Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and lithium fluoride, which is applied in lithium hexafluorophosphate, chemical instruments and methods, lithium compounds, etc., can solve the problems of time-consuming, labor-intensive, easy to agglomerate, time-consuming and labor-intensive, etc., to shorten the crystallization time, shorten the production cycle, Effect of improving crystallization efficiency

Inactive Publication Date: 2018-10-12
MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As an important electrolyte salt of lithium ion battery electrolyte, lithium hexafluorophosphate requires high purity (usually not less than 99.5%), and impurities such as water, alkali metals, heavy metals and other impurities such as PCl 3 and POCl 3 The content must be strictly controlled, otherwise it will lead to increased internal resistance of the battery, rapid decay of battery capacity, shortened cycle life, and even affect the safety of the battery
[0010] (1), the first-level drying in step 4 is standing and drying, and the crystallization time generally takes about 48 hours, and it is easy to agglomerate. After crystallization, the lithium hexafluorophosphate product forms a larger crystal block as a whole, and it is difficult to remove from the crystallization tank. It is difficult to peel off and break in the middle. After the primary drying, the lithium hexafluorophosphate product needs to be crushed according to the particle size requirements, which is time-consuming and laborious. The product particles obtained by the prior art are as follows: figure 1 As shown, its shape is irregular and its surface is rough;
[0011] (2) Only a small amount of reaction raw materials can be processed each time, which cannot meet the production needs of large quantities
[0012] (3) It needs to be dried twice, which takes a long time and consumes time and energy.

Method used

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

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[0037] (1) Preparation of high-purity raw materials: Anhydrous hydrogen fluoride is sent to a distillation tower for refining, the distillation temperature is controlled at 20-25°C, and the hydrogen fluoride gas evaporated is condensed by a condenser to produce hydrogen fluoride liquid with a purity of more than 99.99wt%. ;

[0038] (2) Preparation and purification of phosphorus pentafluoride: add hydrogen fluoride liquid into the reaction kettle that has added phosphorus pentachloride, wherein the hydrogen fluoride liquid is excessive relative to phosphorus pentachloride, and control the temperature at 178 ° C ~ Between 182°C and the pressure controlled between 0.13MPa and 0.17MPa, hydrogen fluoride reacts with phosphorus pentachloride to produce a mixed gas of phosphorus pentafluoride and hydrogen chloride. After the reaction is completed, the excess hydrogen fluoride liquid is absorbed by the condensed water of the condensing device. By-product hydrofluoric acid;

[0039] ...

Embodiment 1

[0052] A method for rapidly preparing lithium hexafluorophosphate, specifically comprising the following steps:

[0053] (1) Preparation of high-purity raw materials: Anhydrous hydrogen fluoride is sent to a distillation tower for refining, the distillation temperature is controlled at 20-25°C, and the hydrogen fluoride gas evaporated is condensed by a condenser to produce hydrogen fluoride liquid with a purity of more than 99.99wt%. ;

[0054] (2) Preparation and purification of phosphorus pentafluoride: add hydrogen fluoride liquid into the reaction kettle that has added phosphorus pentachloride, wherein the hydrogen fluoride liquid is excessive relative to phosphorus pentachloride, and control the temperature at 178 ° C ~ Between 182°C and the pressure controlled between 0.13MPa and 0.17MPa, hydrogen fluoride reacts with phosphorus pentachloride to produce a mixed gas of phosphorus pentafluoride and hydrogen chloride. After the reaction is completed, the excess hydrogen flu...

Embodiment 2

[0059] A method for preparing lithium hexafluorophosphate with special specifications, specifically comprising the following steps:

[0060] (1) Preparation of high-purity raw materials: Anhydrous hydrogen fluoride is sent to a distillation tower for refining, the distillation temperature is controlled at 20-25°C, and the hydrogen fluoride gas evaporated is condensed by a condenser to produce hydrogen fluoride liquid with a purity of more than 99.99wt%. ;

[0061] (2) Preparation and purification of phosphorus pentafluoride: add hydrogen fluoride liquid into the reaction kettle that has added phosphorus pentachloride, wherein the hydrogen fluoride liquid is excessive relative to phosphorus pentachloride, and control the temperature at 178 ° C ~ Between 182°C and the pressure controlled between 0.13MPa and 0.17MPa, hydrogen fluoride reacts with phosphorus pentachloride to produce a mixed gas of phosphorus pentafluoride and hydrogen chloride. After the reaction is completed, the...

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Abstract

The invention discloses a preparation method of lithium hexafluorophosphate. The preparation method comprises the following steps: (1) introducing phosphorus pentafluoride gas into a reaction kettle filled with lithium fluoride and hydrogen fluoride liquid and carrying out reaction for 1 to 2 hours to obtain a lithium hexafluorophosphate solution; (2) realizing partial crystallisation under a stirring condition; (3) carrying out drying. The preparation method of lithium hexafluorophosphate disclosed by the invention has the advantages that the operation is convenient, the lithium hexafluorophosphate which is obtained by carrying out partial crystallisation is directly formed into uniform particles, so that the steps of multiple drying and pulverization are eliminated, and the partial crystallisation time is shortened.

Description

technical field [0001] The present application relates to the technical field of lithium ion batteries, in particular to a method for preparing lithium hexafluorophosphate. Background technique [0002] Lithium-ion batteries have outstanding advantages such as high working voltage, high energy density (light weight), low self-discharge rate, no memory effect, long cycle life and no pollution. In recent years, it has quickly occupied many fields with its incomparable advantages over other batteries, and is widely used in well-known mobile phones, notebook computers, small cameras, electric vehicles and other products. With the industrialization of electric vehicles, the amount of lithium-ion batteries is bound to increase. The application shows that lithium-ion battery is an ideal small green power source. [0003] Lithium hexafluorophosphate is an important electrolyte salt of lithium-ion battery electrolyte, which requires high purity (usually not less than 99.5%), and im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00
CPCC01D15/005C01P2004/02C01P2004/60C01P2004/61C01P2006/80
Inventor 堀尾博英
Owner MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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