Preparation method of lithium oxalyldifluoroborate

A technology of lithium difluorooxalate borate and lithium tetrafluoroborate, which is applied in the field of lithium ion battery electrolyte preparation, can solve the problems of high requirements for lithium difluorooxalate borate, difficult separation of main and side reaction products, and generation of corrosive gases, etc., to achieve Low cost, improved reaction conversion rate, and high conversion rate

Active Publication Date: 2020-11-17
DONGYING HI TECH SPRING CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention is aimed at the preparation of difluorooxalate lithium borate in the above-mentioned background technology, which requires high reaction equipment, the main and side reaction products are not easy to separate, and corrosive gases are produced in the

Method used

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preparation example Construction

[0022] The invention provides a kind of preparation method of lithium difluorooxalate borate, comprising the steps of:

[0023] 1) mixing lithium tetrafluoroborate, lithium oxalate, an organic solvent and an auxiliary agent, reacting the obtained mixed solution to obtain a reaction solution containing LiODFB;

[0024] The auxiliary agent is niobium pentachloride, niobium pentafluoride or antimony pentafluoride;

[0025] 2) Filtrating the reaction solution containing LiODFB in step 1), and concentrating the filtrate to obtain the crude product of lithium difluorooxalate borate;

[0026] 3) Recrystallize and dry the crude product of lithium difluorooxalate borate in the step 2) to obtain lithium difluorooxalate borate.

[0027] The invention mixes lithium tetrafluoroborate, lithium oxalate, an organic solvent and an auxiliary agent, and reacts the obtained mixed solution to obtain a reaction solution containing LiODFB. In the present invention, the molar ratio of lithium tetra...

Embodiment 1

[0034] (1) Take 320g of acetonitrile solvent into the reaction vessel, add 31.25g of lithium tetrafluoroborate and 40.76g of lithium oxalate under stirring, continue stirring for 60min, and adjust the solution temperature to 10°C;

[0035] (2) After the temperature was constant, 6.0 g of niobium pentachloride was added to the solution, and the reaction was completed after 16 hours to obtain a reaction solution containing lithium difluorooxalate borate.

[0036] (3) Filter the reaction solution containing lithium difluorooxalate borate obtained in step (2) to remove insoluble matter, distill under reduced pressure at 0.005Mpa until the solution becomes turbid, then cool down to -5°C to crystallize for 3 hours, and filter to obtain lithium difluorooxalate borate Crude product; the crude product was dissolved in dimethyl carbonate for recrystallization, and vacuum-dried at 150° C. with a vacuum degree of 90 Kpa to obtain lithium difluorooxalate borate.

[0037](4) Recover and enr...

Embodiment 2

[0039] (1) Add 400g of acetonitrile solvent into the reaction vessel, add 35g of lithium tetrafluoroborate and 38g of lithium oxalate under stirring, continue stirring for 60min, and adjust the temperature of the solution to 15°C;

[0040] (2) After the temperature was constant, 4.18 g of niobium pentafluoride was added to the solution, and the reaction was continued after 24 hours to obtain a reaction solution containing lithium difluorooxalate borate.

[0041] (3) Filter the reaction solution containing lithium difluorooxalate borate obtained in step (2) to remove insoluble matter, distill under reduced pressure at 0.02Mpa until the solution becomes turbid, then cool down to 5°C for crystallization for 5 hours, and filter to obtain the crude product of lithium difluorooxalate borate ; Dissolve the crude product in dimethyl carbonate for recrystallization, and dry it in vacuum at 80°C and a vacuum of 80Kpa to obtain lithium difluorooxalate borate.

[0042] (4) Recover and enr...

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Abstract

The invention discloses a preparation method of lithium oxalyldifluoroborate, and belongs to the technical field of lithium ion battery electrolyte preparation. The preparation method comprises the following steps: 1) mixing lithium tetrafluoroborate, lithium oxalate, an organic solvent and an auxiliary agent, and carrying out a reaction on the obtained mixed solution to obtain a reaction solutioncontaining LiODFB, wherein the auxiliary agent is niobium pentachloride, niobium pentafluoride or antimony pentafluoride; 2) filtering the reaction solution containing LiODFB, and concentrating the filtrate to obtain a lithium oxalyldifluoroborate crude product; and 3) recrystallizing the lithium oxalyldifluoroborate crude product, and conducting drying to obtain lithium oxalyldifluoroborate. Thepreparation method provided by the invention has the advantages of high conversion rate, high product purity and high yield, and no corrosive gas is generated in the reaction process.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery electrolyte preparation, in particular to a preparation method of lithium difluorooxalate borate. Background technique [0002] Lithium-ion battery is a new type of high-energy secondary battery, which has excellent properties such as small size, light weight, high-rate discharge, high specific energy, and no memory effect. Lithium-ion batteries are widely used in electronics, automobiles, household appliances and other fields. Electrolyte is one of the main components of lithium-ion batteries and one of the key materials affecting the performance of lithium-ion batteries. The electrolyte of commonly used lithium-ion batteries is mainly lithium hexafluorophosphate (LiPF6), but lithium hexafluorophosphate is easy to absorb water and deliquescence, and the decomposition product HF will corrode the electrode, and lithium hexafluorophosphate must be used in combination with ethylene carbo...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022Y02E60/10
Inventor 滕文彬张生安刘博闻张友强
Owner DONGYING HI TECH SPRING CHEM IND
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