Preparation process of lithium difluoro (oxalato) borate

A technology for preparing lithium difluorooxalate borate, which is applied in the fields of compounds containing group 3/13 elements of the periodic table, chemical instruments and methods, organic chemistry, etc., can solve the problem of low purity and complex preparation process of lithium difluorooxalate borate , Lithium difluorooxalate borate can not be applied on a large scale, etc., to achieve the effect of less impurities, simple purification method, and less side reactions

Inactive Publication Date: 2021-10-19
河北津宏化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the preparation process of lithium difluorooxalate borate is complicated at present, and the purity of obtained lithium difluorooxalate borate is relatively low, so lithium difluorooxalate borate cannot be applied on a large scale

Method used

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  • Preparation process of lithium difluoro (oxalato) borate
  • Preparation process of lithium difluoro (oxalato) borate
  • Preparation process of lithium difluoro (oxalato) borate

Examples

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Embodiment 1

[0045] A preparation process for lithium difluorooxalate borate, comprising the following steps:

[0046] S1, reaction, the raw material dimethyl dichlorosilane 100kg, oxalic acid 90kg, lithium tetrafluoroborate 94kg are added in the dimethyl carbonate of 500kg, react 6h, reaction equation is as shown in reaction formula (1), reaction temperature is 57 ℃;

[0047] (Me) 2 SiCl 2 +H 2 C 2 o 4 +LiBF 4 →LiBC 2 o 4 f 2 +(Me)2 SiF 2 +2HCl (1)

[0048] S11, absorb the gaseous dimethyldifluorosilane and hydrogen chloride generated by the reaction in S1, and pass it into a condenser to condense. The condensation medium is a mixture of ice and water. After the dimethyldifluorosilane is condensed into a liquid state, it is separated from the gaseous hydrogen chloride. Methyldifluorosilane and hydrogen chloride were stored separately for subsequent by-product preparation.

[0049] S2, filtering, after the material is filtered after the reaction of S1, the filtrate is obtained,...

Embodiment 2

[0066] The difference from Example 1 is that 375kg of dimethyl carbonate was evaporated in step S3 of this example.

Embodiment 3

[0068] The difference from Example 1 is that 400kg of dimethyl carbonate is evaporated in step S3 of this example.

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Abstract

The invention relates to the field of lithium battery electrolytic solution, and particularly discloses a preparation process of lithium difluoro (oxalato) borate. The preparation method comprises the following steps: adding raw materials for reaction according to a ratio of the metering number of a reaction formula (1) (Me)2SiCl2+H2C2O4+LiBF4->LiBC2O4F2+(Me)2SiF2+2HCl, and filtering after reaction; performing concentration; and crystallizing and drying to obtain the product. The preparation method provided by the invention has the advantage that the prepared lithium difluoro (oxalato) borate is high in purity.

Description

technical field [0001] This application relates to the field of lithium battery electrolyte, more specifically, it relates to a kind of preparation technology of lithium difluorooxalate borate Background technique [0002] Electrolyte is one of the key materials of lithium-ion batteries. It is called the "blood" of lithium-ion batteries. Its function is to conduct electrons between the positive and negative electrodes of the battery. It is also an important factor for lithium-ion batteries to obtain the advantages of high voltage and high specific energy. ensure. The electrolyte is generally composed of solvents, lithium salts, additives, etc., and the composition of the lithium salt plays an important role in the quality of the electrolyte. [0003] In related fields, lithium salts are often selected from lithium hexafluorophosphate (LiPF6), lithium bisoxalate borate (LiBOB), lithium tetrafluoroborate (LiBF4), lithium difluorooxalate borate (LiODFB) and the like. Among th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 刘康王宏义
Owner 河北津宏化工有限公司
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