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Method for reducing acid value of lithium bis(oxalate)borate and low-acid-value lithium bis(oxalate)borate

A technology of bisoxalate lithium borate and low acid value, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problems of limited application and reduce moisture and free acid Effects of residue, improvement of product quality, mild reaction

Inactive Publication Date: 2020-04-07
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the stringent requirements of the industry, the application of this product in the lithium-ion battery industry is partially limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 194g of bisoxalate lithium borate crude product with a water content of 260ppm and an acid value of 145ppm based on oxalic acid into a dry three-necked flask with stirring under a nitrogen atmosphere, and then add ethyl acetate with a water content of 4 times the mass and a water content of 180ppm , stirred to dissolve for 30min. Then, 19.4 g of granular anhydrous calcium chloride was added, and the mixture was stirred and reacted for 10 minutes before filtration. The filtrate was concentrated under reduced pressure, recrystallized and filtered, and vacuum dried to obtain 186 g of lithium bisoxalate borate product. The detected acid value is 12ppm, and the moisture content is 65ppm.

Embodiment 2

[0027] Add 194g of bisoxalate lithium borate crude product with a water content of 120ppm and an acid value of 86ppm in terms of oxalic acid into a dry three-necked flask with stirring under a nitrogen atmosphere, then add acetonitrile with a water content of 6 times the mass and a water content of 350 ppm, and stir Dissolve for 60min. Then 0.2 g of calcium oxide was added, and the mixture was stirred and reacted for 180 minutes before filtration. The filtrate was concentrated under reduced pressure, recrystallized and filtered, and vacuum dried to obtain 178 g of lithium bisoxalate borate product. The detected acid value was 8ppm, and the water content was 62ppm.

Embodiment 3

[0029] Add 200g of bisoxalate lithium borate crude product with 85ppm moisture and 50ppm acid value based on oxalic acid into a dry three-necked flask with stirring under a nitrogen atmosphere, then add acetone with 3 times the mass of moisture and 500ppm of moisture, and stir Dissolve for 30min. Then 10 g of calcium bicarbonate was added, and the mixture was stirred and reacted for 90 minutes before filtration. The filtrate was concentrated under reduced pressure, recrystallized and filtered, and vacuum dried to obtain 185 g of lithium bisoxalate borate product. The detected acid value was 5ppm, and the moisture content was 52ppm.

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Abstract

The invention discloses a method for reducing the acid value of lithium bis(oxalate)borate and the low-acid-value lithium bis(oxalate)borate. The method is characterized by comprising the following steps: dissolving a lithium bis(oxalate)borate crude product into a polar solvent, adding an acid chelating agent into an obtained mixture, stirring to react for 10-180 minutes, filtering, evaporating the solvent from an obtained filtrate, and drying under reduced pressure to obtain low-acid-value lithium bis(oxalate)borate; wherein the acid chelating agent is an anhydrous inorganic calcium salt. The technical scheme provided by the invention has the beneficial effects that the defect of high acid value residue of lithium bis(oxalate)borate products prepared by the conventional method is effectively solved, and the moisture and free acid residue in the products can be obviously reduced.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolytes, and in particular relates to a method for reducing the acid value of lithium bisoxalate borate and lithium bisoxalate borate with low acid value prepared by the method. 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 secondary batteries with development potential. preferred. Electrolyte is one of the basic key materials of lithium-ion batteries, and its performance plays a decisive role in electrolyte and lithium-ion batteries. Lithium bisoxalate borate (LiBOB), as a new electrolyte lithium salt, has good chemical properties and stability, and its thermal decomposition temperature can reach 300 °C. The addition of bisoxalate lithium borate (LiBOB) can form a stable SEI film on the carbon negative electrode,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/02
Inventor 杨志勇李伟锋沈鸣周立新
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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