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Preparation method of lithium bis (oxalato) borate

A technology of lithium bis-oxalate borate and boric acid, applied in the field of lithium ion batteries, can solve the problems of poor thermal stability, high moisture content, low product yield, etc., and achieves improved product yield and purity, simple and convenient post-processing, and residual moisture. low volume effect

Pending Publication Date: 2022-07-22
WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium hexafluorophosphate is easy to hydrolyze and has poor thermal stability. It will decompose in the presence of trace moisture and generate corrosive hydrofluoric acid, which will cause attenuation and failure of lithium-ion battery performance.
[0008] In the above preparation method, it is unavoidable to produce water in the reaction process; and the existence of water will cause the moisture content in the final product to be high, and it is difficult to remove; meanwhile, bisoxalate lithium borate will be partially hydrolyzed, especially when heating and dehydrating , the hydrolysis is accelerated, resulting in a low product yield and a lot of three wastes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of lithium bis-oxalate borate, comprising the following steps:

[0028] (1) get 198g (2.2mol) anhydrous oxalic acid and 62g (1mol) boric acid and join in the there-necked flask with stirring device, above-mentioned reaction raw material under normal pressure, mechanical stirring condition, be warming up to 80 ℃ of reaction 8 hours; After pressing, continue to be warming up to 200 ℃, and vacuum-dry 5 hours at this temperature; Obtain white solid reactant in the flask; In the above-mentioned reaction process, oxalic acid and boric acid generate two oxalic acid boric acid, and the reaction equation is as follows:

[0029] 2H 2 C 2 O 4 +H 3 BO 3 →HC 4 BO 8 +3H 2 O

[0030] (2) under nitrogen atmosphere, the reactant obtained in step (1) was cooled to room temperature, 26.4 g (1.1 mol) of lithium hydroxide and 19 g of anhydrous magnesium sulfate were added, the temperature was raised to 100° C., and the reaction was carried out under stirring for...

Embodiment 2

[0035] A preparation method of lithium bis-oxalate borate, comprising the following steps:

[0036] (1) get 189g (2.1mol) anhydrous oxalic acid and 62g (1mol) boric acid and join in the there-necked flask with stirring device, above-mentioned reaction raw material under normal pressure, mechanical stirring condition, be warming up to 60 ℃, react 10 hours; After decompression, continue to heat up to 180 ° C, and vacuum dry at this temperature for 8 hours; white solid reactant is obtained in the flask; in the above-mentioned reaction process, oxalic acid and boric acid generate bisoxalic acid boric acid;

[0037] (2) under nitrogen atmosphere, the reactant obtained in step (1) was cooled to room temperature, 37 g (0.5 mol) of lithium carbonate and 24 g of phosphorus pentoxide were added, the temperature was raised to 110 ° C, and the reaction was stirred for 8 hours; in this step In, bis-oxalate borate reacts with lithium carbonate to generate bis-oxalate borate, and the reactio...

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Abstract

The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of lithium bis (oxalato) borate. When the lithium bis (oxalato) borate is prepared, oxalic acid and boric acid are utilized to generate an intermediate bis (oxalato) boric acid, the bis (oxalato) boric acid cannot be combined with water molecules to form a crystal water complex, and after vacuum drying, moisture is thoroughly removed; therefore, in the next reaction process of the bis (oxalato) boric acid and the lithium compound, the drying agent is continuously combined with the reacted water, so that the reaction is in a condition close to no water, the hydrolysis caused by contact between the lithium bis (oxalato) borate product obtained after the reaction and the water can be avoided, and the yield and purity of the product are improved. According to the preparation method disclosed by the invention, the post-treatment after the reaction is simple and convenient, and the lithium bis (oxalato) borate product can be obtained by dissolving, decoloring, concentrating, crystallizing, washing and drying. The preparation method disclosed by the invention is high in reaction yield, and the obtained product is low in water residue, easy to purify and high in purity.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, relates to the synthesis of electrolyte lithium salts, and in particular relates to a preparation method of lithium bis-oxalate borate. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, high output voltage, long cycle life, no memory effect, and low environmental pollution. They are the most attractive and potential secondary batteries. Preferred. Electrolyte is one of the basic key materials of lithium-ion battery. As the main component of electrolyte, the performance of electrolyte plays a decisive role in electrolyte and lithium-ion battery. [0003] Lithium hexafluorophosphate, as the most mature and commonly used electrolyte salt in commercialization, has certain defects. Lithium hexafluorophosphate is easily hydrolyzed and has poor thermal stability. In the presence of trace moisture, a decomposition reaction occurs to generate c...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 蒋颉李新华饶婷王敏贾莉伟王家明
Owner WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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