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Preparation method of lithium difluoro bis (oxalato) phosphate

A technology of lithium difluorobisoxalate phosphate and lithium bisoxalate phosphate, which is applied in chemical instruments and methods, phosphorus compounds, secondary batteries, etc., can solve the problems of high reaction pressure and high equipment requirements, and achieve good product quality and product yield. The effect of high efficiency and high product selectivity

Active Publication Date: 2021-12-07
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The patent CN109956976A of Dongguan Dongguangke Research and Development Co., Ltd. discloses the preparation method of phosphorus pentafluoride and lithium oxalate to prepare lithium difluorobisoxalate phosphate, but this method needs to be reacted in supercritical carbon dioxide, the reaction pressure is high, and the equipment requirements are very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In a drying room with a dew point lower than -40°C, weigh 38.0g of lithium hexafluorophosphate (0.25mol), 79.5g (0.25mol) of anhydrous aluminum oxalate (moisture content: 75ppm) that is finely ground (mesh: 800) and add it to 500ml for a three-port reaction In the bottle, 400ml of ethyl methyl carbonate (moisture content 4.2ppm) was added. Raise the temperature to 100°C and keep it warm for 16 hours, take the reaction solution to measure P 31 NMR, showed disappearance of starting material. After cooling to room temperature, use a 0.1 μm filter membrane to remove insoluble matter (mainly composed of aluminum fluoride) to obtain 460 g of ethyl methyl carbonate solution of lithium difluorobisoxalate phosphate, with a concentration of about 13.1% and a yield of 95.6%. The ion chromatograph detects that almost no chloride ion (<0.1ppm) is detected, and the acidity of the solution measured by titration is 6ppm (in HF).

Embodiment 2

[0048] In a drying room with a dew point lower than -40°C, weigh 38.0g of lithium hexafluorophosphate (0.25mol), 238.5g (0.75mol) of finely ground (mesh 600) anhydrous aluminum oxalate (moisture content 87ppm) and add it to 1000ml for a three-port reaction In the bottle, 700ml of diethyl carbonate (moisture content 3.9ppm) was added. Raise the temperature to 115°C and keep it warm for 8 hours, take the reaction solution to measure P 31 NMR, showed disappearance of starting material. After cooling to room temperature, use a 0.1 μm membrane filter to remove insoluble matter (the main component is aluminum fluoride), and use a small amount of fresh diethyl carbonate to wash the filter cake. Obtain 772g of ethyl methyl carbonate solution of lithium difluorobisoxalate phosphate, the concentration is about 7.5%, and the yield is 91.9%. After detection by ion chromatography, almost no chloride ion (<0.1ppm) is detected, and the acidity of the solution is measured by titration It is...

Embodiment 3

[0050] The operation of this example is the same as that of Example 1, the only difference being that the ethyl methyl carbonate solution obtained from lithium difluorobisoxalate phosphate is further processed to obtain a solid product of lithium difluorobisoxalate phosphate. The specific processing steps are as follows:

[0051] Heat up the ethyl methyl carbonate solution of lithium difluorobisoxalate phosphate to about 55°C and distill under reduced pressure to recover the ethyl methyl carbonate solvent, add 200ml of dry dichloromethane after evaporating most of the solvent, heat and reflux for 0.5 hours, then cool to room temperature . Vacuum drying after filtration obtains 58.1g white solid powdery lithium difluorobisoxalate phosphate, yield 92.2%, detects through ion chromatograph, almost does not detect chloride ion (<0.1ppm), records acidity through titration and is 33ppm (with HF meter), the solid product purity of lithium difluorobisoxalate phosphate is 99.3%.

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Abstract

The invention discloses a preparation method of lithium difluoro bis (oxalato) phosphate, the preparation method comprises the following step: reacting lithium hexafluorophosphate with anhydrous aluminum oxalate in an aprotic solvent to obtain the lithium difluoro bis (oxalato) phosphate, wherein the water content of the anhydrous aluminum oxalate is less than 500ppm, and the anhydrous aluminum oxalate is obtained by removing crystal water through secondary vacuum drying of aluminum oxalate. The method has the advantages of simple process, high yield, high product purity, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to a lithium ion battery electrolyte additive, in particular to a synthesis method of a lithium salt additive lithium difluorobisoxalate phosphate. Background technique [0002] The use of lithium salt containing oxalic acid structure as an additive product for lithium-ion power batteries can effectively improve the structure of the passivation film, reduce the impedance of the passivation film, and improve the stability of the positive and negative electrode structures in high and low temperature cycles. The performance of the high-nickel power battery system plays an important role, and lithium difluorobisoxalate phosphate (LiDFBP) is a typical representative thereof. [0003] When lithium difluorobisoxalate phosphate is used in lithium-ion batteries, the purity requirements are very high, especially the chloride ion concentration and acidity. In order to reduce the concentration of chloride ions in lithium difluorobisoxalate p...

Claims

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Application Information

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IPC IPC(8): C01B25/41C01B25/455H01M10/0525H01M10/0567
CPCC01B25/41C01B25/455H01M10/0567H01M10/0525Y02E60/10
Inventor 沈方烈夏旭建尚雁陈慧闯王国超
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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