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Preparation method of lithium difluorophosphate

A technology of lithium difluorophosphate and lithium hexafluorophosphate, applied in chemical instruments and methods, lithium halides, phosphorus compounds, etc., can solve the problems of heavy metal impurity sources, limitations, and high requirements for reaction conditions, and achieve stable and easy-to-control reactions

Active Publication Date: 2018-11-30
SHENZHEN YANYI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of the above-mentioned methods have high requirements on reaction conditions and it is difficult to get out of the laboratory, and the production process of some raw materials will bring heavy metal impurities and the source is limited.

Method used

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  • Preparation method of lithium difluorophosphate
  • Preparation method of lithium difluorophosphate
  • Preparation method of lithium difluorophosphate

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Embodiment 2

[0023] The preparation method of the lithium difluorophosphate of the embodiment of the present invention comprises the following steps:

[0024] 1) dissolving lithium hexafluorophosphate in an organic solvent to obtain a first solution, and adjusting the temperature of the first solution to 20-30°C;

[0025] 2) Dissolving lithium hydroxide in an organic solvent to obtain a second solution, adjusting the temperature of the second solution to 15-30°C;

[0026] 3) adding the second solution dropwise to the first solution to react to obtain a reactant;

[0027] 4) performing solid-liquid separation on the reactant to obtain a lithium difluorophosphate solution;

[0028] 5) Filtering the lithium difluorophosphate solution, crystallizing to obtain lithium difluorophosphate crystals, and drying to obtain a finished product.

[0029] In order to better understand the above technical solution, the technical solution of the present application will be described in detail below throug...

Embodiment 1

[0043] figure 1It is a process flow chart of the preparation method of lithium difluorophosphate in the embodiment of the present invention; the preparation method of lithium difluorophosphate in the present embodiment comprises the following steps:

[0044] Prepare lithium hexafluorophosphate solution: Take 40Kg of dimethyl carbonate liquid and add it to the reactor, slowly add 10Kg of lithium hexafluorophosphate, stir for 30 minutes after completion, and adjust the solution temperature to 20°C.

[0045] Prepare lithium hydroxide solution: Take 18Kg of dimethyl carbonate liquid and add it to the reactor, slowly add 2.66Kg of lithium hydroxide, stir for 30min after completion, and adjust the solution temperature to 15°C.

[0046] Add the lithium hydroxide solution dropwise to the lithium hexafluorophosphate solution at a rate of 10L / min, stirring continuously during this period. The dropping process takes about 3-4 hours in total. After the dropping is completed, continue to s...

Embodiment 2

[0053] The preparation method of lithium difluorophosphate of the present embodiment comprises the following steps:

[0054] Prepare lithium hexafluorophosphate solution: Take 800Kg of diethyl carbonate and add it to the reactor, slowly add 200Kg of lithium hexafluorophosphate, stir for 30 minutes after completion, and adjust the solution temperature to 20°C.

[0055] Prepare lithium hydroxide solution: Take 360Kg of diethyl carbonate and add it into the reactor, slowly add 53.2Kg of lithium hydroxide, stir for 30 minutes after completion, and adjust the solution temperature to 15°C.

[0056] Add the lithium hydroxide solution dropwise into the lithium hexafluorophosphate solution at a rate of 200 L / min, while stirring continuously. It takes about 3-4 hours in total. After the dropwise addition was completed, the lithium hexafluorophosphate solution was continuously stirred for 2 hours.

[0057] After the reaction is completed, the reactant is centrifuged to obtain a lithium...

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Abstract

The invention provides a preparation method of lithium difluorophosphate, wherein the preparation method comprises the following steps: 1) dissolving lithium hexafluorophosphate in an organic solventto obtain a first solution, and adjusting the temperature of the first solution to 20-30 DEG C; 2) dissolving lithium hydroxide in an organic solvent to obtain a second solution, and adjusting the temperature of the second solution to 15-30 DEG C; 3) dropwise adding the second solution to the first solution, and carrying out a reaction to obtain a reactant; 4) carrying out solid-liquid separationof the reactant to obtain a lithium difluorophosphate solution; and 5) filtering the lithium difluorophosphate solution, then crystallizing to obtain lithium difluorophosphate crystals, and drying toobtain the finished product. The preparation method has the advantages of high conversion rate of raw materials, fewer by-products, stable reaction and easy control, and can realize industrialized production.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a preparation method of lithium difluorophosphate. Background technique [0002] Lithium difluorophosphate, LiPO 2 f 2 , LiDFP, CAS: 24389-25-1, mainly used as lithium ion battery electrolyte electrolyte, is a lithium battery electrolyte salt that has been widely studied in recent years, and the existing commercial lithium battery electrolyte lithium hexafluorophosphate (LiPF 6 ), LiDFP can form a more stable SEI film on the surface of the graphite anode to improve the cycle performance of the battery. It has excellent high and low temperature performance and a wider applicable temperature range, and has attracted increasing attention. Although its excellent performance is widely recognized by the industry, the shortage of market supply and high price have restricted the development of new energy lithium batteries. Many companies have conducted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455C01D15/04
CPCC01B25/455C01D15/04C01P2006/80
Inventor 王静静
Owner SHENZHEN YANYI NEW MATERIALS CO LTD
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