Preparation method and device of high-purity lithium sulfide

A technology of lithium sulfide and lithium sulfide hydride, applied in the field of chemistry, can solve the problems of irritation and toxicity, flammable and explosive organic solvents, high reaction temperature, high product yield and purity, direct and simple purification process, and high reaction temperature. low temperature effect

Inactive Publication Date: 2015-11-04
FIRST RARE MATERIALS CO LTD
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Problems solved by technology

[0005] However, the existing preparation method of high-purity lithium sulfide has the disadvantages of hig

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  • Preparation method and device of high-purity lithium sulfide

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Example Embodiment

[0043] The present invention provides a method for preparing high-purity lithium sulfide, including:

[0044] Lithium hydroxide is purified, the purification temperature is 110~120℃, and the purification time is 3~4h; the lithium hydroxide and N-methylpyrrolidone are mixed to obtain a mixed solution; the mixed solution is heated to 130 under the protection of inert gas -140℃, the inert gas can be argon or nitrogen, the flow of inert gas is 0.15~0.25m 3 / h, while heating, start stirring, the stirring time is 2 to 3 hours, the stirring speed is 150 to 250 revolutions per minute; hydrogen sulfide gas is passed into the mixed solution, and the reaction time is 2 to 4 hours to obtain Lithium hydrogen sulfide slurry; use high temperature method to remove hydrogen sulfide from the lithium hydrogen sulfide, and remove the hydrogen sulfide at a temperature of 170-180°C to obtain a lithium sulfide slurry; use inert gas to remove excess hydrogen sulfide gas , The purging process lasts for 2...

Example Embodiment

[0054] Example 1

[0055] Take 500g of lithium hydroxide monohydrate in a 5L round-bottomed flask at 120°C for 3h under reduced pressure distillation, remove the crystal water, and purify the lithium hydroxide. After cooling down, add 3.5L of N-methylpyrrolidone, evacuate, purge the system with argon, flow rate is 0.15m 3 / h, after this is repeated three times, the temperature is increased to 140°C, and mechanical stirring is performed for 3 hours, and the stirring speed is 160 rpm. Pass hydrogen sulfide gas and react for 4h at the above temperature and stirring. After that, the hydrogen sulfide was stopped, the temperature was raised to 180°C, and the reaction was carried out for 2 hours to remove hydrogen sulfide to generate lithium sulfide, and then argon purge to remove excess hydrogen sulfide gas. The purge process lasts for 2 hours. The reaction slurry was centrifuged at a speed of 7000 rpm and a centrifugal time of 0.5h. The centrifuged precipitate was re-dissolved in 500...

Example Embodiment

[0057] Example 2

[0058] Take 500g of lithium hydroxide monohydrate in a 5L round-bottomed flask and distill under reduced pressure at 120°C to remove crystal water. After cooling, 4LNMP was added, evacuated, and argon purged to remove the system. After repeating this three times, the temperature was raised to 140°C and mechanically stirred for 3 hours. Pass hydrogen sulfide gas and react for 2h at the above temperature and stirring. After that, hydrogen sulfide was stopped and the temperature was raised to 190°C to remove hydrogen sulfide to generate lithium sulfide. After the reaction slurry was centrifuged, the centrifuged precipitate was re-dissolved in 300ml NMP and refluxed at 150°C for 2h, filtered and dried while hot to obtain 246.10g of high-purity lithium sulfide. The decolorization of centrifugal liquid by vacuum distillation can recycle NMP.

[0059] Take 500g of lithium hydroxide monohydrate in a 5L round-bottomed flask at 120°C for 3h under reduced pressure distil...

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Abstract

The embodiment of the invention discloses a preparation method and device of high-purity lithium sulfide, which have the advantages that reaction temperature are low, production period is short, and used solvent is high in stability and non-toxic. The method comprises the steps of: mixing lithium hydroxide and N-methyl pyrrolidone to obtain a mixed solution; heating the mixed solution under the protection of inert gas to 130 to 140 DEG C; introducing hydrogen sulfide gas into the mixed solution to react for 2 to 4 hours to obtain lithium hydrogen sulfide serous fluid; removing hydrogen sulfide from the lithium hydrogen sulfide to obtain lithium sulfide serous fluid; removing excessive hydrogen sulfide gas; and removing impurities in the lithium sulfide serous fluid, and drying to obtain the high-purity lithium sulfide. The device comprises a reaction device, a stirring device, a water distributor, a condensation device, a first anti-suck-back device, a second anti-suck-back device, a vacuum device, a tail gas absorption device and a buffer device.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method and device for preparing high-purity lithium sulfide. Background technique [0002] Lithium batteries account for a large proportion of new energy batteries, providing important energy storage guarantees for the era of clean energy. [0003] High-purity lithium sulfide is a potential electrolyte material for lithium-ion batteries. Lithium sulfide batteries have the characteristics of long life, high capacity and high energy, and are not prone to overheating. [0004] At present, the methods for preparing high-purity lithium sulfide mainly include: synthesis of lithium and sulfur directly or in liquid ammonia, reaction of lithium and hydrogen sulfide in tetrahydrofuran, decomposition of ethanol adduct of lithium sulfide by lithium ethoxide, lithium carbonate and hydrogen sulfide response etc. [0005] However, the existing preparation method of high-purity lithium sulfide has ...

Claims

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Application Information

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IPC IPC(8): C01B17/22
Inventor 何志达朱刘高远胡智向余芳
Owner FIRST RARE MATERIALS CO LTD
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