Preparation method of high-purity lithium tetrafluoroborate

A technology of high-purity lithium tetrafluoroborate and lithium tetrafluoroborate, which is applied in the field of preparation of high-purity lithium tetrafluoroborate, can solve the problems of high production cost and environmental pollution, and achieves low water content, strong operability, and no The effect of three wastes discharge

Inactive Publication Date: 2015-01-28
DO FLUORIDE CHEM CO LTD
View PDF9 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The non-aqueous solvent method uses a large amount of organic solvents as the extrac

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:

[0025] (1) Under the condition of -10°C, boric acid is slowly added to a hydrofluoric acid solution with a mass percentage concentration of 10%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:4, then continue to stir, react for 2h, and prepare fluoroboric acid solution;

[0026] (2) At -10°C, add lithium carbonate to the fluoroboric acid solution prepared in step (1) according to the molar ratio Li:B=1.05, and stir for 0.5 h to obtain a lithium tetrafluoroborate solution;

[0027] (3) The lithium tetrafluoroborate solution is concentrated at -0.05MPa and 90°C to 1 / 8 of the original volume of the lithium tetrafluoroborate solution, then cooled to crystallize at room temperature at 20°C, filtered, and the obtained solid is four Lithium fluoroborate crystal;

[0028] (4) Lithium tetrafluoroborate crystals were preliminarily dried at 60°C...

Embodiment 2

[0032] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:

[0033] (1) Under the condition of 10 DEG C, boric acid is slowly added to the hydrofluoric acid solution whose mass percent concentration is 60%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:6, then continue to stir, react for 0.5h, and prepare fluoboric acid solution;

[0034] (2) under the condition of 15° C., lithium hydroxide was added into the fluoroboric acid solution prepared in step (1) according to the molar ratio Li:B=1.5, and the reaction was stirred for 5 hours to obtain a lithium tetrafluoroborate solution;

[0035] (3) The lithium tetrafluoroborate solution is concentrated at -0.09MPa and 50°C to 1 / 3 of the original volume of the lithium tetrafluoroborate solution, then cooled to crystallize at room temperature at 20°C, filtered, and the obtained solid is four Lithium fluoroborate crystal;

[0036] (4) Lithium tetraflu...

Embodiment 3

[0040] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:

[0041] (1) Under the condition of 0 DEG C, boric acid is slowly added into the hydrofluoric acid solution whose mass percent concentration is 30%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:4.5, then continue to stir, react for 5h, and prepare fluoboric acid solution;

[0042] (2) Add lithium bicarbonate into the fluoroboric acid solution prepared in step (1) according to the ratio of molar ratio Li:B=1.2 at 0° C., and stir for 2 hours to obtain a lithium tetrafluoroborate solution;

[0043] (3) Lithium tetrafluoroborate solution was concentrated at -0.08MPa and 70°C to 1 / 5 of the original volume of the lithium tetrafluoroborate solution, then cooled to room temperature at 20°C for cooling and crystallization, and filtered to obtain a solid of four Lithium fluoroborate crystal;

[0044] (4) Lithium tetrafluoroborate crystals were ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention belongs to the technical field of electrolyte lithium salts for lithium ion batteries, and particularly discloses a preparation method of high-purity lithium tetrafluoroborate. The preparation method comprises the following steps: synthesizing lithium tetrafluoroborate by taking hydrofluoric acid, boric acid and lithium compound as raw materials, carrying out concentration, crystallization and secondary drying on lithium tetrafluoroborate to obtain the crude product of the lithium tetrafluoroborate; dissolving the crude product of the lithium tetrafluoroborate in anhydrous hydrogen fluoride again, and feeding high-purity fluorine into the solution for purifying and removing impurities; then, carrying out cooling crystallization, filtering and drying to obtain the high-purity lithium tetrafluoroborate product, wherein the purity of the product reaches up to more than 99.99%. According to the preparation method, the high-purity fluorine is used for purifying, and the high-purity lithium tetrafluoroborate product with high purity and low water content can be prepared. The raw materials are easy to obtain, the whole production process is mild in conditions, high in operability, high in raw material utilization rate and free from discharge of 'three wastes', and the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of electrolyte lithium salts for lithium ion batteries, in particular to a preparation method of high-purity lithium tetrafluoroborate. Background technique [0002] Lithium tetrafluoroborate, molecular formula LiBF 4 , molecular weight 93.74, mainly used as electrolyte lithium salt for lithium-ion battery electrolyte. With the rapid development of mobile communications and portable appliances in modern society, lithium-ion secondary batteries are widely used in people's daily life due to their high energy density, high working voltage, small memory effect, low self-discharge rate, lightness and convenience. application. At present, the classic electrolyte system used in lithium-ion secondary batteries is that the electrolyte salt is dissolved in an organic aprotic solvent. As one of the basic raw materials of lithium-ion batteries, the electrolyte directly affects the working performance of lithium-ion ba...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B35/06
CPCC01B35/066C01P2006/80C01P2006/82
Inventor 李云峰杨华春侯红军郑金霞马广辉陈虎薛峰峰贾雪枫李磊王晓峰
Owner DO FLUORIDE CHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap