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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 acidity of the product, difficult removal of crystal water, product wrapping, etc., and achieve high yield and process Simple, high product purity effect

Active Publication Date: 2022-07-05
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, LiBF 4 The preparation methods mainly include the following: 1) gas-solid reaction method, such as solid LiF and BF 3 Gas reaction, high temperature and high pressure or product encapsulation phenomenon; 2) aqueous solution method, such as the reaction of lithium source and tetrafluoroboric acid aqueous solution, the crystal water carried by the crude product is difficult to remove; 3) non-aqueous solution method, LiF in anhydrous HF or organic solvent with BF 3 Gas reaction, the prepared product has high acidity and is difficult to purify

Method used

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  • Preparation method of high-purity lithium tetrafluoroborate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of high-purity lithium tetrafluoroborate, specifically comprising the following steps (technical process such as figure 1 shown):

[0027] Add 25g (0.5mol) of lithium metaborate to the vertical fluorination furnace replaced by nitrogen and spread it on the material plate, replace it with nitrogen again, set the temperature of the fluorination furnace to 50 ° C, containing F 2 The gas is introduced from the bottom of the vertical fluorination furnace, set F 2 / N 2 The flow rate of the mixed gas is 100mL / min, open F 2 / N 2 Mixed gas intake valve, start to pass F into the furnace at a constant speed 2 F with a quality score of 10% 2 / N 2 The mixed gas was introduced for 600 min. After the reaction, the heating of the fluorination furnace was stopped and the temperature was lowered to room temperature. During the reaction, the excess F 2 / N 2 Mixed gas and by-product O 2 (Tail gas) into 100g / L sodium hydroxide solution for absorption treatment...

Embodiment 2

[0031] A preparation method of high-purity lithium tetrafluoroborate, specifically comprising the following steps:

[0032] Add 25g (0.5mol) lithium metaborate to the vertical fluorination furnace replaced by nitrogen and spread it on the material plate, replace it with nitrogen again, set the temperature of the fluorination furnace to 180 ℃, containing F 2 The gas is introduced from the bottom of the vertical fluorination furnace, set F 2 / N 2 The flow rate of the mixed gas is 500mL / min, open F 2 / N 2 Mixed gas intake valve, start to pass F into the furnace at a constant speed 2 F with a quality score of 20% 2 / N 2 The mixed gas was introduced for 285 min. After the reaction, the heating of the fluorination furnace was stopped, and the temperature was lowered to room temperature. During the reaction, the excess F 2 / N 2 Mixed gas and by-product O 2 (Tail gas) into 100g / L sodium hydroxide solution for absorption treatment.

[0033]The product was added to 500 g of et...

Embodiment 3

[0036] A preparation method of high-purity lithium tetrafluoroborate, specifically comprising the following steps:

[0037] Add 25g (0.5mol) of lithium metaborate to the vertical fluorination furnace replaced by nitrogen and spread it on the material plate, replace it with nitrogen again, set the temperature of the fluorination furnace to 50 ° C, containing F 2 The gas is introduced from the bottom of the vertical fluorination furnace, set F 2 / N 2 The flow rate of the mixed gas is 100mL / min, open F 2 / N 2 Mixed gas intake valve, start to pass F into the furnace at a constant speed 2 F with a quality score of 30% 2 / N 2 The mixed gas was introduced for 300 min. After the reaction, the heating of the fluorination furnace was stopped and the temperature was lowered to room temperature. During the reaction, the excess F 2 / N 2 Mixed gas and by-product O 2 (Tail gas) into 100g / L sodium hydroxide solution for absorption treatment.

[0038] The product was added to 500 g o...

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Abstract

The invention relates to a preparation method of high-purity lithium tetrafluoroborate, which comprises the following steps: by taking lithium metaborate as a raw material, carrying out fluorination reaction on the lithium metaborate and excessive F2-containing gas at 50-180 DEG C for 200-600 minutes, after the reaction is finished, dissolving a reaction product in a benign organic solvent under the protection of nitrogen, filtering out insoluble substances, and carrying out spray drying on filtrate, thereby obtaining the high-purity lithium tetrafluoroborate. According to the method, F2-containing gas is adopted as a raw material for fluorinating lithium metaborate, the non-fluorinated raw material lithium metaborate is recovered after a reaction product is dissolved by a benign organic solvent, high-purity lithium tetrafluoroborate is prepared by spray drying of a dissolved solution, and meanwhile, the organic solvent is recovered for recycling. Excessive F2-containing gas is absorbed by alkali liquor to prepare a high-purity sodium fluoride by-product. The whole process is simple, the product purity is high, the yield is high, no wastewater or solid is discharged, and the method is economical and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery additives, and particularly relates to a preparation method of high-purity lithium tetrafluoroborate. Background technique [0002] Lithium tetrafluoroborate, molecular formula LiBF 4 , molecular weight 93.74, appearance white powder, melting point 293-300 ℃, the main use is industrial catalyst and lithium ion battery electrolyte additive. In the current field of lithium-ion batteries, lithium hexafluorophosphate is the main electrolyte salt, which has the advantages of fast charging and discharging speed, strong applicability, and high safety, but its thermal stability is poor, and a new type of electrolyte with better performance is needed to supplement it. or alternative. LiBF 4 Its chemical properties and thermal stability are good, it is not easy to decompose at high temperature, and the charge transfer resistance is small at low temperature. Adding it to the electrolyte of lit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/06
CPCC01B35/06Y02E60/10
Inventor 杨华春李云峰杨明霞高胜军张永明杨水艳赵艳玲郭海涛
Owner DO FLUORIDE CHEM CO LTD