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A kind of preparation method of lithium sulfide, lithium sulfide and application thereof

A technology of lithium sulfide and anhydrous sodium sulfide, applied in the direction of alkali metal sulfide/polysulfide, lithium battery, structural parts, etc., can solve the problem of high cost of lithium sulfide preparation, and achieve suitable mass production and environmental protection Friendly, reproducible results

Active Publication Date: 2022-04-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is high temperature and high energy and the emission of greenhouse gas carbon dioxide
[0007] In summary, various preparation methods of lithium sulfide have shortcomings of one kind or another, which has caused the preparation cost of lithium sulfide to remain high, and has become an important factor in promoting the practical application of lithium-sulfur batteries and all-solid-state batteries based on sulfide electrolytes. Therefore, it is of great significance to develop a low-cost, environmentally friendly and easy-to-large-scale industrialization of lithium sulfide synthesis methods

Method used

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  • A kind of preparation method of lithium sulfide, lithium sulfide and application thereof
  • A kind of preparation method of lithium sulfide, lithium sulfide and application thereof
  • A kind of preparation method of lithium sulfide, lithium sulfide and application thereof

Examples

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Effect test

example 1

[0036] Method for preparing sulfide, including the following steps:

[0037] S1, under argon atmosphere protection, sodium dehydrated anhydrous sodium sulfide (NA) 2 S) and lithium chloride (LiCl) raw materials Mass mole ratio 0.5: 2. In the argon atmosphere glove box, sodium sulfide mass was 102 mg, 10 ml of anhydrous ethanol was added. The container is placed on a magnetic stirrer and the rotational speed is 520 rpm, and the stirring time is 30 min. The lithium chloride mass was 185 mg, and 4 ml of absolute ethanol magnet was stirred, the rotational speed was 520 rpm, and the stirring time was 20 min. The configured lithium chloride / ethanol solution was added to the sodium sulfide / ethanol solution, and stirred while stirring, a white precipitate was stirred, continuously stirred for 12 h, and the rotational speed was 520 rpm to obtain a suspension. Among them, the reactive reaction between sodium sulfide and lithium chloride is:

[0038] NA 2 S (SOL) + 2Licl (SOL) → Li 2 S (...

example 2

[0044] Method for preparing sulfide, including the following steps:

[0045] S1, 5g nine water sodium sulfide (NA 2 S · 9h 2 O) The raw material is heated in the muffle furnace of nitrogen protection, and the temperature is set to 300 to 350 ° C, and the time is set to 6 to 12 hours to give 1.6 g of anhydrous sodium sulfide. Under a nitrogen atmosphere, anhydrous sodium sulfide and lithium chloride raw materials were measured from 1: 2. In the nitrogen atmosphere glove box, the sodium sulfide mass was measured at 170 mg, 10 ml of anhydrous ethanol was added. The container is placed on a magnetic stirrer and the rotation speed is 720 rpm, and the stirring time is 60 min. The lithium chloride mass was 185 mg, and 4 ml of absolute anhydrous ethanol was stirred, the rotational speed was 720 rpm, and the stirring time was 15 min. The configured lithium chloride / ethanol solution was added to a sodium sulfide / ethanol solution, and stirred while stirring, a white precipitate was forme...

example 3

[0052] Method for preparing sulfide, including the following steps:

[0053] S1, under argon atmosphere protection, dried dehydrated anhydrous sodium sulfide and lithium chloride raw materials were measured from 0.8: 2. In the argon atmosphere glove box, the sodium sulfide mass was 136 mg, 8 ml of anhydrous ethanol was added. The container is placed on a magnetic stirrer and the rotation speed is 900 rpm, and the stirring time is 30 min. It is weighed with a lithium chloride mass of 190 mg, and 4 ml of anhydrous ethanol magnetic stirring was added, the rotational speed was 900 rpm, and the stirring time was 20 min. The configured lithium chloride / ethanol solution was added to the sodium sulfide / ethanol solution, and stirred while stirring, it immediately had a white precipitate, continuously stirred for 12 h, and the rotation speed was 500 rpm, and the suspension was obtained. Among them, the reactive reaction between sodium sulfide and lithium chloride is:

[0054] NA 2 S (SO...

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Abstract

The invention provides a preparation method of lithium sulfide. First, under the protection of an inert atmosphere, weigh a lithium source compound and a sulfur source compound and prepare their alcohol solutions respectively, and then add the alcohol solution of the lithium source compound to the alcohol solution of the sulfur source compound In the process, centrifuge the fully reacted product after magnetic stirring, and collect the supernatant; then transfer it to a tube furnace for heating and crystallization to obtain a crude lithium sulfide product; then use N-methylpyrrolidone or acetone to wash and centrifuge the crude lithium sulfide product, collect the solid product; then use n-hexane to wash and centrifuge the solid product, and vacuum-dry to obtain lithium sulfide. Compared with the prior art, in the method provided by the present invention, the lithium source compound and the sulfur source compound are subjected to a metathesis reaction in an alcoholic solution to obtain lithium sulfide, and the obtained lithium sulfide has high purity and good reproducibility, and the preparation process does not involve high temperature High pressure, no greenhouse gas emissions, environmental friendliness, no need for complicated and expensive instruments and equipment, and easy for large-scale industrial production.

Description

Technical field [0001] The present invention relates to the field of secondary battery, and more particularly to the preparation method of lithium sulfide, lithium sulfide and its application thereof. Background technique [0002] Lithium-ion batteries have now widely used in the fields of digital products, electric vehicles, and energy storage power stations, but because of its liquid electrolyte, there is a safety hazard during integrated applications; and it is more than energy is close to the theoretical limit, it is difficult to meet the new generation A higher requirements for power batteries. The full solid state battery can effectively solve safety problems due to the use of uncommon solid electrolytes; the lithium-sulfur battery is positive because of the use of metal lithium as a negative electrode and sulfur (or lithium sulfide) to have higher theoretical ratio energy (five times the traditional lithium) Ion batteries), so in recent years have become a scientific and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/22H01M4/58H01M10/052
CPCC01B17/22H01M4/5815H01M10/052C01P2002/72Y02E60/10
Inventor 杨永安方俪然万丰铭
Owner TIANJIN UNIV
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