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Preparation method of lithium phosphate difluoride

A technology of lithium difluorophosphate and lithium difluorotetrahalophosphate, which is applied in the field of preparation of lithium difluorophosphate, can solve the problems of difficulty in obtaining and separating raw materials, numerous by-products, and unsuitability for large-scale production.

Active Publication Date: 2018-08-17
如鲲(山东)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation methods of difluorophosphate mentioned in the existing literature or patents generally have problems such as difficult acquisition of raw materials or difficulty in separation, and it is difficult to meet the requirements of large-scale industrial production
For example: Japanese Patent Laid-Open 2014-62036 uses LiPF 6 Lithium difluorophosphate is obtained by mixing with LiCl and then passing water vapor. Although this method has cheap raw materials, 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.

Method used

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preparation example Construction

[0029] In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing lithium difluorophosphate, at least including the following steps:

[0030] (1) Lithium halide LiX, phosphorus pentahalide PX 5 and lithium hexafluorophosphate LiPF 6 The reaction yields lithium difluorotetrahalophosphate LiPF 2 x 4 ;

[0031] (2) Lithium difluorotetrahalophosphate LiPF 2 x 4 Reaction with substances containing active oxygen to obtain lithium difluorophosphate LiPO 2 f 2 .

[0032]The "halogen" in lithium halide, phosphorus pentahalide and lithium difluorotetrahalophosphate in the present invention refers to halogen, specifically refers to the elements of group VIIA of the periodic table of elements, including fluorine (F), chlorine (Cl) , Bromine (Br), Iodine (I), Astatine (At), Ishida (Ts).

[0033] As a preferred technical solution of the present invention, the lithium halide is selected from any one of lithium fluoride, li...

Embodiment 1

[0083] Embodiment 1 provides a kind of preparation method of lithium difluorophosphate, at least comprises the following steps:

[0084] In a dry reactor, under nitrogen protection, 2.6g (0.1mol) LiF and 43g (0.1mol) phosphorus pentabromide, 15.2g (0.1mol) lithium hexafluorophosphate were added to 300mL dry diethyl carbonate at room temperature, Stir, slowly raise the temperature of the reactor to 45-55°C, react for 25 hours, then lower the temperature of the reactor to room temperature, and filter to obtain 45.3g LiPF 2 Br 4 .

[0085] In another dry reactor, under nitrogen protection, 36g (0.1mol) LiPF 2 Br 4 Add it to 200mL of dry ethyl methyl carbonate, slowly add 18g (0.3mol) isopropanol dropwise under stirring, and control the temperature of the reaction kettle to be less than or equal to 50°C. After the dropwise addition, keep the reaction at 45°C for 5 hours, then evaporate the solvent to dryness under reduced pressure, redissolve the obtained solid in freshly drie...

Embodiment 2

[0087] Embodiment 2 provides a kind of preparation method of lithium difluorophosphate, at least comprises the following steps:

[0088] In a dry reaction kettle, under nitrogen protection, 8.7g (0.1mol) LiBr and 43g (0.1mol) phosphorus pentabromide, 15.2g (0.1mol) lithium hexafluorophosphate were added to 300mL dry diethyl carbonate at room temperature, Stir, slowly raise the temperature of the reactor to 45-55°C, react for 25 hours, then lower the temperature of the reactor to room temperature, and filter to obtain 46.8g LiPF 2 Br 4 .

[0089] In another dry reactor, under nitrogen protection, 36g (0.1mol) LiPF 2 Br 4 Add it to 200mL of dry ethyl methyl carbonate, slowly add 31.2g (0.4mol) dimethyl sulfoxide dropwise under stirring, and control the temperature of the reaction kettle to be less than or equal to 50°C. After the dropwise addition, keep the reaction at 45°C for 5 hours, then evaporate the solvent to dryness under reduced pressure, redissolve the obtained sol...

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Abstract

The invention relates to a preparation method of lithium phosphate difluoride, in particular to a method for producing industrially and economically-superior lithium phosphate difluoride for producingnonaqueous electrolyte batteries. The preparation method of the lithium phosphate difluoride at least comprises the following steps: (1) performing a reaction on lithium halide, phosphorus pentahalide and lithium hexafluorophosphate to obtain tetra-halogen lithium phosphate difluoride; (2) making tetra-halogen lithium phosphate difluoride react with a substance containing active oxygen to obtainlithium phosphate difluoride.

Description

technical field [0001] The present invention relates to a preparation method of lithium difluorophosphate, more particularly to an industrially and economically excellent method for producing lithium difluorophosphate for non-aqueous electrolyte batteries. Background technique [0002] In recent years, driven by small storage system products with high energy density applications such as smartphones, mobile power supplies, and tablet computers, the output value of the domestic lithium battery industry has continued to grow; at the same time, the application of lithium-ion batteries is no longer limited to consumer electronics products , The two new application directions of power and energy storage have brought unlimited markets for lithium batteries. The space is mainly focused on large storage systems suitable for power applications including auxiliary power supplies and electrical energy storage bodies for electric vehicles, hybrid vehicles and fuel cell vehicles. Driven ...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80
Inventor 张连成刘俊
Owner 如鲲(山东)新材料科技有限公司
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