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Synthetic method of hexafluorophosphate

A technology of hexafluorophosphate and synthesis method, applied in the field of synthesis of hexafluorophosphate, can solve the problems of difficulty in purification, storage, transportation and use of phosphorus pentafluoride, difficulty in large-scale industrial application, and high requirements on structure and material, To achieve the effect of rationalizing the separation sequence, simplifying the separation process, and improving the solvent recovery rate

Active Publication Date: 2022-03-04
ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0025] The elemental phosphorus method is to place elemental phosphorus (red phosphorus, yellow phosphorus, white phosphorus, etc.) in a special reactor, introduce fluorine gas, and obtain phosphorus pentafluoride through gas-solid phase reaction. The purity of phosphorus is high, and high-purity phosphorus pentafluoride can be obtained without complicated purification operations. The disadvantage is that fluorine gas needs to be prepared through an additional electrolytic fluorine production process, and the reaction process is a gas-solid phase reaction. The reactor structure It has high requirements on materials and harsh reaction conditions, so it is difficult for large-scale industrial application
[0028] (2) Phosphorus pentafluoride obtained by the reaction of phosphorus pentachloride and hydrogen fluoride is a gas with a low boiling point of only -84.6°C. It is difficult to liquefy, making it difficult to purify, store, transport and use phosphorus pentafluoride, resulting in synthesis Costs rise, production efficiency falls
[0029] (3) The raw materials used in the synthesis of hexafluorophosphate are highly toxic and dangerous, and there are major safety risks in the reaction process. At present, hexafluorophosphate is generally synthesized by batch reaction, which poses serious production safety hazards.

Method used

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  • Synthetic method of hexafluorophosphate
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  • Synthetic method of hexafluorophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0106] As a continuous reactor with a microreactor, a phosphorus, lithium chloride, hydrogen fluoride is a raw material, and a lithium hexafluorophosphate is synthesized by toluene is an inert organic solvent. figure 1 The synthesis process is as follows:

[0107] (1) The quantitative toluene is added to the formulating kettle of the phosphloride toluene solution, and the quantitative pentachloride solid is added under nitrogen protection, stir up to 60 to 65 ° C, after all dissolution, cool down to 20 ~ 25 ° C gave a high mass concentration of 25% pentachloride solution, and preservation was stored under nitrogen protection. The phosphonated phosphorne solution is divided into AB kettle, and the two are used.

[0108] (2), the quantitative water-free hydrogen fluoride liquid is added to the fluorinated hydrogen fluoride solution formulation, nitrogen protection, temperature control - 10 ~ -5 ° C, slowly add quantitative lithium chloride solid, stirred and dissolved, resulting in ...

Embodiment 2

[0117] As a continuous reactor with a microreactor, phosphorus phosphorus, sodium fluoride, hydrogen fluoride is a raw material, and the sodium hexafluorophosphate is synthesized by chlorofluorine. figure 1 The synthesis process is as follows:

[0118] (1), the quantitative chlorobenzene is added to the formulation of the phosphrachloride chloride solution. Under nitrogen protection, the quantitative pentachloride solid is added, and the stirring is warmed to 50 to 55 ° C, and after all of the solid is all dissolved, it will cool down. 10 ~ 15 ° C, resulting in a hydrochloride chloride solution having a mass concentration of 20%, and is preserved under nitrogen protection. The phosphrachloride chloride chlorobenzene solution is divided into AB kettle, two kette crossings.

[0119] (2), the quantitative water-free hydrogen fluoride liquid is added to the fluorinated sodium fluoride solution formulation, nitrogen protection, temperature control 10 ~ 15 ° C, slowly add quantitative f...

Embodiment 3

[0128] As a continuous reactor with a microreactor, a phosphorus, potassium chloride, hydrogen fluoride is a raw material, and the potassium organic solvent, the synthesis of hexafluoro phosphate, and the process flow is combined. figure 1 The synthesis process is as follows:

[0129] (1), the quantitative chloroform is added to the formulating kettle with a pentachloride chloride. Under nitrogen protection, a quantitative pentachloride solid is added, and the stirring is warmed to 40 to 45 ° C, and after all of the solid is dissolved, it will cool down to 20 ~ 25 ° C, the mass concentration of 30% p-chloride chloride solution is preserved under nitrogen protection. Penthalchloride chloroform solution is divided into AB kettle, two altitude cross-use.

[0130] (2), the quantification of water-free hydrogen fluoride liquid is added to the fluorinated potassium hydrogen fluoride solution, nitrogen protection, temperature control - 15 ~ -10 ° C, slowly add quantitative sostatis solid...

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Abstract

The invention discloses a synthesis method of hexafluorophosphate, which belongs to the technical field of chemical synthesis, and is characterized by comprising the following steps: dissolving phosphorus pentahalide in an inert solvent to obtain a phosphorus pentahalide inert solvent solution, dissolving alkali metal halide salt in anhydrous hydrogen fluoride to obtain an alkali metal villiaumite hydrogen fluoride solution, the method comprises the following steps: inputting hexafluorophosphate, hydrogen fluoride, an inert solvent and hydrogen halide into a reactor in proportion for reaction to obtain a mixture consisting of the hexafluorophosphate, the hydrogen fluoride, the inert solvent and the hydrogen halide, firstly removing hydrogen halide gas through gas-liquid separation, then recovering the hydrogen fluoride through heating evaporation, finally recovering the inert solvent through solid-liquid separation, and drying a solid to obtain the hexafluorophosphate, the synthesis method disclosed by the invention has the advantages of simplicity in operation, good safety, high reaction yield, excellent product quality, capability of realizing continuous production and the like.

Description

Technical field [0001] The present invention belongs to the technical field of chemical synthesis, in particular, it relates to a method for the synthesis of hexafluorophosphate. Background technique [0002] Global warming is a major issue facing humanity in the 21st century, not only human development, and even affect the survival of humanity. Solve the global warming problem, the first thing is based on solar, wind and other new clean energy alternative to traditional high pollution and high emissions of fossil fuels and reduce carbon dioxide and other greenhouse gases, therefore, the development of green, environmental protection has become a secondary battery to solve the problem The essential. After half a century of research and industrial development, the current lithium-ion batteries have large-scale production, widely used in energy storage, power and so on, the sodium ion battery into the fast lane, and gradually into the application stage, while potassium ions battery...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01D15/005C01P2006/80Y02E60/10C01B25/455C01B25/10
Inventor 袁其亮陈建陈海峰徐鹏飞竺坚飞蒋栋栋陈寅镐王超
Owner ZHEJIANG ZHONGXIN FLUORIDE MATERIALS CO LTD
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