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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the existing preparation method of high-purity lithium sulfide has the disadvantages of high reaction temperature, long cycle, flammable and explosive organic solvents, irritation and toxicity, etc.

Method used

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  • Preparation method and device of high-purity lithium sulfide

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preparation example Construction

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

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

Embodiment 1

[0055] Take 500g of lithium hydroxide monohydrate in a 5L round-bottomed flask and dehydrate under reduced pressure at 120°C for 3 hours to remove the crystal water and purify the lithium hydroxide. After cooling down, add 3.5L N-methylpyrrolidone, vacuumize, and purge the system with argon gas, the flow rate is 0.15m 3 / h, after repeating this three times, the temperature was raised to 140°C, mechanically stirred for 3h, and the stirring speed was 160 rpm. Introduce hydrogen sulfide gas, react at the above temperature and stir for 4h. After that, stop passing hydrogen sulfide, raise the temperature to 180°C, react for 2 hours, remove hydrogen sulfide to generate lithium sulfide, and then purge with argon to remove excess hydrogen sulfide gas, and the purge process lasts for 2 hours. The reaction slurry was centrifuged at a centrifugal speed of 7000 rpm and a centrifugation time of 0.5h. The centrifuged precipitate was redissolved in 500ml of N-methylpyrrolidone and refluxed ...

Embodiment 2

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

[0059] Take 500g of lithium hydroxide monohydrate in a 5L round-bottomed flask and dehy...

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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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