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Method for analyzing sulfate ions in preparation process of lithium ion battery

A sulfate ion and lithium ion battery technology, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, can solve the problem of low accuracy and uncertainty of the specific value of the test results. , Organic solvents and water insoluble problems, to achieve the effect of improving accuracy

Inactive Publication Date: 2020-06-30
SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the production of lithium batteries, the turbidimetric method is usually used to test the sulfate ions of the lithium battery electrolyte and the organic solvent system, but when the visual colorimetry is used to test the sulfate ions of the lithium battery electrolyte and the organic solvent system, there are mainly the following Problems: (1) Visual colorimetry cannot determine the specific value of the test results, the data results are in a range, and the accuracy is not high; (2) Organic solvents are difficult to dissolve in water
The disadvantage is that the obtained measurement results are in a range, and the accuracy is not high

Method used

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  • Method for analyzing sulfate ions in preparation process of lithium ion battery
  • Method for analyzing sulfate ions in preparation process of lithium ion battery
  • Method for analyzing sulfate ions in preparation process of lithium ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Lithium hexafluorophosphate (LiPF 6 ) detection of sulfate ion in the electrolyte, the electrolyte consists of 54.3wt% (wt%, mass percent) of dimethyl carbonate (DMC), 7.7wt% of diethyl carbonate (DEC), 27wt% % ethylene carbonate (EC), 10wt% LiPF 6 And the vinylene carbonate of 1wt% is formulated, comprises the following steps:

[0044] 1. Instruments and reagents

[0045] (1) microburette 2ML, division value 0.01ML;

[0046] (1) One ten-thousandth balance (accurate to 0.0002g);

[0047] (2) Nitric acid solution (8+92), analytically pure;

[0048] (3) Acetic acid (glacial acetic acid), analytically pure;

[0049] (4) nitric acid, AR grade; Ammonia (mass percentage concentration is 25%), analytically pure;

[0050] (5) 100ml glass beaker, 1 glass stirring rod;

[0051] (6) Nitric acid solution (1+2000), analytically pure;

[0052] (7) ethanol (mass percentage concentration is 95%), analytically pure;

[0053] (8) Hexamethylenetetramine, analytically pure;

[0054...

Embodiment 2

[0086] Electrolyte containing lithium difluorooxalate borate (LiODFB) (by 58wt% of DMC, 27wt% of EC, 10wt% of LiPF 6 , the LiODFB of 1.5wt% and the 1.3-propane sultone of 3.5wt% are formulated) the detection of sulfate ion in, comprises the following steps:

[0087] 1. Instruments and reagents

[0088] (1) microburette 2ML, division value 0.01ML;

[0089] (2) One ten-thousandth balance (accurate to 0.0002g)

[0090] (3) Nitric acid solution (8+92), analytically pure;

[0091] (4) Acetic acid (glacial acetic acid), analytically pure;

[0092] (5) Nitric acid, AR grade; Ammonia (mass percentage concentration is 25%), analytically pure;

[0093] (6) 100ml glass beaker, 1 glass stirring rod;

[0094] (7) Nitric acid solution (1+2000), analytically pure;

[0095] (8) ethanol (mass percentage concentration is 95%), analytically pure;

[0096] (9) Hexamethylenetetramine, analytically pure;

[0097] (10) Acetone, analytically pure;

[0098] (11) Disodium ethylenediaminetetraa...

Embodiment 3

[0129] The detection of sulfate ion in solvent dimethyl carbonate comprises the following steps:

[0130] 1. Instruments and reagents

[0131] (1) microburette 2ML, division value 0.01ML;

[0132] (2) One-ten-thousandth balance (accurate to 0.0002g);

[0133] (3) Nitric acid solution (8+92), analytically pure;

[0134] (4) Acetic acid (glacial acetic acid), analytically pure;

[0135] (5) Nitric acid, AR grade; Ammonia (mass percent concentration is 25%), analytically pure

[0136] (6) 100ml glass beaker, 1 glass stirring rod;

[0137] (7) Nitric acid solution (1+2000), analytically pure;

[0138] (8) ethanol (mass percentage concentration is 95%), analytically pure;

[0139] (9) Hexamethylenetetramine, analytically pure;

[0140] (10) Acetone, analytically pure;

[0141] (11) Disodium ethylenediaminetetraacetic acid [c(EDTA)=0.05mol / L;

[0142] (12) Xylenol Orange (2g / L);

[0143] (13) Dithizone, analytically pure;

[0144] (14) Lead nitrate, analytically pure

[...

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Abstract

The invention discloses a method for analyzing sulfate ions in the preparation process of a lithium ion battery. The method comprises the following steps: adjusting the pH value of a to-be-detected sample to 7.5-8.5 by using an alkaline substance and then adding deionized water; then adding a bromophenol blue indicator until the solution becomes blue; adjusting the solution to yellow green by using a (8 + 92) nitric acid solution or a 0.2 mol / L ammonia water solution, adding an acetone acetate solution and a dithizone acetone solution until the solution is turned into treasure green, and finally titrating by using a Pb (NO3) 2 standard solution until the solution is turned into brownish red from treasure green, thereby obtaining the end point. When the method is used at an equivalent point, the color of the indicator is changed into brownish red from royal green, the color change is sensitive, trace and ultratrace sulfate radicals can be measured, and the method has the advantages of simplicity, convenience, accuracy and rapidness.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to an analysis method for sulfate ions in the preparation process of lithium ion batteries. Background technique [0002] Lithium-ion battery electrolyte is one of the four key materials of lithium-ion batteries (positive electrode, negative electrode, separator, electrolyte), and is the "blood" of lithium-ion batteries, which plays the role of transmitting current between the positive and negative electrodes of the battery. Among the currently commercialized lithium-ion battery electrolytes, liquid organic electrolytes are commonly used, and their main components are electrolyte lithium salts, organic solvents and additives. Commonly used electrolyte lithium salts include lithium hexafluorophosphate, lithium tetrafluoroborate, Commonly used solvents include dimethyl carbonate, ethylene carbonate, ethyl methyl carbonate, diethyl carbonate, etc. In solvents and lithium...

Claims

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Application Information

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IPC IPC(8): G01N21/78
CPCG01N21/78
Inventor 吴财平周小华
Owner SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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