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Preparation method of crystal lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and crystals, which is applied in the field of preparation of crystal lithium hexafluorophosphate, can solve the problems of difficulty in guaranteeing product quality, poor quality stability of high-purity lithium fluoride, and high production costs, and achieve low production costs, stable product quality, and three-waste discharge little effect

Active Publication Date: 2015-11-11
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the advantages of high reaction rate and good production continuity; because the raw material directly uses high-purity lithium fluoride,

Method used

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  • Preparation method of crystal lithium hexafluorophosphate
  • Preparation method of crystal lithium hexafluorophosphate
  • Preparation method of crystal lithium hexafluorophosphate

Examples

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Example Embodiment

[0044] Example 1

[0045] The preparation method of crystalline lithium hexafluorophosphate in this embodiment, the process flow is as follows figure 1 As shown, including the following steps:

[0046] 1) Pour fluorine gas into 3kg of industrial anhydrous hydrogen fluoride to fully oxidize to obtain a mixed gas; the mixed gas is subjected to two-stage rectification below 0.1Mpa; the temperature of the tower kettle of the first-stage rectification is 20℃, and the outlet temperature is 19℃ ; The temperature of the tower kettle of the secondary rectification is 15℃, and the outlet temperature is 12℃; the hydrogen fluoride after rectification is filtered through a 0.2μm microporous membrane and a secondary 0.05μm microporous membrane to remove the tiny amounts of industrial hydrogen fluoride raw materials Particulate impurities, 2.88kg of high-purity anhydrous hydrogen fluoride (purity ≥99.999wt%);

[0047] Mix 0.4kg of industrial lithium carbonate and water into a 3wt% slurry, and the...

Example Embodiment

[0054] Example 2

[0055] The preparation method of crystalline lithium hexafluorophosphate in this embodiment has the same process flow as that of embodiment 1, including the following steps:

[0056] 1) Pass fluorine gas into 16kg of industrial anhydrous hydrogen fluoride to fully oxidize to obtain a mixed gas; the mixed gas is subjected to two-stage rectification below 0.1Mpa; the temperature of the tower kettle of the first-stage rectification is 35℃ and the outlet temperature is 25℃ ; The temperature of the tower kettle of the secondary rectification is 25℃, and the outlet temperature is 18℃; the hydrogen fluoride after rectification is filtered through the first-level 0.2μm microporous membrane and the second-level 0.05μm microporous membrane to remove the tiny amounts of industrial hydrogen fluoride raw materials Granular impurities, 14.65kg of high-purity anhydrous hydrogen fluoride (purity ≥99.999wt%) is prepared;

[0057] A 3wt% slurry was prepared by 0.8kg industrial lith...

Example Embodiment

[0064] Example 3

[0065] The preparation method of crystalline lithium hexafluorophosphate in this embodiment has the same process flow as that of embodiment 1, including the following steps:

[0066] 1) Pass fluorine gas into 20kg of industrial anhydrous hydrogen fluoride to fully oxidize to obtain a mixed gas; carry out the two-stage rectification of the mixed gas below 0.1Mpa; among them, the temperature of the tower kettle of the first-stage rectification is 20℃~35℃, and the outlet The temperature is 19~25℃; the temperature of the second-stage distillation column is 15℃~25℃, and the outlet temperature is 12~18℃; the hydrogen fluoride after rectification is passed through the first-stage 0.2μm microporous membrane and the second-stage 0.05μm microporous membrane. Porous membrane filtration to remove tiny particulate impurities in industrial hydrogen fluoride raw materials to obtain 18.2kg of high-purity anhydrous hydrogen fluoride (purity ≥99.999wt%);

[0067] Prepare a 5wt% slu...

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Abstract

The invention discloses a preparation method of crystal lithium hexafluorophosphate. The method comprises: 1) preparing industrial lithium carbonate and water into a slurry with concentration of 2%-5%; reacting with CO2, conducting resin exchange and gradient crystallization to obtain a high purity lithium hydrogencarbonate solution; reacting the high purity lithium hydrogencarbonate with high purity hydrogen fluoride, filtering, washing and drying to obtain high purity lithium fluoride; 2) reacting high purity hydrogen fluoride with high purity lithium fluoride to prepare a hydrogen fluoride lithium solution; 3) reacting high purity hydrogen fluoride with phosphorus pentachloride to obtain a mixture of phosphorus pentafluoride, hydrogen fluoride and hydrogen chloride; introducing the mixture as stream stirred bubble stream into a hydrogen fluoride lithium solution to obtain a lithium hexafluorophosphate solution; and 4) crystallizing, filtering and drying lithium hexafluorophosphate solution to obtain the crystal lithium hexafluorophosphate. The method uses conventional raw materials for industrial production, ensures product quality and stability, and has the advantages of high utilization of raw materials, low production cost, and good environmental performance.

Description

Technical field [0001] The invention belongs to the technical field of lithium ion batteries, and specifically relates to a method for preparing crystal lithium hexafluorophosphate. Background technique [0002] With the ever-increasing energy crisis and environmental pollution, new energy vehicles are increasingly being pursued, and countries in the world are now raising the development of new energy vehicles to a national strategic level. As a major resource and consumer country, my country ranks first in the world in terms of production and consumption. However, due to the manufacturing bottleneck of new energy vehicles-lithium-ion battery manufacturing technology, subject to the monopoly of the United States, Japan, and South Korea, the development of my country's new energy industry has basically stagnated. [0003] Lithium hexafluorophosphate is an irreplaceable and only recombinable core raw material for manufacturing lithium-ion batteries. Its product form, purity, trace i...

Claims

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Application Information

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IPC IPC(8): C01B25/10
Inventor 侯红军杨华春李云峰薛旭金于贺华闫春生刘海霞薛峰峰贾雪枫贾棉
Owner DO FLUORIDE CHEM CO LTD
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