Synthesis technique for obtaining difluoro oxalate lithium borate and di-oxalate lithium borate

A technology of lithium difluorooxalate borate and lithium bisoxalate borate, which is applied in the field of synthetic technology for simultaneously obtaining lithium difluorooxalate borate and lithium bisoxalate borate, can solve the problems of limited research, high equipment requirements, unfavorable industrial production, difluorooxalate Lithium borate is developed late and other issues, to achieve the effect of simple process

Active Publication Date: 2010-02-10
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The aqueous phase synthesis is LiBOB synthesized in water with lithium hydroxide, oxalic acid, and boric acid. This method involves high temperature and oxalic acid aqueous solution requires extremely high equipment; 3 ) 3 with (CH 3 ) 3 SiOOCCOOSi (CH 3 ) 3 Synthetic, but the raw material price of this method is expensive and not suitable for industrial production; the solid-phase method is synthesized with lithium hydroxide, oxalic acid, and boric acid after being evenly ground and generated at a high temperature. This method requires high equipment requirements as the water-phase method.
[0010] Lithium difluo

Method used

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  • Synthesis technique for obtaining difluoro oxalate lithium borate and di-oxalate lithium borate
  • Synthesis technique for obtaining difluoro oxalate lithium borate and di-oxalate lithium borate
  • Synthesis technique for obtaining difluoro oxalate lithium borate and di-oxalate lithium borate

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Experimental program
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Effect test

Embodiment 1

[0024] Using boron trifluoride ether solution and lithium oxalate as raw materials to prepare lithium difluorooxalate borate and lithium bisoxalate borate.

[0025] Step 1. Add 101.9g of lithium oxalate dried at 150°C for 10h into a dry reaction vessel equipped with a magnetic stirrer and a thermometer, add 500g of dimethyl carbonate and stir, and slowly add 94.5g of boron trifluoride ether solution dropwise, while Heat and stir the reaction while adding dropwise, the addition is completed in 2 hours, the reaction temperature is adjusted to 80°C for 24 hours, and the reaction produces lithium difluorooxalate borate soluble in dimethyl carbonate and lithium bisoxalate borate insoluble in dimethyl carbonate and fluorine Lithium, then cooled to room temperature.

[0026] Step 2, filter the reacted mixture at normal temperature to remove unreacted lithium oxalate and lithium fluoride and lithium bisoxalate borate generated after the reaction, extract the lithium bisoxalate borate ...

Embodiment 2

[0030] Lithium difluorooxalate borate and lithium bisoxalate borate were prepared by using fluoboric acid, oxalic acid and lithium carbonate as raw materials.

[0031] Step 1. In a reactor equipped with a magnetic stirrer, add 136g of oxalic acid and 160g of fluoboric acid to 300g of acetonitrile and stir until the emulsion is dissolved, then slowly add 295g of lithium carbonate, and stir the reaction while adding. When no gas appeared, the reaction was continued for 5 hours to obtain lithium difluorooxalate borate, lithium bisoxalate borate solution and lithium fluoride.

[0032] Step 2, filter the reaction mixture at room temperature to remove unreacted lithium oxalate and lithium fluoride generated after the reaction, evaporate the solution to solids on a rotary evaporator, and extract the difluorine in the solids with diethyl carbonate several times Lithium oxalate borate, concentrated under reduced pressure, crystallized by cooling with diethyl carbonate, and recrystalliz...

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Abstract

The invention discloses a synthesis technique for simultaneously obtaining difluoro oxalate lithium borate and di-oxalate lithium borate with outstanding performances, comprising the following steps:1. reacting fluorinated compound, boracic compound, lithium-containing compound and oxalate-containing compound in a reaction medium at 100 DEG C with reaction pressure of 0.1-1MPa, wherein the mol ratio of lithium, fluorine, boron and oxalate ions is 5-9:5-9:-2-3:3-4, and generating a reaction solution containing difluoro oxalate lithium borate and di-oxalate lithium borate; 2. carrying out initial separation on the difluoro oxalate lithium borate and di-oxalate lithium borate in the reaction solution, then carrying out further extraction separation by using organic solvent capable of extracting difluoro oxalate lithium borate or di-oxalate lithium borate; and 3. respectively carrying out recrystallization and vacuum drying to obtain the difluoro oxalate lithium borate and di-oxalate lithium borate of battery level. The invention is suitable for industrially producing two types of lithium salts with excellent performance used for lithium ion batteries.

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 bisoxalate borate. Background technique [0002] As the main component of lithium-ion batteries, electrolyte has always been one of the research focuses in this technical field. LiPF currently in commercial large-scale application 6 Insufficient thermal stability, easy to decompose into LiF and PF 5 , the latter is readily hydrolyzed to form HF and PF 3 O. These two hydrolysis products have high reactivity for both positive and negative electrodes, and they inevitably exist in LiPF 6 have a detrimental effect on the performance of the electrode. LiAsF 6 Due to its high toxicity due to its arsenic content, large-scale use is not advocated. LiClO 4 It is a strong oxidant, easy to explode, and poor in safety. LiBF 4 Poor ...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 何永刚钱晓兵陈剑徐晓强陈晓荣陶荣辉李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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