Preparation method of low moisture lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and hydrated lithium metaborate, which is applied in the directions of tetrafluoroboric acid, borates, boron oxide compounds, etc., can solve the problems of being unsuitable for industrial production, increasing production costs, complicated operations, etc., and shortening the drying time. , the effect of reducing energy consumption and simple process control

Active Publication Date: 2015-04-22
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is novel, but the operation is complicated, and a large amount of organic solvents are used in the production process,

Method used

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  • Preparation method of low moisture lithium tetrafluoroborate

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Embodiment 1

[0022] A preparation method of low-moisture lithium tetrafluoroborate, the steps are as follows:

[0023] 1) Weigh 86.1g of lithium metaborate dihydrate and dissolve it in 86.2g of pure water, and stir fully to obtain a lithium metaborate slurry;

[0024] 2) Slowly add the above slurry into a polytetrafluoroethylene reactor filled with 200.4g of 40% hydrofluoric acid for reaction and fully stir to obtain a crude solution of lithium tetrafluoroborate, and the reaction time is 1h;

[0025] 3) Slowly add boric acid to the above solution, and fully stir until the reaction is complete to obtain a clear lithium tetrafluoroborate solution, consuming 27.8g of boric acid, and the reaction time is 1h;

[0026] 4) Filter the above clarified lithium tetrafluoroborate solution, concentrate it in a water bath at 80°C until the content of lithium tetrafluoroborate is 55%, then adjust the temperature of the water bath to 30°C, and centrifuge to obtain lithium tetrafluoroborate after the cryst...

Embodiment 2

[0030] A preparation method of low-moisture lithium tetrafluoroborate, the steps are as follows:

[0031] 1) Weigh 172.0g of lithium metaborate dihydrate and dissolve it in 258.4g of pure water, and stir fully to obtain a lithium metaborate slurry;

[0032] 2) Slowly add the above slurry into a polytetrafluoroethylene reactor filled with 410.5g of 40% hydrofluoric acid for reaction and fully stir to obtain a crude solution of lithium tetrafluoroborate, and the reaction time is 1.5h;

[0033] 3) Boric acid was slowly added to the above solution, and fully stirred until the reaction was complete to obtain a clear lithium tetrafluoroborate solution, 59.6 g of boric acid was consumed, and the reaction time was 1.5 h;

[0034] 4) Filter the above-mentioned lithium tetrafluoroborate clarified solution, concentrate it in a water bath at 90°C until the content of lithium tetrafluoroborate is 65%, then adjust the temperature of the water bath to 35°C, and centrifuge to obtain lithium t...

Embodiment 3

[0038] A preparation method of low-moisture lithium tetrafluoroborate, the steps are as follows:

[0039] 1) Weigh 258.0g of lithium metaborate dihydrate and dissolve it in 516.3g of pure water, and fully stir to obtain a lithium metaborate slurry;

[0040] 2) Slowly add the above slurry into a polytetrafluoroethylene reactor filled with 631.2g of 40% hydrofluoric acid for reaction and fully stir to obtain a crude solution of lithium tetrafluoroborate, and the reaction time is 2h;

[0041] 3) Boric acid was slowly added to the above solution, and fully stirred until the reaction was complete to obtain a clear lithium tetrafluoroborate solution, 90.1 g of boric acid was consumed, and the reaction time was 2 hours;

[0042] 4) Filter the above-mentioned lithium tetrafluoroborate clarified solution, concentrate it in a water bath at 90°C until the content of lithium tetrafluoroborate is 75%, then adjust the temperature of the water bath to 40°C, and centrifuge to obtain lithium t...

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Abstract

The invention belongs to the preparation technology field of electrolyte lithium salt for a lithium ion battery, and particularly discloses a preparation method of low moisture lithium tetrafluoroborate. The preparation method comprises the following steps that dihydrate lithium metaborate is dissolved in pure water so that seriflux is prepared, the seriflux is added to hydrofluoric acid to react so that a lithium tetrafluoroborate rough solution is prepared, a small amount of boric acid is added into the solution and performs reacting completely, lithium tetrafluoroborate crystals are prepared through filtration, evaporation and concentration, cooling crystallization and centrifugal separation, the crystals are dissolved in absolute ethyl alcohol and subject to the first drying, the materials are subject to the second drying in vacuum environment, and the low moisture lithium tetrafluoroborate is obtained. According to the preparation method, the technology is simple, the energy consumption is low, the operability is strong, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of electrolyte lithium salt for lithium ion batteries, in particular to a preparation method of low-moisture lithium tetrafluoroborate. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, high output power, high charging efficiency, long service life and environmental friendliness. , electric vehicles and other fields, the global demand for lithium batteries is increasing year by year with the continuous expansion of application fields. [0003] Electrolyte is the core component of lithium-ion batteries. It is responsible for the transfer of charge between the positive and negative electrodes. It has an extremely important impact on the cycle performance, operating temperature range, and battery durability of the battery. At present, the main electrolyte lithium salt in the market is LiPF 6 , but LiPF 6 Too sensitive to moisture, unstable to heat,...

Claims

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Application Information

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IPC IPC(8): C01B35/12
CPCC01B35/066
Inventor 纪东海黄磊徐涛陈格陈力
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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