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Preparation method of lithium bis(oxalato)borate

A technology of bisoxalate lithium borate and anhydrous oxalic acid, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve problems such as high energy consumption, high cost, and difficult purification , to achieve the effect of high energy consumption, high solution cost and high difficulty in purification

Inactive Publication Date: 2020-05-08
TIANJIN JINNIU POWER SOURCES MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of this, in order to overcome the problems and deficiencies of high cost, difficult purification and high energy consumption in the above-mentioned process, the present invention provides a method for preparing lithium bisoxalate borate with a simple synthesis method

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  • Preparation method of lithium bis(oxalato)borate

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preparation example Construction

[0046] The invention discloses a method for preparing lithium bisoxalate borate, which mainly includes synthesizing a crude product of lithium bisoxalate borate and concentrating, crystallizing and purifying, specifically including the following steps:

[0047] (1) Take boron simple substance, lithium powder and anhydrous oxalic acid and mix uniformly to obtain mixed raw materials;

[0048] (2) Put the mixed raw material in step (1) into a ball mill and react under normal pressure for 2-6 hours to obtain the product, then add an organic solvent for wet grinding to obtain a solution containing the crude lithium bisoxalate borate;

[0049] (3) Concentrating, crystallizing, filtering, and drying the solution containing the crude lithium bisoxalate borate obtained in step (2) to obtain a lithium bisoxalate borate.

[0050] (1) In order to further realize the technical effect of the present invention, in the mixed raw material of step (1), the molar ratio of boron simple substance,...

Embodiment 1

[0059] At room temperature, add 1.79g lithium powder, 46.46g anhydrous oxalic acid, 2.79g boron powder, reacted at 80°C for 4 hours, cooled to room temperature, slowly added 150g of ethylene glycol dimethyl ether through the solvent inlet, and stirred for 12 hours to completely dissolve the product in the solvent to obtain a solution containing the crude bisoxalate lithium borate .

[0060] Transfer the solution containing the crude lithium bisoxalate borate to a concentration kettle, and concentrate the solution to 80% of the original volume by heating, after cooling it to room temperature, add 150g of dichloromethane for crystallization, and filter to obtain the The wet product of the solvent, which was transferred to the lithium bisoxalate borate product of the organic solvent was dried in a 316L stainless steel drier to obtain the lithium bisoxalate borate product.

[0061] The quality of the obtained lithium bisoxalate borate after drying was 48.24g, the purity of the ob...

Embodiment 2

[0065] At room temperature, add 1.79g lithium powder, 46.46g anhydrous oxalic acid, 2.79g boron Powder, reacted at 80°C for 4 hours, cooled to room temperature, slowly added 150g of ether through the solvent inlet, stirred for 12 hours, completely dissolved the product in the solvent, and obtained a solution containing the crude lithium bisoxalate borate.

[0066] Transfer the solution containing the crude lithium bisoxalate borate to a concentration kettle, and concentrate the solution to 80% of the original volume by heating, after cooling it to room temperature, add 150g of dichloromethane for crystallization, and filter to obtain the The wet product of the solvent, which was transferred to the lithium bisoxalate borate product of the organic solvent was dried in a 316L stainless steel drier to obtain the lithium bisoxalate borate product.

[0067] The quality of the obtained lithium bisoxalate borate product after drying was 48.72g, the purity of the obtained product was 9...

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Abstract

The invention discloses a preparation method of lithium bis(oxalato)borate. The preparation method mainly comprises: synthesizing a lithium bis(oxalato)borate crude product, concentrating, crystallizing and purifying, and specifically comprises the following steps: weighing and uniformly mixing elemental boron, lithium powder and anhydrous oxalic acid to obtain a raw material mixture; putting theraw material mixture into a ball mill, performing a normal-pressure reaction for 2-6 h, then adding an organic solvent, and performing wet grinding to obtain a solution containing the lithium bis(oxalato)borate crude product; and concentrating, crystallizing and filtering the solution containing the lithium bis(oxalato)borate crude product, and then drying to obtain the lithium bis(oxalato)borate.Production links are few, purification is convenient, the purity of the prepared lithium bis(oxalato)borate product can reach 99.99%, the moisture content is lower than 10 ppm, and the production requirements of lithium ion battery electrolytes are met.

Description

technical field [0001] The invention belongs to the technical field of preparation of lithium ion battery materials, and relates to a method for preparing an electrolyte salt, more specifically, to a method for preparing lithium bisoxalate borate. Background technique [0002] Lithium-ion batteries have been widely used as portable power sources in mobile phones, notebook computers, cameras, etc. due to their advantages such as high working voltage, high energy density, low self-discharge rate, no memory effect, long cycle life, lightness and convenience. Electrolyte is one of the basic raw materials of lithium-ion battery electrolyte, which directly affects the working performance of lithium-ion batteries. As a new electrolyte lithium salt, LiBOB has good thermal and chemical stability, high electrical conductivity and wide electrochemical window, so its synthesis research has attracted extensive attention. [0003] At present, the preparation methods of lithium bis(oxalat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 王坤赵庆云袁莉陈运甫孙培亮安峰李勇林张梦
Owner TIANJIN JINNIU POWER SOURCES MATERIAL
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