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Method for synthesizing and purifying lithium bis(oxalato)borate

A bisoxalate lithium borate and synthesis method technology, which is applied in the field of synthesis and purification of bisoxalate lithium borate, can solve the problems of long time consumption and difficulty in industrial production, and achieve the effects of convenient operation and control, low cost and high yield

Active Publication Date: 2015-03-25
BLUE OCEAN & BLACK STONE TECH CO LTD BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Further, the present invention also solves the technical problems that the existing method for purifying lithium bisoxalate borate takes a long time and is not easy for industrial production, and provides a method for purifying lithium bisoxalate borate

Method used

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  • Method for synthesizing and purifying lithium bis(oxalato)borate
  • Method for synthesizing and purifying lithium bis(oxalato)borate
  • Method for synthesizing and purifying lithium bis(oxalato)borate

Examples

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Embodiment 1

[0027] Example 1: A method for synthesizing lithium bisoxalate borate, comprising the following steps: dispersing 63.04g of oxalic acid, 11.97g of lithium hydroxide and 30.92g of boric acid in 300mL of xylene, adding 200g of zirconium beads, fully ball milling and mixing for 3 h at normal temperature and pressure . After the reaction, the solution was filtered with suction, and the obtained solid mixture was placed in a vacuum drying oven, and the temperature was gradually raised to 120° C. for 8 h to obtain 53.4 g of a crude product.

[0028] Further, for the purification method of lithium bisoxalate borate, dissolve the above-mentioned crude product in 500mL acetone to saturation, filter to remove insoluble matter and zirconium beads; At this time, a large number of crystals were precipitated in the bottle; the solution after atmospheric distillation was suction-filtered, and the crystals were washed with cyclohexane for 3 times, and the crystals were dried in a vacuum env...

Embodiment 2

[0029] Example 2: A method for synthesizing lithium bisoxalate borate, comprising the following steps: dispersing 31.52g of oxalic acid, 5.99g of lithium hydroxide and 15.46g of boric acid in 150mL of benzene, adding 150g of zirconium beads, and fully ball milling and mixing for 5 hours at normal temperature and pressure. After the reaction, the solution was filtered with suction, the obtained solid mixture was placed in a vacuum drying oven, the temperature was raised to 120°C step by step, and after drying for 12 hours, 27.8 g of crude product was obtained.

[0030] Further, for the above method of purifying lithium bisoxalate borate, dissolve the crude product in 250mL of acetonitrile to saturation, filter to remove insoluble matter and zirconium beads; then add benzene to the saturated solution until precipitation occurs, and distill out acetonitrile under reduced pressure. A large number of crystals were precipitated in the bottle; the solution after vacuum distillation ...

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Abstract

The invention provides a method for synthesizing and purifying lithium bis(oxalato)borate. The method comprises the following steps: by taking a lithium source compound, a boron compound and an oxalic acid compound as main raw materials, reacting, carrying out sucking filtration and vacuum drying by using a solid-liquid phase combination method, thereby preparing a crude lithium bis(oxalato)borate product; and effectively purifying the crude product with the synthetic cooperation of a solvent-out crystallization method and a thermal crystallization method, thereby preparing high-purity lithium bis(oxalato)borate. The method has the advantages that the synthesis yield is high, the purity of the prepared product is high, the process is simple, the operation and the control are convenient and the cost is low, can be used in large-scale production and is applicable to industrialization.

Description

technical field [0001] The invention belongs to the technical field of lithium ions, especially lithium borate batteries, and in particular relates to a method for synthesizing and purifying lithium bisoxalate borate. Background technique [0002] Lithium-ion batteries are particularly suitable for use in electronic devices due to their high energy density and power density. Lithium-ion batteries are generally divided into non-rechargeable lithium primary batteries containing a small amount of lithium metal anode and rechargeable lead-acid batteries. These two types of battery packs contain liquid or gel conductive particle electrolytes, and their conductive salts include LiPF6, LiBF4, methyllithium, imidelithium, or lithium borates (such as lithium bisoxalate borate LiBOB), etc. These conductive Salts are all present in dissolved form. [0003] The electrolyte is an important part of the lithium battery, its performance directly affects the capacity of the battery, and ...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 李强郭大京杜夕彦罗贺斌
Owner BLUE OCEAN & BLACK STONE TECH CO LTD BEIJING
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