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A kind of preparation method of crystalline lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and crystal, which is applied in the field of preparation of crystal lithium hexafluorophosphate, can solve the problems of difficulty in ensuring product quality, high production cost, poor quality stability of high-purity lithium fluoride, etc., and achieves low production cost, low three-waste discharge, and product quality. stable effect

Active Publication Date: 2017-03-29
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, the production cost is high, and the quality stability of domestic high-purity lithium fluoride is poor, so it is difficult to guarantee product quality

Method used

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  • A kind of preparation method of crystalline lithium hexafluorophosphate
  • A kind of preparation method of crystalline lithium hexafluorophosphate
  • A kind of preparation method of crystalline lithium hexafluorophosphate

Examples

Experimental program
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Effect test

Embodiment 1

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

[0046] 1) Introduce fluorine gas into 3kg of industrial anhydrous hydrogen fluoride to fully oxidize to obtain a mixed gas; carry out secondary rectification of the mixed gas below 0.1Mpa; the temperature of the tower tank of the first-stage rectification is 20°C, and the outlet temperature is 19°C ;The temperature of the tower kettle of the secondary rectification is 15°C, and the outlet temperature is 12°C; the hydrogen fluoride after rectification is filtered through a primary 0.2μm microporous membrane and a secondary 0.05μm microporous membrane to remove tiny Granular impurities, obtained 2.88kg high-purity anhydrous hydrogen fluoride (purity ≥ 99.999wt%);

[0047] 0.4kg industrial lithium carbonate and water are made into a 3wt% slurry, and then through carbon dioxide carbonization (feeding CO 2 The rea...

Embodiment 2

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

[0056] 1) Feed fluorine gas into 16kg of industrial anhydrous hydrogen fluoride to fully oxidize it to obtain a mixed gas; carry out secondary rectification of the mixed gas below 0.1Mpa; the temperature of the tower tank of the first-stage rectification is 35°C, and the outlet temperature is 25°C ;The temperature of the tower kettle of the secondary rectification is 25°C, and the outlet temperature is 18°C; the hydrogen fluoride after rectification is filtered through a primary 0.2μm microporous membrane and a secondary 0.05μm microporous membrane to remove tiny Granular impurities, produced 14.65kg of high-purity anhydrous hydrogen fluoride (purity ≥ 99.999wt%);

[0057] 0.8kg industrial lithium carbonate and water preparation 3wt% slurry, then through carbon dioxide carbonization (feed into CO 2 The re...

Embodiment 3

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

[0066] 1) Feed fluorine gas into 20kg of industrial anhydrous hydrogen fluoride to fully oxidize to obtain a mixed gas; carry out two-stage rectification of the mixed gas below 0.1Mpa; wherein, the temperature of the tower bottom of the first-stage rectification is 20 ° C ~ 35 ° C, and the outlet The temperature is 19-25°C; the temperature of the bottom of the secondary rectification is 15°C-25°C, the outlet temperature is 12-18°C; Porous membrane filtration to remove tiny particulate impurities in industrial hydrogen fluoride raw materials to produce 18.2kg of high-purity anhydrous hydrogen fluoride (purity ≥ 99.999wt%);

[0067] 0.48kg industrial Lithium Retard and water preparation 5wt% slurry, then through carbon dioxide carbonization (feed into CO 2 The reaction was carried out with an inflow rate of...

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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 in particular relates to a preparation method of crystalline lithium hexafluorophosphate. Background technique [0002] With the increasing energy crisis and environmental pollution, new energy vehicles are becoming more and more popular, and all countries in the world are now raising the development of new energy vehicles to the national strategic level. As a resource-rich country and a big consumer country, my country ranks first in the world in both production and consumption. However, due to the manufacturing bottleneck of new energy vehicles - lithium-ion battery manufacturing technology, subject to monopoly enterprises in 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 composite lithium-ion battery manufacturing core raw material. Its pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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