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Sample pretreatment method for determining content of chloride ions in lithium ion battery electrolyte

A chlorine ion content, lithium-ion battery technology, applied in the field of lithium-ion batteries, can solve the problems of ion chromatography instrument system damage, impact on test accuracy, instrument life, etc., to achieve small human error, good reproducibility, and fast analysis Effect

Inactive Publication Date: 2021-01-05
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the electrolyte is an organic solution, which contains a relatively high content of ester compounds, these organic solvents will cause damage to the ion chromatography instrument system, affect the test accuracy and instrument life, so it is necessary to perform sample pretreatment on the electrolyte, and it is suitable The pretreatment method is very important for the accurate determination of chloride ion using ion chromatography

Method used

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  • Sample pretreatment method for determining content of chloride ions in lithium ion battery electrolyte
  • Sample pretreatment method for determining content of chloride ions in lithium ion battery electrolyte

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Embodiment 1

[0013] 1. Instruments and equipment

[0014] AQUION ion chromatograph (Thermo Fisher, USA), adjustable electric heating plate, UPR-10T ultra-pure water machine (Xi’an Youpu), electronic balance of 1 / 10,000 (Mettler Toledo), AS22 4×250mm ion Separation column, 0.22μm organic filter membrane, 0.22μm organic syringe filter, 10ml disposable syringe, nitrogen 99.999%.

[0015] 2. Reagents and solutions

[0016] (1) nitric acid, excellent grade pure (68-70%) Sinopharm Chemical Reagent (Shanghai); (2) Na 2 CO 3 (excellent grade), NaHCO 3 (Excellent pure), Aladdin chemical reagent; (3) Chloride ion standard solution: 1000ug / ml, Beijing Institute of Nonferrous Metals; (4) Deionized water, resistivity ≥ 18 megohm.cm; (5) Hydrogen peroxide (excellent grade pure) Aladdin Chemical Reagent.

[0017] 3. Standard solution preparation

[0018] Chloride ion standard solution: Use the deionized water stepwise dilution method to prepare 1000ug / ml chloride ion standard product with concentra...

Embodiment 2

[0034] A sample pretreatment method for measuring chloride ion content in lithium-ion battery electrolyte comprises the following steps:

[0035] (1) Add 25ml of 17% sodium carbonate aqueous solution and place it in a glass separatory funnel.

[0036] (2) Pipette 20 ml of the electrolyte sample and place it in a glass separatory funnel filled with 17% sodium carbonate aqueous solution for thorough mixing.

[0037] (3) After the electrolyte sample is mixed with the sodium carbonate solution, remove the organic phase, move the aqueous solution containing sodium carbonate into a 100ml glass volumetric flask, use deionized water to constant volume, and the solution after constant volume is used as the sample to be tested .

[0038] (4) Use a 0.22 μm nylon filter membrane to filter the sample to be tested, and the filtrate sample solution needs to be properly diluted, and then analyzed by an ion chromatograph.

Embodiment 3

[0040] A sample pretreatment method for measuring chloride ion content in lithium-ion battery electrolyte comprises the following steps:

[0041] (1) Add 25ml of 22% sodium carbonate aqueous solution and place in a glass separatory funnel.

[0042] (2) Pipette 40ml of the electrolyte sample and place it in a glass separatory funnel filled with 22% sodium carbonate aqueous solution for thorough mixing.

[0043] (3) After the electrolyte sample is mixed with the sodium carbonate solution, remove the organic phase, move the aqueous solution containing sodium carbonate into a 100ml glass volumetric flask, use deionized water to constant volume, and the solution after constant volume is used as the sample to be tested .

[0044] (4) Use a 0.22 μm nylon filter membrane to filter the sample to be tested, and the filtrate sample solution needs to be properly diluted, and then analyzed by an ion chromatograph.

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Abstract

The invention discloses a sample pretreatment method for determining the content of chloride ions in a lithium ion battery electrolyte, and relates to the technical field of lithium ion batteries. Thesample pretreatment method comprises the steps of adding an electrolyte sample into a sodium carbonate aqueous solution, extracting, separating liquid, removing an organic phase, and retaining a water phase; and filtering and diluting the water phase, and analyzing by using an ion chromatograph. According to the method, the sodium carbonate aqueous solution is adopted to extract chloride ions inthe electrolyte, the chloride ions can completely enter the water phase, and then the organic phase in the electrolyte is removed, so that an organic solvent is prevented from being directly contactedwith an ion chromatographic column and an anion suppressor for a long time to damage the ion chromatographic column and the anion suppressor. According to the method, the electrolyte sample is accurately detected and qualitatively analyzed by ion chromatography after being pretreated, the analysis is fast, the manual operation error is small, the reproducibility is good, and the method is particularly suitable for measuring the content of chloride ions in the electrolyte.

Description

technical field [0001] The invention relates to the technical field of lithium-ion batteries, in particular to a sample pretreatment method for measuring the content of chloride ions in electrolytes of lithium-ion batteries. Background technique [0002] Lithium-ion batteries are widely used due to their advantages of high energy density, high voltage and long cycle life, while lithium-ion batteries used in the commercial automotive industry need to further improve their energy density and safety. Electrolyte is an important part of lithium-ion batteries. It is a mixed solution composed of solvents, additives, and lithium salts. Among them, the solvents are mainly chain and cyclic carbonate compounds, which will introduce chloride ions during industrial production. kinds of impurities. Chloride ions in lithium-ion batteries will corrode the positive and negative electrode materials of the battery, seriously affect the performance of the battery, and cause battery damage. T...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/96
CPCG01N30/02G01N30/06G01N30/14G01N30/96G01N2030/062G01N2030/146
Inventor 李涛张峥胡淑婉
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY