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Synthesizing process for obtaining lithium difluoro-oxalato-borate and lithium tetrafluoroborate

A technology of lithium difluorooxalate borate and lithium tetrafluoroborate, which is applied in the field of synthesis technology for obtaining lithium difluorooxalate borate and lithium tetrafluoroborate at the same time, can solve the problems of high equipment requirements and unfavorable industrial production, and achieve the effect of simple process

Inactive Publication Date: 2010-02-17
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In European Patent No., the following method is disclosed in the document of EP1308449A2: react in dimethyl carbonate with oxalic acid, lithium tetrafluoroborate and aluminum chloride or silicon tetrachloride or react with oxalic acid, lithium tetrafluoroborate, lithium fluoride and The reaction of boron trichloride or trimethoxyboron in dimethyl carbonate realizes the synthesis of LiODFB, but HCl is produced in the reaction of this method and the reaction is violent, which requires high equipment requirements and is not conducive to industrial production.

Method used

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  • Synthesizing process for obtaining lithium difluoro-oxalato-borate and lithium tetrafluoroborate
  • Synthesizing process for obtaining lithium difluoro-oxalato-borate and lithium tetrafluoroborate
  • Synthesizing process for obtaining lithium difluoro-oxalato-borate and lithium tetrafluoroborate

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Embodiment 1

[0022] Using boron trifluoride ether solution and lithium oxalate as raw materials to prepare lithium difluorooxalate borate and lithium tetrafluoroborate.

[0023] Step 1. Add 500g of diethyl carbonate and 101.9g of lithium oxalate dried at 150°C for 10 hours into a dry reaction vessel equipped with a magnetic stirrer and a thermometer, stir to form an emulsion, slowly add 286g of boron trifluoride ether, and react The temperature was adjusted to 80° C. for 24 hours to react to form lithium difluorooxalate borate and lithium tetrafluoroborate, and then cooled to room temperature.

[0024] Step 2: Filtrate to obtain solid lithium difluorooxalate borate and a filtrate containing lithium tetrafluoroborate, extract the solid lithium difluorooxalate borate with ethyl acetate, concentrate under reduced pressure with ethyl acetate, cool and crystallize with ethyl acetate, and recrystallize. At the same time, the filtrate containing lithium tetrafluoroborate was concentrated under re...

Embodiment 2

[0028] Using boric acid, oxalic acid, hydrofluoric acid and lithium carbonate as raw materials to prepare lithium difluorooxalate borate and lithium tetrafluoroborate.

[0029] Step 1. Add 300g of hydrofluoric acid (weight concentration: 48%), 123g of boric acid and 90g of oxalic acid in a tetrafluoro reactor equipped with a magnetic stirrer, and control the temperature at about 0°C. After stirring until all are dissolved, slowly add 125g of carbonic acid Stir the lithium to react and release gas while keeping the temperature below 10°C, and continue stirring for 3 hours after no gas is released.

[0030] Step 2, filtering off unreacted lithium carbonate and lithium fluoride, and evaporating the solvent from the filtrate at 0.1Mpa to obtain a white solid. Dissolve the white solid with dimethyl carbonate to a light yellow clear liquid, concentrate and filter to obtain a dimethyl carbonate solution of lithium difluorooxalate borate crystals and lithium tetrafluoroborate. Extrac...

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Abstract

The invention discloses a synthesizing process for simultaneously obtaining lithium difluoro-oxalato-borate and lithium tetrafluoroborate with favorable performance, which comprises the following steps: (1) leading a fluorine-contained compound, a boron-contained compound, a lithium-contained compound and an oxalate-contained compound to react in a reaction medium at the reaction pressure of 0.1-1MPa and the temperature of 0-100 DEG C, wherein the molar ratio of lithium element, fluorine element, boron element and oxalate ion is (2-3):(5-6):6:2:1; generating reaction liquid containing the lithium difluoro-oxalato-borate and the lithium tetrafluoroborate; (2) carrying out initial separation on the lithium difluoro-oxalato-borate and the lithium tetrafluoroborate in the reaction liquid and then carrying out further extraction separation by an organic solvent which can extract the lithium difluoro-oxalato-borate or the lithium tetrafluoroborate; and (3) respectively carrying out recrystallization and vacuum drying to obtain the battery-grade lithium difluoro-oxalato-borate and the lithium tetrafluoroborate. The invention is suitable for industrially producing two lithium salts which have favorable performance and are used for a lithium ion battery.

Description

technical field [0001] The invention relates to the technical field of preparation of electrolyte salts used in lithium ion batteries, in particular to a synthesis process capable of simultaneously obtaining lithium difluorooxalate borate and lithium tetrafluoroborate. Background technique [0002] Lithium difluorooxalate borate, a lithium salt that can be used in lithium-ion batteries, has a unique chemical structure that combines the advantages of lithium bisoxalate borate and lithium tetrafluoroborate, making it have better high and low temperature performance. It can be seen that lithium bisoxalate borate, lithium difluorooxalate borate and lithium tetrafluoroborate all have relatively excellent properties. Although they have similar structures, the synthetic routes are completely different processes, and the required equipment is also very different, and the cost of producing any one of them is very high. [0003] Lithium tetrafluoroborate (LiBF 4 ) has the following ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02C01B35/06
Inventor 何永刚钱晓兵陈剑徐晓强陈晓荣陶荣辉李建中
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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