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A kind of 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 purity and low yield of crude products

Active Publication Date: 2018-02-23
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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  • A kind of preparation method of difluorophosphate
  • A kind of preparation method of difluorophosphate
  • A kind of 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) non-aqueous solvent, fluoride salt and compound with formula I structure are mixed and stirred to obtain suspension;

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

[0056] formula I;

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

[0058] formula II;

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

[0060] In the present invention...

Embodiment 1～22

[0122] Embodiments 1-22 are specifically described, and the specific experimental operation steps are as follows: adding the fluoride salt, the compound having the structure of formula I and a non-aqueous solvent into a dry inert gas-protected closed container, and mixing and stirring to form a suspension , and then cooled to a low temperature (10°C), and a certain amount of PF was introduced at this temperature 5 Then, the temperature was raised to 60 °C for 12 hours. After the reaction was completed, the temperature was lowered to room temperature. The unreacted fluoride salt and other insoluble impurities were removed by filtration, and then the solvent was removed by rotary evaporation, and high-purity difluorophosphate was obtained 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 c...

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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, in particular to a preparation method of difluorophosphate. Background technique [0002] Difluorophosphates are widely used in industry, such as stabilizers for vinyl chloride polymers (US Patent No. 2,846,412), catalysts for reaction lubricating oils (Japanese Patent Laid-Open No. 5-255133), and bactericides for toothbrushes ( Japanese Patent Publication No. Hei 10-503196), wood preservatives (Japanese Patent Publication No. Hei 2002-501034), and additives for lithium secondary batteries (Japanese Patent Publication No. Hei 08-078053, Japanese Patent Publication No. Hei 11-185804 Gazette, Chinese Patent Publication No. CN102134065B, Chinese Patent Publication No. CN102064345B, Chinese Patent Publication No. CN101507041B) are used. [0003] The preparation method of difluorophosphate can be carried out according to the reactions represented by the following reaction formulae (i) and (...

Claims

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Application Information

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Patent Type & Authority Patents(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