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Purification method of lithium bis(oxalato) borate and lithium bis(oxalato)borate

A technology of lithium bis-oxalate borate and purification method, which is applied in chemical instruments and methods, compounds containing periodic table Group 3/13 elements, electrochemical generators, etc. Battery-level use requirements, affecting the quality of lithium bis-oxalate borate, etc., to achieve the effect of easy removal

Inactive Publication Date: 2020-04-24
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems in the prior art that the water removal method of lithium bisoxalate borate cannot remove residual trace moisture and other impurities, and cannot meet the requirements of battery-level use and affect the quality of lithium bisoxalate borate, the purpose of the present invention is to provide a lithium bisoxalate borate Purification method and bisoxalate lithium borate to reduce water residue and impurity content

Method used

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  • Purification method of lithium bis(oxalato) borate and lithium bis(oxalato)borate

Examples

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Embodiment 1

[0026] This example is used to illustrate a method for purifying lithium bisoxalate borate disclosed by the present invention.

[0027] First, the purity is 300 grams of bisoxalate lithium borate crude product (purity 97%, moisture 5000ppm) and 2000 grams of ethyl acetate are mixed and dissolved and filtered, and the filtrate is transferred to the reaction flask, and then 49 grams of thionyl chloride are added dropwise to the reaction flask (The molar ratio with water is 5:1), after the dropwise addition, heat to 45°C, stir and react for 3 hours, then lower the temperature, transfer the reaction solution to a concentrated bottle, then vacuumize and distill the solvent off, and concentrate to the total weight Cool down and add dichloromethane to 400 grams, filter to obtain a solid semi-finished product and transfer it to a crystallization bottle, add a mixed solution of 900 grams of dichloromethane and ethyl acetate (mass ratio 10:1) (the amount of mixed solvent is the crude pro...

Embodiment 2

[0029] This example is used to illustrate a method for purifying lithium bisoxalate borate disclosed by the present invention.

[0030] First, the purity is 300 grams of bisoxalate lithium borate crude product (purity 97%, moisture 0.5%) is filtered after mixing and dissolving with 1000 grams of acetonitrile, and the filtrate is transferred to the reaction flask, and then 65 grams of acetyl chloride (with water) are added dropwise to the reaction flask. The molar ratio is 10:1), heated to 55°C after the dropwise addition, stirred and reacted for 4 hours, then lowered the temperature, transferred the reaction solution to a concentrated bottle, then vacuumed and distilled off the solvent, concentrated to a total weight of 380 grams Cool down and add normal hexane, filter to obtain solid semi-finished product and transfer in the crystallization bottle, add the mixed solution of 1200 grams of normal hexane and acetonitrile (mass ratio 5:1) (the amount of mixed solvent is 4 times of...

Embodiment 3

[0032] This example is used to illustrate a method for purifying lithium bisoxalate borate disclosed by the present invention.

[0033]First, the purity is 300 grams of bisoxalate lithium borate crude product (purity 97%, moisture 0.5%) and 1500 grams of tetrahydrofuran (THF) are mixed and dissolved and filtered, and the filtrate is transferred to the reaction flask, and then 117 grams of methyl chloroformate ( The molar ratio with water is 15:1), after the dropwise addition is completed, it is heated to 66° C., and the temperature is lowered after stirring for 5 hours. Cool down and add toluene at 390 grams, filter to obtain a solid semi-finished product and transfer it to a crystallization bottle, add a mixed solution of 1800 grams of toluene and tetrahydrofuran (mass ratio 15:1) (the amount of mixed solvent is 6 times the weight of the crude product of lithium bisoxalate borate), and heat To the reflux state, keep reflux for 6 hours and then cool down, let it slowly crystal...

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Abstract

The invention discloses a purification method of lithium bis(oxalato)borate and the lithium bis(oxalato)borate, wherein the purification method comprises the steps: dissolving a lithium bis(oxalato)borate crude product in an organic solvent, and filtering to remove insoluble substances after the lithium bis(oxalato)borate crude product is completely dissolved; putting the filtered filtrate into areaction bottle, calculating the moisture content in the filtrate according to the moisture content in the lithium bis(oxalato)borate crude product and the dilution ratio after dissolution; then adding acyl chloride or thionyl chloride compounds in a certain proportion; after addition of the acyl chloride or thionyl chloride compound is finished, heating the mixture to any temperature between 35 DEG C and 70 DEG C; carrying out a heating reaction for any time between 3 hours and 9 hours; evaporating the reaction solution under reduced pressure to remove the solvent to obtain a semi-finished product, and recrystallizing the semi-finished product by using a mixed solvent to finally obtain the electronic-grade lithium bis(oxalate)borate of which the purity is more than 99.9 percent, the watercontent is less than 50 ppm, the acid value is less than 10 ppm, and the contents of potassium ions, sodium ions, calcium ions, magnesium ions and the like are all less than 10 ppm. The method has the beneficial effect of reducing water residue and impurity content.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolytes, and in particular relates to a method for purifying lithium bisoxalate borate and the lithium bisoxalate borate obtained by using the method. Background technique [0002] With the continuous expansion of the use of lithium-ion batteries, the technology of lithium-ion batteries is also improving. Adding some additives to the electrolyte as the "blood" of lithium-ion batteries can improve many performances of the battery. Lithium bisoxalate borate is a new type of lithium salt with excellent performance at low and high temperatures. It has excellent electrical conductivity and good film-forming performance. Due to its stability at high temperatures, it can also be used as a The solid polymer electrolyte monomer has great commercial application prospects and research value. At present, the process of preparing lithium bisoxalate borate will cause high water content, becaus...

Claims

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Application Information

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IPC IPC(8): C07F5/02H01M10/0567
CPCC07F5/022H01M10/0567H01M2300/0025Y02E60/10
Inventor 吴国栋曹娜张丽亚滕斌
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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