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Detection method of impurities in lithium hexafluorophosphate

A lithium hexafluorophosphate and detection method technology, applied in the field of chemical analysis, can solve the problems of few qualitative and quantitative reports

Active Publication Date: 2019-04-02
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Impurities such as phosphorus oxyfluoride and phosphorus fluoride are mainly introduced by lithium salts in the electrolyte, and there are few qualitative and quantitative reports on these impurities in lithium salts

Method used

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  • Detection method of impurities in lithium hexafluorophosphate
  • Detection method of impurities in lithium hexafluorophosphate
  • Detection method of impurities in lithium hexafluorophosphate

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0050] The present embodiment detects lithium hexafluorophosphate impurity qualitative and quantitative method, comprises the following steps:

[0051] (1) deuterated solvent pretreatment;

[0052] In a nitrogen-filled glove box, the deuterated acetonitrile was dehydrated by molecular sieves to within 10 μg / g (the moisture content was tested by a Karl Fischer moisture meter).

[0053] (2) Calibration

[0054] A coaxial NMR tube is used, and a deuterated acetonitrile solution of hexafluorobenzene and a deuterated acetonitrile solution of lithium hexafluorophosphate with a concentration of 200 μg / g are respectively added to the inner and outer tubes for fluorine spectrum detection; figure 1 shown.

[0055] The deuterated acetonitrile solution of phosphoric acid and the deuterated acetonitrile solution of lithium hexafluorophosphate with a concentration of 1000 μg / g were respectively added into the inner and outer tubes for phosphorus spectrum detection; figure 2 shown.

[0...

Embodiment 2

[0079] The present embodiment detects lithium hexafluorophosphate impurity qualitative and quantitative method, comprises the following steps:

[0080] (1) deuterated solvent pretreatment;

[0081] In a nitrogen-filled glove box, the deuterated acetone was refluxed with calcium hydride to remove water to within 10 μg / g (the moisture content was tested by a Karl Fischer moisture meter).

[0082] (2) Calibration

[0083] A coaxial nuclear magnetic tube is used, and a deuterated acetone solution of hexafluorobenzene and a deuterated acetone solution of lithium hexafluorophosphate with a concentration of 200 μg / g are respectively added to the inner and outer tubes for fluorine spectrum detection;

[0084] The deuterated acetone solution of phosphoric acid and the deuterated acetone solution of lithium hexafluorophosphate with a concentration of 1000 μg / g were respectively added to the inner and outer tubes for phosphorus spectrum detection;

[0085] (3) Lithium hexafluorophospha...

Embodiment 3

[0089] The present embodiment detects lithium hexafluorophosphate impurity qualitative and quantitative method, comprises the following steps:

[0090] (1) deuterated solvent pretreatment;

[0091] In a nitrogen-filled glove box, the deuterated dimethyl sulfoxide was dehydrated by molecular sieves to within 10 μg / g (the moisture content was tested by a Karl Fischer moisture meter).

[0092] (2) Calibration

[0093] A coaxial NMR tube is used, and a deuterated dimethyl sulfoxide solution of hexafluorobenzene and a deuterated dimethyl sulfoxide solution of lithium hexafluorophosphate are added to the inner and outer tubes with a concentration of 200 μg / g, respectively, for fluorine spectrum detection;

[0094] A coaxial nuclear magnetic tube is used, and a deuterated dimethyl sulfoxide solution of phosphoric acid and a deuterated dimethyl sulfoxide solution of lithium hexafluorophosphate are added to the inner and outer tubes with a concentration of 1000 μg / g, respectively, for...

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Abstract

The invention discloses a method for detecting impurities in lithium hexafluorophosphate. The method includes steps of (1), carrying out calibration, to be more specific, adding deuterated reagent solution of hexafluorobenzene and deuterated reagent solution of the lithium hexafluorophosphate into inner and outer tubes of coaxial nuclear magnetic tubes, carrying out fluorine spectrum detection, adding deuterated reagent solution of phosphoric acid and deuterated reagent solution of the lithium hexafluorophosphate into the inner and outer tubes of the coaxial nuclear magnetic tubes and carrying out phosphorus spectrum detection; (2), carrying out measurement, to be more specific, preparing to-be-detected samples with certain concentration from the lithium hexafluorophosphate and deuterated reagents and carrying out fluorine spectrum and phosphorus spectrum detection by the aid of nuclear magnetic resonators. Compared with the traditional method, the method has the advantages that the fluorine-containing and phosphorus-containing impurities in the lithium hexafluorophosphate can be qualitatively and quantitatively detected by the aid of the method, and the method is short in analysis time, easy to implement and high in sensitivity, equipment can be prevented from being damaged by fluorine-containing strong corrosive substances, and the like.

Description

technical field [0001] The invention relates to a chemical analysis method, in particular to a method for detecting fluorine-containing and phosphorus-containing impurities in lithium hexafluorophosphate. Background technique [0002] Lithium-ion battery is a green, high-energy and environment-friendly battery that appeared in the 1990s. It has been widely used in portable electronic products, power tools, electric bicycles and other fields. Among them, the organic electrolyte is an important part of the lithium-ion battery. It is responsible for the transfer of charges between the positive and negative electrodes in the battery. Therefore, the type and content of impurities in the electrolyte directly affect the usability and safety of the battery. [0003] Impurities that generally affect battery performance are: water and hydrofluoric acid, impurity metal ions, substances containing oxidation or reduction, and organic substances containing active hydrogen. At present, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 罗海英孙伏恩丁友婷
Owner GUANGZHOU TINCI MATERIALS TECH
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