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A kind of preparation method of lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and lithium fluoride, applied in tetrafluoroboric acid, boron halide compounds and other directions, can solve the problems of difficult purification and many production links, and achieve the effect of simple preparation method and cost saving

Active Publication Date: 2016-03-30
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the problems and shortcomings of many production links and difficult purification in the above-mentioned process, the present invention provides a preparation method of lithium tetrafluoroborate with few production links and convenient purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] At room temperature, add 9.24gLiF and 105.25gHF to a 316L reaction vessel with a jacket, and stir overnight to completely dissolve LiF in HF, and introduce 5.41g of diborane into the jacket to cool medium, control the temperature at 10°C, then slowly introduce fluorine gas, and stir. As the reaction progresses, its pressure gradually decreases. Then the filtrate is filtered, and the quality of the filtrate is 49.87g, and the obtained lithium tetrafluoroborate product is dried, and the quality of the product is 23.78g, and LiBF in the filtrate 4 The content is 18.23%, the product purity of the obtained product is 99.97%, the water content is 4.8ppm, and the acid content is 10ppm.

[0021] Table I

[0022] project

Embodiment 2

[0024] At room temperature, 4.31g LiF was added to a 316L reaction vessel with a jacket, and 49.87g of the filtrate obtained in Example 1 was added to it, stirred overnight to completely dissolve LiF in HF, and 5.41g of diborane was introduced , a low-temperature cooling medium is passed into the jacket, the temperature is controlled at 10°C, and then fluorine gas is slowly introduced and stirred. As the reaction progresses, the pressure gradually decreases. After the pressure no longer changes, continue to stir for 6 hours, and then About 50% of its original volume, will then filter the filtrate, the quality of the gained filtrate is 24.56g, after drying the lithium tetrafluoroborate product, the quality of the gained product is 19.96g, the LiBF in the filtrate 4 The content is 18.36%, the yield of the product obtained is 98.79%, the product purity is 99.33%, the water content is 6.2ppm, and the acid content is 13ppm.

[0025] Table II

[0026] project

Embodiment 3

[0028] At room temperature, add 10.51gLiF and 106.23gHF to a tetrafluoro reaction vessel with a jacket, and stir for one night to fully dissolve LiF in HF, and pass 5.93g of diborane into the jacket. Cooling medium, control the temperature at 10°C, then slowly introduce fluorine gas, and stir. As the reaction progresses, its pressure gradually decreases. , and then the filtrate is filtered, and the quality of the filtrate is 46.27g. After drying the lithium tetrafluoroborate product, the quality of the product is 29.52g. LiBF in the filtrate 4 The content is 18.62%, the yield of the product obtained is 98.66%, the water content is 3.2ppm, and the acid content is 12ppm.

[0029] Table three

[0030] project

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PUM

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Abstract

The invention relates to a preparation method of lithium tetrafluoroborate, which is characterized in that borane and fluorine gas react to generate boron trifluoride, and the boron trifluoride reacts with halogenated lithium salt dissolved in hydrogen fluoride to generate lithium tetrafluoroborate. The method comprises the following steps: putting LiF in a stainless steel reaction vessel, sufficiently dissolving the LiF in HF, and introducing a certain amount of borane, wherein the mole ratio of the boron element in the borane to the lithium element in the halogenated lithium salt is (1.2-1):1; slowly introducing fluorine gas, sufficiently reacting, and continuing stirring for 2-6 hours, wherein the reaction temperature is -20-15 DEG C; and after the reaction finishes, concentrating the reaction solution to 40-80% of the original volume by heating, filtering to obtain a LiBF4 crystal, and drying to obtain the lithium tetrafluoroborate product.

Description

technical field [0001] The invention relates to the technical field of manufacturing lithium-ion battery materials, in particular to a method for preparing lithium tetrafluoroborate, an electrolyte lithium salt. 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. [0003] Electrolyte is one of the basic raw materials of lithium-ion battery electrolyte, which directly affects the working performance of lithium-ion batteries. The lithium salt used in lithium-ion batteries is generally LiPF 6 、LiBF 4 , LiClO 4 , LiAsO 4 , LiN(CF 3 SO 2 )Wait. LiClO 4 Due to its strong oxidizing properties, there are large safety issues, so it is mainly used in experimental research. LiAsO 4 It has the advantages of simple purif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06
CPCC01B35/066
Inventor 王坤刘红光叶学海刘大凡袁莉赵洪孙培亮
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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