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A kind of preparation method of bisoxalate lithium borate

A technology of bisoxalate lithium borate and lithium oxalate, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problem that the raw materials of the synthetic route are difficult to obtain and are not suitable for industrial production and industrialization Problems such as production difficulties, to achieve the effects of easy product purification, increased productivity, and sufficient sources

Active Publication Date: 2021-06-15
TIANJIN JINNIU POWER SOURCES MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the raw materials of the synthetic route are difficult to obtain, the cost is high, and it is not suitable for industrial production
[0008] Chinese patent CN200510011555.7 uses a solid-phase method to synthesize LiBOB, but this method has the disadvantages of high energy consumption, low synthesis efficiency, and difficult industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The embodiment of the present invention discloses a preparation method of lithium bisoxalate borate, and the adopted technical scheme is as follows:

[0047] S1, adding 150g of anhydrous hydrofluoric acid into a 316L stainless steel reaction kettle with a solid feeding device, a jacket, a thermometer, a pressure gauge, a vent, a pressure relief port and a filtering device, and feeding 18g of boron trifluoride, Control the reaction temperature to -10°C, control the pressure below 0.01MPa, and fully stir for 4 hours under airtight conditions, and dissolve boron trifluoride in anhydrous hydrofluoric acid to generate tetrafluoroboric acid;

[0048] S2, slowly add 55.45g of lithium oxalate to the reaction kettle and keep stirring, pass a low-temperature cooling medium into the jacket, control the temperature in the reaction kettle to 0°C, after the addition is complete, fully react for 2 hours, continue stirring for 4 hours;

[0049] S3, heat-treating the product obtained in...

Embodiment 2

[0054] The embodiment of the present invention discloses a preparation method of lithium bisoxalate borate, and the adopted technical scheme is as follows:

[0055] S1, adding 180g of anhydrous hydrofluoric acid into a 316L stainless steel reaction kettle with a solid feeding device, a jacket, a thermometer, a pressure gauge, a vent, a pressure relief port and a filtering device, and feeding 18g of boron trifluoride, Control the reaction temperature to 0°C, control the pressure below 0.01MPa, fully stir for 5 hours under airtight conditions, and dissolve boron trifluoride in anhydrous hydrofluoric acid to generate tetrafluoroboric acid;

[0056] S2, slowly add 55.46g of lithium oxalate into the reaction kettle and keep stirring, pass a low-temperature cooling medium into the jacket, control the temperature in the reaction kettle to 0°C, after the addition is complete, fully react for 3 hours, continue stirring for 5 hours;

[0057] S3, heat-treating the product obtained in S2,...

Embodiment 3

[0062] The embodiment of the present invention discloses a preparation method of lithium bisoxalate borate, and the adopted technical scheme is as follows:

[0063] S1, adding 90g of anhydrous hydrofluoric acid into a 316L stainless steel reaction kettle with a solid feeding device, a jacket, a thermometer, a pressure gauge, a vent, a pressure relief port and a filtering device, and feeding 18g of boron trifluoride, Control the reaction temperature to 10°C, control the pressure below 0.01MPa, and fully stir for 6 hours under airtight conditions, and dissolve boron trifluoride in anhydrous hydrofluoric acid to generate tetrafluoroboric acid;

[0064] S2, slowly add 55.45g of lithium oxalate to the reaction kettle and keep stirring, pass a low-temperature cooling medium into the jacket, control the temperature in the reaction kettle to 0°C, after the addition is complete, fully react for 4 hours, continue to stir for 6 hours;

[0065] S3, heat-treating the product obtained in S2...

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Abstract

The invention discloses a preparation method of lithium bisoxalate borate. The method comprises: dissolving boron trifluoride in anhydrous hydrofluoric acid to generate tetrafluoroboric acid; adding lithium oxalate, heating to remove hydrofluoric acid, and filtering to obtain fluorine-containing lithium bisoxalate borate product; adding a solvent with high solubility to lithium bisoxalate borate, filtering to obtain a solution containing only lithium bisoxalate borate, evaporating the solution and drying to obtain lithium bisoxalate borate. The method of the invention has simple process operation, easy purification, low cost and low energy consumption, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery material manufacture, and more specifically relates to a preparation method of lithium bisoxalate borate. Background technique [0002] Lithium-ion batteries have been widely used as portable power sources 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. At present, the lithium salt used in lithium-ion batteries is generally LiPF 6 . But LiPF 6 It is extremely sensitive to moisture, and a trace amount of moisture can react with it. At the same time, LiPF 6 Its thermal stability is poor. At high temperature, it will decompose and produce HF, which will corrode the electrode material and current collector. Therefore, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 王坤赵庆云桑俊利袁莉安峰孙培亮陈运甫秦凯张冬青
Owner TIANJIN JINNIU POWER SOURCES MATERIAL