed filter with a pore size of 5 μm. The resulting filtrate is stored in container A for later use, ...

Embodiment 3

[0065] (1)LiPO 2 f 2 Synthesis of DEC: In a glove box environment, add 600mL of DEC to a 1L PFA container, and at the same time turn on the magnetic stirrer to make the stirring bar in the PFA container start to work, the stirring speed is 250r / min, and then add 1.2mol of lithium carbonate, to form a suspension.

[0066] (2) Turn on the high and low temperature circulation device, heat the PFA container, control the temperature at 55-65°C, and start adding 0.5mol LiPF slowly 6 , The feeding time is 10 minutes, the reaction temperature is observed during the feeding process, and the temperature is controlled below 68°C. After the feeding is completed, use a high and low temperature circulation device to raise the temperature in the PFA container to 75°C, and continue to stir and react for 2 hours.

[0067] (3) The resulting suspension is filtered through a pressurized closed filter with a pore size of 5 μm. The resulting filtrate is stored in container A for later use, and t...

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Abstract

A preparation method of lithium difluorophosphate, comprising the steps of: heating LiPF at the first heating temperature 6 Join in the carbonate suspension of carbonate; Reaction under the second heating temperature obtains lithium difluorophosphate (LiPO 2 f 2 ); wherein, the second heating temperature is higher than the first heating temperature. The preparation method provided by the invention has simple process, low cost and high purity of the prepared product.

Description

technical field [0001] The invention belongs to the technical field of power lithium ion battery manufacturing, in particular to a preparation method of lithium difluorophosphate lithium battery additive. Background technique [0002] At present, driven by products such as smartphones, mobile power supplies, and tablet computers, the output value of the domestic lithium battery industry continues to grow. At the same time, the application of lithium-ion batteries is no longer limited to consumer electronics products, and the two new application directions of power and energy storage have brought unlimited market space for lithium batteries. In the next few years, lithium-ion batteries will become an expanding global industry. At the same time, with the expansion of its application field, the demand for further improvement of battery characteristics is also increasing. [0003] Existing studies have shown that adding lithium difluorophosphate to the electrolyte can improve ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455C01D15/04
CPCC01B25/455C01D15/04C01P2002/86C01P2006/80
Inventor 贾风雷陈效飞吕蕾魏林埔马震袁磊谷洪闪季凯强
Owner 东营石大胜华新能源有限公司
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