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Preparation method of difluorophosphate

A technology of difluorophosphate and fluoride salt, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low yield and low purity of crude products

Active Publication Date: 2016-07-06
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the required raw material is lithium hexafluorophosphate, lithium hexafluorophosphate is only an intermediate, and it is not the initial cheap raw material
[0026] And adopt the preparation method of the reaction of above-mentioned reaction formula (vii) and (viii) expression, owing to make gas-solid two-phase reaction, productive rate is low, and crude product purity is low

Method used

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

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preparation example Construction

[0053] A kind of preparation method of difluorophosphate, is characterized in that, comprises the following steps:

[0054] A) mixing and stirring the non-aqueous solvent, the fluoride salt and the compound having the structure of formula I to obtain a suspension;

[0055] B) Passing PF into the suspension 5 After the gas is heated and reacted, it is recrystallized to obtain difluorophosphate;

[0056] Formula I;

[0057] In formula I, R 1 ~R 6 are independently selected from H, C1-C50 hydrocarbon groups, C1-C50 substituted hydrocarbon groups or groups with the structure of formula II; or, R 1 ~R 6 Any two or more groups in are combined with each other to form a ring structure;

[0058] Formula II;

[0059] In formula II, R 7 ~R 9 are independently selected from H, C1-C50 hydrocarbon groups, C1-C50 substituted hydrocarbon groups, or R 7 ~R 9 Any one or more groups in are further substituted by a group having the structure of formula II.

[0060] In the present ...

Embodiment 1～22

[0122] Embodiment 1-22 is described in detail, and its specific experimental operation steps are: adding fluoride salt, a compound having the structure of formula I and a non-aqueous solvent into a dry closed container protected by an inert gas, and mixing and stirring to form a suspension , then lower the temperature to a low temperature (10°C), and pass a certain amount of PF at this temperature 5 Then heat up to 60°C to react for 12 hours. After the reaction, cool down to room temperature, filter to remove unreacted fluoride salt and other insoluble impurities, then remove the solvent by rotary evaporation, and then obtain high-purity difluorophosphate by recrystallization , filtered to remove the recrystallization solvent (acetone: anhydrous ether = 1:4, v / v), the obtained crystals were dried under reduced pressure at 80°C for 6 hours, the obtained white powder was weighed, and the yield was calculated. The results are shown in Table 1 for the reaction conditions and resul...

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Abstract

The invention provides a preparation method of difluorophosphate. The preparation method comprises the following steps: (A) mixing a non-aqueous solvent, fluoride salts, and compounds having a structure represented by the formula (I), and stirring to obtain suspension liquid; (B) introducing PF5 gas into the suspension liquid, heating the suspension liquid to carry out reactions, and performing recrystallization to obtain difluorophosphate. In the formula (I), R1 to R6 individually represent H, a C1-C50 hydrocarbyl group, a C1-C50 substituted hydrocarbyl group, or a group having a structure represented by the formula (II); or two or more of R1 to R6 are combined with each other to form a ring structure, in the formula (II), R7 to R9 individually represent H, a C1-C50 hydrocarbyl group, or a C1-C50 substituted hydrocarbyl group, or one or more of R7 to R9 is further substituted by a group having a structure represented by the formula (II).

Description

technical field [0001] The invention belongs to the technical field of difluorophosphate, and in particular relates to a preparation method of difluorophosphate. Background technique [0002] Difluorophosphate is widely used in industry, for example, it can be used as a stabilizer for vinyl chloride polymers (US Patent No. 2846412 specification), a catalyst for reaction lubricating oil (Japanese Patent Application Laid-Open No. 5-255133), a bactericide for toothbrushes ( JP-P 10-503196 Gazette), and wood preservative (JP-P 2002-501034 Gazette), and lithium secondary battery additive (JP-P 08-078053 Gazette, JP-P 11-185804 Bulletin, publication number is the Chinese patent of CN102134065B, and publication number is the Chinese patent of CN102064345B, and publication number is the Chinese patent of CN101507041B) use. [0003] As the preparation method of difluorophosphate, can carry out (JournalofFluorineChemistry (1988), 38 (3), 297.; InorganicChemistry (1967), 6 (10), 1915...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80
Inventor 骆浩夏永高刘兆平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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