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Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof

A technology of Karl Fischer reagent and electrolyte, which is applied in the field of Karl Fischer reagent for electrolyte moisture detection and its preparation, which can solve the problems of endangering human health, high moisture detection value, and unstable drift value, etc., to ensure accuracy Effect

Active Publication Date: 2017-02-22
SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the electrolyte contains boron additives, due to the electron loss of the boron atom, it is easy to undergo an esterification reaction with the hydroxyl compound in the Karl Fischer reagent to release water, such as boric acid and methanol, that is, H 3 BO 3 +3CH 3 OH→B(OCH 3 ) 3 +3H 2 O, resulting in high moisture detection value and unstable drift value; in addition, due to the foul smell of pyridine, it pollutes the operating environment; while methanol is highly toxic, endangers human health, has poor storage stability, short storage time and is flammable
Therefore, the currently commercially available Karl Fischer reagent cannot be directly used to test the trace moisture content in the electrolyte

Method used

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  • Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof
  • Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof
  • Karl-Fischer reagent for electrolyte moisture detection and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] At normal temperature, add 54wt% ethylene glycol dimethyl ether, 20wt% aniline and 1.5wt% iodine into the reaction kettle successively, and stir fully to form a mixed solution; bath, and slowly feed 1wt% sulfur dioxide gas, stir evenly, at this time the pH of the solution is 5.4; the temperature is raised to normal temperature, add 20wt% aniline hydroiodide and 3.5wt% carbon tetrachloride, stir until completely dissolved, Leave it for 24 hours to get the product.

Embodiment 2

[0031] At room temperature, successively add 70wt% propylene glycol dimethyl ether, 10wt% aniline and 3wt% iodine into the reaction kettle, and fully stir to form a mixed solution; then place the mixed solution in an ice bath with a temperature of 0-4°C, And slowly feed 2wt% sulfur dioxide gas, stir evenly, at this time the pH of the solution is 5.0; raise the temperature to normal temperature, add 10wt% aniline hydriodide and 5wt% carbon tetrachloride, stir until completely dissolved, place for 24h, that is get the product.

Embodiment 3

[0033] At room temperature, sequentially add 40wt% hexamethylene glycol dimethyl ether, 20wt% aniline and 8wt% iodine into the reaction kettle, and stir fully to form a mixed solution; then place the mixed solution in an ice bath with a temperature of 0-4°C and slowly feed 8wt% sulfur dioxide gas into the solution, stir evenly, at this time the pH of the solution is 4.0; raise the temperature to room temperature, add 20wt% aniline hydroiodide and 4wt% carbon tetrachloride, stir until completely dissolved, and place for 24h , that is, the product is obtained.

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Abstract

The invention belongs to the technical field of a battery and especially relates to a Karl-Fischer reagent for electrolyte moisture detection and a preparation method thereof. The Karl-Fischer reagent comprises the following components by weight percent: 1-8% of iodine, 1-8% of sulfur dioxide, 2-10% of carbon tetrachloride, 10-30% of aniline, 10-30% of aniline hydriodate and 40-70% of hydroxyl-free alcohol ether compound. Compared with the present Karl-Fischer reagent containing methyl alcohol, 2-methoxyethanol, and the like, the Karl-Fischer reagent provided by the invention contains no hydroxyl compound, so that the Karl-Fischer reagent can be effectively prevented from having esterification reaction with a boracic additive in the electrolyte and further influencing the determination for trace water in electrolyte, and the detection accuracy can be guaranteed. Besides, the Karl-Fischer reagent provided by the invention contains no toxic or environmental pollution components, such as methyl alcohol and pyridine, so that the Karl-Fischer reagent is more safe and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of batteries, and in particular relates to a Karl Fischer reagent for electrolyte moisture detection and a preparation method thereof. Background technique [0002] Lithium-ion battery electrolyte is an important part of lithium-ion batteries. As lithium-ion batteries are more and more widely used in digital, aircraft model, energy storage, power and other fields, more requirements are placed on the electrolyte. Among them, adding boron-containing compounds such as lithium difluorooxalate borate, lithium bisoxalate borate, lithium tetrafluoroborate, and tris(trimethylsilyl) borate to the electrolyte can better improve the thermal performance of lithium-ion batteries. Stability, chemical stability and high and low temperature performance. [0003] However, the existence of trace moisture (20ppm) in the electrolyte will lead to the decomposition of lithium hexafluorophosphate in the electrolyte to generate HF...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
CPCG01N31/168
Inventor 廖红伟王强强
Owner SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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