Detection method for trace free acid in electrolyte lithium salt

A detection method, free acid 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. Long time and other problems, to achieve the effect of wide application range, simple and easy method, high accuracy of results

Inactive Publication Date: 2014-07-09
GUANGZHOU TINCI MATERIALS TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is more expensive equipment, and the detection time is longer
The industry standard HG / T4066~4067-2008 uses potentiometric titration to detect the acidity of lithium hexafluorophosphate. Due to the long titration time, the sample is unstable and easy to decompose, resulting in high results, so the accuracy of the results is not high.

Method used

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  • Detection method for trace free acid in electrolyte lithium salt
  • Detection method for trace free acid in electrolyte lithium salt
  • Detection method for trace free acid in electrolyte lithium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1, the present embodiment detects the method for the acidity of lithium hexafluorophosphate, comprises the following steps:

[0025] (1) Take 100g of deionized water at a temperature of 0°C, add 1-3 drops of bromothymol blue indicator, use 0.05mol / L sodium hydroxide as the titrant, and titrate to blue-green with a digital titrator (deduct reagent blank);

[0026] (2) Weigh 5g of lithium hexafluorophosphate, add it to the deionized water titrated in step (1), let it stand for 0min after dissolving, use 0.05mol / L sodium hydroxide as titrant, and titrate to blue-green with a digital titrator, The whole titration process is completed within 1 min, and the content of free acid in lithium hexafluorophosphate is calculated by the volume of sodium hydroxide consumed. The corresponding results are shown in Table 1. Intermediate precision data such as figure 1 shown.

[0027] (3) The calculation formula is as follows:

[0028] w = ...

Embodiment 2

[0033] Embodiment 2, the method for detecting the acidity of lithium tetrafluoroborate in this embodiment comprises the following steps:

[0034] (1) Take 100g of deionized water at a temperature of 1°C, add 1-3 drops of bromothymol blue indicator, use 0.01mol / l sodium hydroxide as the titrant, and titrate to blue-green with a digital titrator (deduct reagent blank);

[0035] (2) Weigh 2g of lithium tetrafluoroborate, add it to the deionized water titrated in step (1), dissolve it and let it stand for 1min, use 0.01mol / l sodium hydroxide as the titrant, and titrate with a digital titrator To blue-green, calculate the free acid content in lithium tetrafluoroborate from the volume of sodium hydroxide consumed. The corresponding results are shown in Table 1.

[0036] (3) The calculation formula is the same as step (3) of Example 1.

Embodiment 3

[0037] Embodiment 3, the method for detecting the acidity of lithium hexafluoroarsenate in this embodiment comprises the following steps:

[0038] (1) Take 100g of deionized water at a temperature of 4°C, add 1-3 drops of bromothymol blue indicator, use 0.1mol / l sodium hydroxide as the titrant, and titrate to blue-green with a digital titrator (deduct reagent blank);

[0039] (2) Weigh 10g of lithium hexafluoroarsenate, add it into the deionized water titrated in step (1), dissolve it and let it stand for 1min, use 0.1mol / l sodium hydroxide as the titrant, and titrate to the end point, The free acid content in lithium hexafluoroarsenate was calculated by the volume of sodium hydroxide consumed. The corresponding results are shown in Table 1.

[0040] (3) The calculation formula is the same as step (3) of Example 1.

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Abstract

The invention discloses a detection method for trace free acid in an electrolyte lithium salt. The detection method comprises the following steps: (1) weighing a certain amount of de-ionized water and adding a bromothymol blue indicator, and titrating by using a digital titrating device until the solution is blue green based on 0.005-0.1mol/l sodium hydroxide as a titrating agent; and (2) weighing a certain amount of the lithium salt and adding the lithium salt into the de-ionized water titrated by the step (1), agitating and dissolving, standing for 0-1 minute, titrating by using the digital titrating device until the solution is blue green based on 0.005-0.1mol/l sodium hydroxide as the titrating agent, and calculating the content of the free acid of the lithium salt by the consumed volume of the sodium hydroxide. According to the detection method, the temperature of the used de-ionized water is 0-4 DEG C, one part of the lithium salt can be effectively prevented from being decomposed and HF is prevented from being volatilized; the detection accuracy of a sample is improved. According to the detection method, the free acid of the lithium salt is determined by using the electronic titrating device; the detection method has the characteristics of short analyzing time, high precision and the like, and is simple to operate.

Description

technical field [0001] The invention relates to the field of material analysis and testing, in particular to a method for detecting trace free acids in electrolyte lithium salts. Background technique [0002] Lithium-ion battery is a green, high-energy and environmentally friendly battery that appeared in the 1990s. Compared with traditional secondary batteries, it has high working voltage, high specific energy, small self-discharge, long cycle life, no memory effect, and fast charging. Discharge and other unique properties. Based on these advantages, lithium-ion batteries have been developed by leaps and bounds. [0003] In addition to the factors of electrode materials, the advantages and disadvantages of lithium-ion batteries are closely related to the properties of electrolytes. Commonly used lithium salts include lithium hexafluorophosphate, lithium tetrafluoroborate, lithium hexafluoroarsenate, lithium hexafluorostannate, lithium hexafluorogermanate and other inorgan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/79
Inventor 罗海英史利涛徐三善蔡源满
Owner GUANGZHOU TINCI MATERIALS TECH
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