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Lithium bis(oxalato)borate preparation method

A technology of lithium bis-oxalate borate and oxalic acid is applied in the field of preparation of lithium bis-oxalate borate, can solve the problems of harsh preparation conditions, high cost of raw materials, poor thermal stability, etc., achieves cheap and easy-to-obtain raw materials, simple and feasible process, and improved film formation. performance effect

Inactive Publication Date: 2019-01-18
湖南科霸汽车动力电池有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the main electrolyte lithium salts used in lithium battery electrolytes on the market are: 1. Lithium hexafluorophosphate. The low-temperature performance of batteries composed of lithium salts as electrolytes is not particularly good; 2. Lithium tetrafluoroborate: Due to the limitation of preparation conditions, it is difficult to obtain high-purity lithium tetrafluoroborate by the current process, and the ones produced now generally contain a lot of impurities , it is easy to react with the active material of the lithium-ion secondary battery during use, making the battery unable to use normally, etc.

Method used

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  • Lithium bis(oxalato)borate preparation method

Examples

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Embodiment 1

[0017] A method for preparing lithium bis-oxalate borate, weighing each substance at a molar ratio of lithium hydroxide, oxalic acid and boric acid of 1:2:1, and then placing the lithium hydroxide and boric acid in an oven at 60°C for 4 hours Put the oxalic acid in an oven with a temperature of 120°C for 4 hours, then place the dried lithium hydroxide and oxalic acid in a ball mill for 15 minutes, and then add the dried boric acid to the ball mill for 15 minutes until a uniform The mixture was then dry-pressed into tablets under a pressure of 0.2 MPa, and then put into a container, first placed in a vacuum box with a temperature of 120°C for 6 hours, and then the temperature of the vacuum box was increased to 150°C so that the mixture was placed at a temperature of After 15 hours of reaction in a vacuum box at 150°C, a crude product of lithium bisoxalate borate is obtained. The crude product of lithium bisoxalate borate is then ground into a powder and fully dissolved in distill...

Embodiment 2

[0023] A method for preparing lithium bisoxalate borate, the steps of which are basically the same as those of the method for preparing lithium bisoxalate borate in Example 1, and the difference lies in:

[0024] 1. Lithium hydroxide and boric acid are placed in an oven at 50°C for 6 hours, and oxalic acid is placed in an oven at 130°C for 4.5 hours;

[0025] 2. The ball milling time of lithium hydroxide and oxalic acid is 25min, and the ball milling after boric acid is added is 25min;

[0026] 3. The mixture is dry pressed into tablets under a pressure of 0.22 MPa and then put into a container, first placed in a vacuum box with a temperature of 130°C for 5 hours, and then the temperature of the vacuum box is increased to 170°C so that the mixture is placed at 170°C Reaction in a vacuum box for 12 hours to obtain a crude product of lithium bisoxalate borate;

[0027] 4. Evaporate and concentrate the filtrate until the remaining liquid is 2% of the total filtrate;

[0028] 5. The produc...

Embodiment 3

[0031] A method for preparing lithium bisoxalate borate, the steps of which are basically the same as those of the method for preparing lithium bisoxalate borate in Example 1, and the difference lies in:

[0032] 1. Lithium hydroxide and boric acid are placed in an oven at 70℃ for 4.5 hours, and oxalic acid is placed in an oven at 105℃ for 6 hours;

[0033] 2. The ball milling time of lithium hydroxide and oxalic acid is 10 minutes, and the ball milling time after boric acid is added is 25 minutes;

[0034] 3. The mixture is dry pressed into tablets under a pressure of 0.25 MPa and then put into a container, first placed in a vacuum box with a temperature of 105°C for 8 hours, and then the temperature of the vacuum box is increased to 140°C so that the mixture is placed at a temperature of 140°C Reaction in a vacuum box for 24 hours to obtain a crude product of lithium bisoxalate borate;

[0035] 4. Evaporate and concentrate the filtrate until the remaining liquid is 1.5% of the total...

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Abstract

The invention provides a lithium bis(oxalato)borate preparation method. The preparation method comprises the steps: weighing lithium hydroxide, oxalic acid and boric acid according to a certain molarratio; then respectively drying lithium hydroxide, oxalic acid and boric acid; then putting the dried lithium hydroxide, oxalic acid and boric acid into a ball mill to be evenly ball milled to form amixture; then dry pressing the mixture into pieces under the certain pressure P; then putting into a container; reacting under the vacuum environment with a temperature as 105 to 130 DEG C for 5 to 8h; then putting into the vacuum environment with a temperature as 140 to 170 DEG C to react for 12 to 24 h to prepare a lithium bis(oxalato)borate crude product; then grinding the lithium bis(oxalato)borate crude product into powder; fully dissolving into distilled anhydrous acetonitrile; filtering to obtain filtrate; evaporating and concentrating the filtrate until the residual liquid is 1 to 2%of the total amount of the filtrate; finally, pouring the residual liquid and drying a product which is prepared by evaporating and concentrating the filtrate to obtain lithium bis(oxalato)borate. According to the method disclosed by the invention, a technology is simple, the raw materials are cheap and easy to obtain, and the purity of the prepared product is extremely high.

Description

Technical field [0001] The invention relates to a preparation method of lithium bisoxalate borate. Background technique [0002] At present, the main electrolyte lithium salts used in the electrolyte of lithium batteries on the market are: 1. Lithium hexafluorophosphate, its manufacturing process is complicated, the preparation conditions are very harsh, it is very sensitive to moisture, and the cost of raw materials is relatively high, and the thermal stability is relatively poor. The low-temperature performance of the battery composed of electrolyte lithium salt is not particularly good; 2. Lithium tetrafluoroborate: Due to the limitation of preparation conditions, it is difficult to obtain high-purity lithium tetrafluoroborate with the current process, and the current prepared generally contains a lot of impurities , In use, it is easy to react with the active material of the lithium ion secondary battery, making the battery unable to be used normally and so on. As a new type...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 钟发平黄明匡德志宋婷李华柳立新胡向宇
Owner 湖南科霸汽车动力电池有限责任公司
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