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Preparation method of lithium difluorophosphate

A technology of lithium difluorophosphate and ethyl acetate, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as high water content, low purity, and unsuitable conditions for lithium difluorophosphate, and achieve the goal of moisture content The effect of low cost, high purity and easy access to raw materials

Pending Publication Date: 2020-09-29
宁波纳微新能源科技有限公司
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  • Claims
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AI Technical Summary

Problems solved by technology

[0016] However, the lithium difluorophosphate products on the market have low purity and high water content
However, lithium-ion batteries are very strict about moisture control, so that commercially available lithium difluorophosphate does not have the conditions to be used as a battery additive

Method used

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

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preparation example Construction

[0033] The invention provides a preparation method of lithium difluorophosphate, by making RPF 2 o 2 with LiClO 4 The mixed reaction obtains lithium difluorophosphate,

[0034] Wherein, R is K or Na;

[0035] The RPF 2 o 2 with LiClO 4 The molar ratio is 1: (1.8~5).

[0036] According to the present invention, the present invention will RPF 2 o 2 with LiClO 4 The mixed reaction obtains lithium difluorophosphate, wherein, the RPF 2 o 2 with LiClO 4 The molar ratio is preferably 1:(2~3), more preferably 1:(2.5~2.8); the temperature of the reaction is preferably 20~80°C, more preferably 30~70°C, most preferably 40~60°C ℃; the time of the reaction is preferably 6 to 10 hours, more preferably 8 to 9 hours; the present invention has no special requirements for the reaction device, and any device known in the art for the mixed reaction of inorganic substances can be used, as can It is a solid phase reactor; in the mixed reaction of the present invention, the reaction als...

Embodiment 1

[0044] 1) react in a solid-phase reactor, potassium fluoride and phosphorus pentoxide are KF according to the molar ratio of feeding: P 2 o 5 = 2: 1 feed, and adjust the reaction temperature in the kettle to 150 ° C, the reaction time 12h, to obtain RPF 2 o 2 and KPO 3 mixture of and PF 5 gas;

[0045] to RPF 2 o 2 and KPO 3 Ethylene glycol dimethyl ether (DME) is added to the mixture of the mixture, and the product is stirred and extracted, and enriched to obtain KPF-containing 2 o 2 DME solution

[0046] 2) According to KPF 2 o 2 with LiClO 4 The molar ratio is 1: 2 to carry out feeding, the reaction temperature is 40 ℃, the reaction time is 8h, the reaction solution obtained is in N 2 In the atmosphere, distill under reduced pressure at a temperature of 80°C and an air pressure of -0.1 to -0.2MPa for 6 hours, distill off DME and recover it, and dry the obtained crystals under reduced pressure at 80°C for 6 hours to obtain a white powder, which is Lithium diflu...

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Abstract

The invention provides a preparation method of lithium difluorophosphate. According to the method provided by the invention, RPF2O2 and LiClO4 are mixed and react to obtain lithium difluorophosphate,wherein specific raw materials RPF2O2 and LiClO4 are selected, mixed and reacted, and the molar ratio of RPF2O2 to LiClO4 is 1:(1.8-5), so that the obtained lithium difluorophosphate is high in purity, low in moisture content and high in reaction yield, raw materials are easy to obtain, generated byproducts can be recycled, high economic benefits are achieved, and industrial production is easy torealize.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of lithium difluorophosphate. Background technique [0002] Lithium difluorophosphate is an important chemical raw material, such as a stabilizer for vinyl chloride polymers (US Pat. Battery additives (Japanese Patent Application Publication No. 08-078053, Japanese Patent Application Publication No. 11-185804, CN 102134065B, CN102064345B, CN101507041B), wherein, as a lithium-ion battery additive, it has the effect of improving the low-temperature performance and rate performance of the battery . [0003] Regarding the preparation process of difluorophosphate, the patent application number 201010584083 discloses a preparation method of lithium difluorophosphate, a non-aqueous electrolyte, and a non-aqueous electrolyte secondary battery using the non-aqueous electrolyte. The preparation method of lithium difluorophosphate is obtained by reacting hexafluoroph...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80C01P2006/82
Inventor 周明炯庞宝成夏永姚
Owner 宁波纳微新能源科技有限公司
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