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Method for detecting content of ethylene sulfate in mixed solution suitable for chemical synthesis

A vinyl sulfate and mixed solution technology, applied in the direction of measuring devices, scientific instruments, instruments, etc., can solve the problems of inability to achieve accurate determination and quality control of vinyl sulfate content, low accuracy, complicated operation, etc., and achieve linear stability , high accuracy and good repeatability

Inactive Publication Date: 2022-03-08
江苏瀚康新材料有限公司
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Problems solved by technology

[0004] The object of the present invention is to provide the content detection method that is applicable to the vinyl sulfate ester in the mixed solution of chemical synthesis, to solve the above-mentioned background technology and propose existing most detection methods operation complexity and accurate determination are not high, can not realize in the mixed solution Problems of Accurate Determination and Quality Control of Vinyl Sulfate Content

Method used

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  • Method for detecting content of ethylene sulfate in mixed solution suitable for chemical synthesis
  • Method for detecting content of ethylene sulfate in mixed solution suitable for chemical synthesis
  • Method for detecting content of ethylene sulfate in mixed solution suitable for chemical synthesis

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Embodiment

[0032] Instrument and chromatographic conditions: Shimadzu GC2010plus gas chromatograph, capillary column model: HP-5, specification: 30m×0.32mm×0.25μm; analytical balance (accurate to 0.0001g);

[0033] Temperature: inlet temperature: 250°C; detector temperature: 270°C;

[0034] Programmed temperature rise: initial temperature 80°C, hold for 4 minutes, increase temperature to 230°C at 15°C / min, hold for 5 minutes

[0035] Column flow: 1.0mL / min; Split ratio: 39:1; Injection volume: 0.4uL

[0036] Reagent:

[0037] Ethyl methyl carbonate: main content ≥ 99.97%, moisture content less than 20ppm (electronic grade);

[0038] Ethylene carbonate (internal standard): main content ≥ 99.99%, moisture content less than 50ppm (electronic grade);

[0039] Vinyl sulfate: (main content ≥ 99.50%), packed in a glove box and sealed tightly, then taken out for later use.

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Abstract

The invention discloses a method for detecting the content of ethylene sulfate in a mixed solution suitable for chemical synthesis, which comprises the following steps: S1, preparation of an ethylene sulfate standard sample, namely preparation of a standard curve sample: accurately weighing 1.8 g of ethylene sulfate sample, 2.7 g of ethylene sulfate sample and 3.6 g of ethylene sulfate sample in a preparation bottle respectively, diluting the ethylene sulfate sample to 18g by using ethyl methyl carbonate respectively, and adding the standard curve sample; respectively adding 2g of ethylene carbonate into each preparation bottle as an internal standard substance, and sufficiently and uniformly mixing to prepare standard samples with different concentrations, which contain 9%, 13.5% and 18% of ethylene sulfate internal standard substances and 10% of ethylene carbonate internal standard substances, for later use. The detection method provided by the invention has the advantages of simple operation, good repeatability, high accuracy and linear stability, and is suitable for accurate determination and quality control of the content of ethylene sulfate in the 10-20% ethylene sulfate-ethyl methyl carbonate mixed solution.

Description

technical field [0001] The invention relates to the technical field of additive analysis and testing of lithium ion batteries, in particular to a method for detecting the content of vinyl sulfate in a mixed solution suitable for chemical synthesis. Background technique [0002] Vinyl sulfate is a kind of lithium battery electrolyte additive. The main function of vinyl sulfate in lithium batteries is to inhibit the decline of the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after high temperature storage, and improve the charge and discharge performance and cycle times of the battery. And this is formulated into a mixed solution (concentration controlled at 10% to 20%) after being directly synthesized according to the technological route, which can be stored at normal temperature, convenient for transportation, and convenient for quality control. [0003] Most of the existing detection methods are complex in op...

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Application Information

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IPC IPC(8): G01N30/02G01N30/04
CPCG01N30/02G01N30/04G01N2030/045
Inventor 张正洪曹国华姜飞翟涛陈群孙西船
Owner 江苏瀚康新材料有限公司
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