Preparation method of high-purity lithium hexafluorophosphate

A lithium hexafluorophosphate, high-purity technology, applied in the directions of lithium hexafluorophosphate, chemical instruments and methods, phosphorus compounds, etc., to achieve the effect of good purification effect, less waste discharge, and safe production process

Pending Publication Date: 2022-05-27
江西吉翔医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the actual production process also involves the purification of lithium hexafluorophosphate

Method used

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  • Preparation method of high-purity lithium hexafluorophosphate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] like figure 1 As shown, a preparation method of high-purity lithium hexafluorophosphate, comprising the following steps:

[0035] 1) reacting phosphorus pentachloride with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; the phosphorus pentachloride is prepared by reacting phosphorus trichloride and chlorine gas; the preparation of the phosphorus pentachloride The raw material phosphorus trichloride is prepared by the reaction of yellow phosphorus and chlorine;

[0036] 2) LiF is dissolved in the anhydrous HF solvent, and then pass into step 1) gained phosphorus pentafluoride, phosphorus pentafluoride and LiF react to obtain the anhydrous HF solution of lithium hexafluorophosphate, the mol ratio of phosphorus pentafluoride and LiF About 1.1~1.2:1;

[0037] 3) distilling the anhydrous HF solution of the obtained lithium hexafluorophosphate to remove hydrofluoric acid, and the distillation temperature is 30~50 ℃ to obtain solid l...

Embodiment 2

[0047] A preparation method of high-purity lithium hexafluorophosphate, comprising the following steps:

[0048] 1) reacting phosphorus pentachloride with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; the phosphorus pentachloride is prepared by reacting phosphorus trichloride and chlorine gas; the preparation of the phosphorus pentachloride The raw material phosphorus trichloride is prepared by the reaction of yellow phosphorus and chlorine;

[0049] 2) LiF is dissolved in the anhydrous HF solvent, and then pass into step 1) gained phosphorus pentafluoride, phosphorus pentafluoride and LiF react to obtain the anhydrous HF solution of lithium hexafluorophosphate, the mol ratio of phosphorus pentafluoride and LiF About 1.1~1.2:1;

[0050] 3) distilling the anhydrous HF solution of the obtained lithium hexafluorophosphate to remove hydrofluoric acid, and the distillation temperature is 30~50 ℃ to obtain solid lithium hexafluorophosphat...

Embodiment 3

[0056] A preparation method of high-purity lithium hexafluorophosphate, comprising the following steps:

[0057] 1) reacting phosphorus pentachloride with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; the phosphorus pentachloride is prepared by reacting phosphorus trichloride and chlorine gas; the preparation of the phosphorus pentachloride The raw material phosphorus trichloride is prepared by the reaction of yellow phosphorus and chlorine;

[0058] 2) LiF is dissolved in the anhydrous HF solvent, and then pass into step 1) gained phosphorus pentafluoride, phosphorus pentafluoride and LiF react to obtain the anhydrous HF solution of lithium hexafluorophosphate, the mol ratio of phosphorus pentafluoride and LiF About 1.1~1.2:1;

[0059] 3) distilling the anhydrous HF solution of the obtained lithium hexafluorophosphate to remove hydrofluoric acid, and the distillation temperature is 30~50 ℃ to obtain solid lithium hexafluorophosphat...

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Abstract

The invention relates to the technical field of lithium ion batteries, and discloses a preparation method of high-purity lithium hexafluorophosphate, which comprises the following steps: 1) reacting phosphorus pentachloride with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; 2) dissolving LiF in an anhydrous HF solvent, introducing the obtained phosphorus pentafluoride into the anhydrous HF solvent, and reacting to obtain an anhydrous HF solution of lithium hexafluorophosphate; 3) distilling the obtained anhydrous HF solution of lithium hexafluorophosphate to remove hydrofluoric acid to obtain solid lithium hexafluorophosphate; and 4) recrystallizing the lithium hexafluorophosphate solid by adopting supercritical carbon dioxide or liquid carbon dioxide as a solvent to obtain purified lithium hexafluorophosphate. Carbon dioxide is adopted for recrystallization, so that the method is green, environment-friendly, low in cost, safe in production process and good in purification effect; the reaction gas in the step 2) is collected, separated and reused, the whole-process clean production process of the lithium hexafluorophosphate is formed, the whole production process is green and environmentally friendly, and waste emission is little.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of high-purity lithium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate is the most important component (electrolyte) in lithium-ion battery electrolyte, with good ion migration number and dissociation constant, high electrical conductivity and electrochemical stability, as well as good anti-oxidation performance and aluminum foil passivation ability , and can be matched with various positive and negative materials. [0003] Using anhydrous hydrogen fluoride as a solvent to produce lithium hexafluorophosphate, the reaction is easy to carry out, and it is easy to realize industrialization, which is a relatively mature production process route of lithium hexafluorophosphate. The raw material phosphorus pentafluoride is a colorless gas, which is easy to be hydrolyzed and has strong moisture absorption. Due to the high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01D15/005C01P2006/80Y02E60/13
Inventor 王农跃茅晓辉张明闻国强朱九皋王猛章冬霞
Owner 江西吉翔医药化工有限公司
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