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A kind of method that prepares specific lithium salt with organoacyloxysilane

A technology of organic acyloxysilane and lithium salt is applied in the field of preparing lithium difluorooxalate borate and lithium tetrafluorooxalate phosphate, which can solve the problem of high chlorine and water content, and achieve the effects of high yield and simple operation.

Active Publication Date: 2022-06-28
武汉海斯普林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a method for preparing specific lithium salts with organic acyloxysilane, aiming to overcome the high content of chlorine and water in the products in the prior art for the preparation of lithium difluorooxalate borate and lithium tetrafluorooxalate phosphate, which cannot meet industry standards Insufficient requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing lithium difluorooxalate borate with organic acyloxysilane, comprising the steps of:

[0026] Take a three-necked round-bottomed flask and place it on a magnetic stirrer, and install a nitrogen inlet tube, a thermometer, and a water separator (followed by a reflux condenser and a drying tube). Add a magnetic stir bar. Feed nitrogen to replace the air in the system, then add 176g (1mol) dimethyl diacetoxysilane and 90g (1mol) oxalic acid, start heating after the crystals are dissolved, and slowly heat up to 130 ° C, the reaction process continues to have colorless The transparent liquid (acetic acid) enters the water separator. After the liquid in the water separator does not increase significantly, the reaction is continued for 0.5h, and the total reaction time is about 10h. Stop heating, increase nitrogen purging, change the water separator part of the device to a vacuum distillation device, then replace the nitrogen conduit with a glass plug, re...

Embodiment 2

[0030] A method for preparing lithium tetrafluorooxalate phosphate with organic acyloxysilane, comprising the steps:

[0031] Take a three-necked round-bottomed flask and place it on a magnetic stirrer, and install a nitrogen inlet tube, a thermometer, and a water separator (followed by a reflux condenser and a drying tube). Add a magnetic stir bar. Feed nitrogen to replace the air in the system, then add 176g (1mol) dimethyl diacetoxysilane and 100.2g (1.11mol) oxalic acid, start heating after the crystals are dissolved, and slowly heat up to 140 ° C, there are constant reactions during the reaction. The colorless and transparent liquid (acetic acid) enters the water separator. After the liquid in the water separator does not increase significantly, the reaction is continued for 0.5h, and the total reaction time is about 8h. Stop heating, increase nitrogen purging, change the water separator part of the device to a vacuum distillation device, then replace the nitrogen condui...

Embodiment 3

[0035] A method for preparing lithium difluorooxalate borate with organic acyloxysilane, comprising the steps of:

[0036] Take a three-necked round-bottomed flask and place it on a magnetic stirrer, and install a nitrogen inlet tube, a thermometer, and a water separator (followed by a reflux condenser and a drying tube). Add a magnetic stir bar. Feed nitrogen to replace the air in the system, then add 176g (1mol) dimethyl diacetoxysilane and 81.9g (0.91mol) oxalic acid, start heating after the crystals are dissolved, and slowly heat up to 140 ° C, there are constant reactions during the reaction. The colorless and transparent liquid (acetic acid) enters the water separator. After the liquid in the water separator does not increase significantly, the reaction is continued for 0.5h, and the total reaction time is about 10h. Stop heating, increase nitrogen purging, change the water separator part of the device to a vacuum distillation device, then replace the nitrogen conduit w...

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Abstract

The invention relates to a method for preparing a specific lithium salt with an organic acyloxysilane, which comprises the following steps: (1) transesterification and polymerization of an organic acyloxysilane and oxalic acid to obtain polysilyl oxalate; (2) ) react polysilyl oxalate with lithium tetrafluoroborate or lithium hexafluorophosphate in a solvent to obtain the corresponding crude product of lithium difluorooxalate borate or crude product of lithium tetrafluorooxalate phosphate; After drying the solvent, the corresponding battery-grade lithium difluorooxalate borate or battery-grade lithium tetrafluorooxalate phosphate can be obtained. The present invention has the advantages of using organic acyloxysilane as a raw material, no additional introduction of chloride ions and water in the reaction, simple operation, high yield, and extremely low chlorine content in the target product (about 1mg / kg), which is a suitable Industrialized production is a preparation method that can meet the market's demand for the output and quality of lithium difluorooxalate borate and lithium tetrafluorooxalate phosphate.

Description

technical field [0001] The invention belongs to the field of lithium battery electrolyte preparation, and relates to a method for preparing specific lithium salts by using organic acyloxysilanes, in particular to preparing lithium difluorooxalate borate and lithium tetrafluorooxalate phosphate by using polysilyl oxalate. Background technique [0002] Lithium batteries have the characteristics of small size, light weight, large capacity, no pollution, high energy density, low self-discharge rate, etc., and are recognized as high-end and new battery products. According to survey statistics, the global lithium-ion battery market output in 2018 increased by 21.81% year-on-year, reaching 188.80GWh, with a compound annual growth rate of 27.12% in the past five years. Due to the needs of environmental protection and the support of national policies, the new energy vehicle industry is booming, and the proportion of power batteries has risen to 28.26%, becoming an important part of l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02C07F9/6574
CPCC07F5/022C07F9/65742
Inventor 周永妍熊伟陈丹王文郭春花周国武
Owner 武汉海斯普林科技发展有限公司