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Method for purifying lithium difluoroborate and lithium tetrafluoroborate mixed lithium salt and application thereof

A technology of lithium difluorooxalate borate and lithium tetrafluoroborate, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problem of high equipment and technical requirements and separation problems such as high difficulty and low purity of mixed salt

Pending Publication Date: 2021-04-09
SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Since lithium tetrafluoroborate has a structure similar to that of lithium difluorooxalate borate, and the solutions of the two have high viscosity, it is difficult to separate the two in the existing process, and the requirements for equipment and technology are relatively high, and production The purity of the mixed salt of the two obtained is low, and these factors greatly increase the cost of the mixed salt electrolyte

Method used

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  • Method for purifying lithium difluoroborate and lithium tetrafluoroborate mixed lithium salt and application thereof
  • Method for purifying lithium difluoroborate and lithium tetrafluoroborate mixed lithium salt and application thereof
  • Method for purifying lithium difluoroborate and lithium tetrafluoroborate mixed lithium salt and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A kind of preparation method of high-purity fixed ratio mixed lithium salt, comprises the steps:

[0039] (1) Synthesis reaction:

[0040] Add 500mL dimethyl carbonate (DMC) to the three-necked reaction flask, and add 102g lithium oxalate under stirring at 250r / min; raise the temperature to 90°C, stir for 0.5h, and prepare lithium oxalate suspension; weigh trifluoro 252g of boron chloride ether was gradually added dropwise to the lithium oxalate suspension under stirring, and the dropwise addition time was 1h; The mixed reaction solution of lithium oxalate borate and lithium tetrafluoroborate is then purified through a purification aid filter membrane;

[0041] (2) Concentration and crystallization of the reaction solution:

[0042] The purified mixed reaction solution of lithium difluorooxalate borate and lithium tetrafluoroborate was subjected to vacuum distillation at a vacuum degree of -0.11MPa, a rotation speed of 250r / min, and a temperature of 110°C, and the org...

Embodiment 2

[0051] Add 500mL dimethyl carbonate (DMC) to the three-necked reaction flask, and add 102g lithium oxalate under stirring at 250r / min; raise the temperature to 90°C, stir for 0.5h, and prepare lithium oxalate suspension; weigh trifluoro 252g of boron chloride ether was gradually added dropwise to the lithium oxalate suspension under stirring, and the dropwise addition time was 1h; The mixed reaction solution of lithium oxalate borate and lithium tetrafluoroborate is then purified through a purification aid filter membrane;

[0052] (2) Concentration and crystallization of the reaction solution:

[0053] The purified mixed reaction solution of lithium difluorooxalate borate and lithium tetrafluoroborate was subjected to vacuum distillation at a vacuum degree of -0.1MPa, a rotation speed of 250r / min, and a temperature of 110°C to distill out 80% of the organic solvent as the initial solvent. %, stop vacuum distillation to obtain mixed lithium salt crude product;

[0054] (3) P...

Embodiment 3

[0059] Add 500mL dimethyl carbonate (DMC) to the three-necked reaction flask, and add 102g lithium oxalate under stirring at 250r / min; raise the temperature to 90°C, stir for 0.5h, and prepare lithium oxalate suspension; weigh trifluoro 252g of boron chloride ether was gradually added dropwise to the lithium oxalate suspension under stirring, and the dropwise addition time was 1h; The mixed reaction solution of lithium oxalate borate and lithium tetrafluoroborate is then purified through an auxiliary purification filter;

[0060] (2) Concentration and crystallization of the reaction solution:

[0061] The purified mixed reaction solution of lithium difluorooxalate borate and lithium tetrafluoroborate was subjected to vacuum distillation at a vacuum degree of -0.1MPa, a rotation speed of 250r / min, and a temperature of 110°C to distill out 60% of the organic solvent as the initial solvent. %, stop vacuum distillation to obtain mixed lithium salt crude product;

[0062] (3) Pur...

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Abstract

The invention belongs to the technical field of lithium ion battery manufacturing, and discloses a method for purifying lithium difluoroborate and lithium tetrafluoroborate mixed lithium salt and application thereof. According to the preparation method of the high-purity mixed lithium salt with different proportions, industrial-grade lithium oxalate is used as a raw material, the mixed lithium salt with different molar proportions of lithium difluoroborate and lithium tetrafluoroborate is prepared through the processes of synthesis, concentration, auxiliary purification filter membrane purification and the like, and the mixed lithium salt can adapt to various electrolyte formulas, is used for manufacturing lithium ion batteries, and the production cost is reduced; meanwhile, the method provided by the invention avoids the tedious process of recrystallization and the solid-liquid separation operation after crystallization in the prior art, can improve the yield and purity of the product, and simplifies the technological process.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery manufacturing, in particular to a method for purifying a mixed lithium salt of lithium difluorooxalate borate and lithium tetrafluoroborate and an application thereof. Background technique [0002] Lithium battery electrolyte is the carrier of ion transmission in the battery, generally composed of lithium salt and organic solvent. The electrolyte plays the role of conducting ions between the positive and negative electrodes of the lithium battery, which is the guarantee for the high voltage and high specific energy of the lithium ion battery. The electrolyte is generally prepared from high-purity organic solvents, electrolyte lithium salts, necessary additives and other raw materials under certain conditions and in a certain proportion. Currently, the most common electrolyte lithium salt is lithium hexafluorophosphate (LiPF 6 ), in the process of manufacturing the electrolyte, lithiu...

Claims

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Application Information

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IPC IPC(8): C07F5/02H01M10/0525H01M10/0568
CPCC07F5/025H01M10/0568H01M10/0525H01M2300/0091Y02E60/10
Inventor 吴杰杜建委杨冰周彤曹青青
Owner SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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