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Preparation method of lithium sulfide

A lithium sulfide and lithium sulfate technology, applied in the chemical field, can solve the problems of multiple procedures and complicated preparation process, and achieve the effects of high safety, simple preparation method and process, and low production cost

Inactive Publication Date: 2018-08-14
北京天工新材科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is used to prepare high-purity lithium sulfide, and has the advantages of low reaction temperature, high stability when using multiple solvents, and no toxicity. However, the preparation method has many procedures and the preparation process is complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of lithium sulfide, is characterized in that, comprises the steps:

[0026] 1) After grinding and mixing anhydrous lithium sulfate, glucose and hard carbon, move them into the quartz sintered tube of the vacuum tube furnace;

[0027] 2) Preheating the quartz sintered tube, then evacuating the vacuum tube furnace, and connecting the Kaipu generator at the interface of the quartz sintered tube;

[0028] 3) Pass hydrogen gas into the quartz sintered tube and heat the quartz sintered tube to react to prepare the lithium sulfide.

[0029] Wherein, the anhydrous lithium sulfate, hard carbon and glucose were mixed in a mass ratio of 1:2:5, and were ground for 6 hours at room temperature in a planetary ball mill whose model was SK2-4-12PC3, and the ball milling speed was 400 rpm , the particle size of the anhydrous lithium sulfate, glucose and hard carbon after grinding is 20 microns; the preheating temperature of the quartz sintered tube is 290°C;...

Embodiment 2

[0032] A kind of preparation method of lithium sulfide, is characterized in that, comprises the steps:

[0033] 1) After grinding and mixing anhydrous lithium sulfate, glucose and hard carbon, move them into the quartz sintered tube of the vacuum tube furnace;

[0034] 2) Preheating the quartz sintered tube, then evacuating the vacuum tube furnace, and connecting the Kaipu generator at the interface of the quartz sintered tube;

[0035] 3) Pass hydrogen gas into the quartz sintered tube and heat the quartz sintered tube to react to prepare the lithium sulfide.

[0036] Wherein, the anhydrous lithium sulfate, hard carbon and glucose were mixed in a mass ratio of 10:1:5, and were ground for 9 hours at room temperature in a planetary ball mill whose model was SK2-4-12PC3, and the ball milling speed was 600 rpm , the particle size of the anhydrous lithium sulfate, glucose and hard carbon after grinding is 5 microns; the preheating temperature of the quartz sintered tube is 230°C;...

Embodiment 3

[0039] A kind of preparation method of lithium sulfide, is characterized in that, comprises the steps:

[0040] 1) After grinding and mixing anhydrous lithium sulfate, glucose and hard carbon, move them into the quartz sintered tube of the vacuum tube furnace;

[0041] 2) Preheating the quartz sintered tube, then evacuating the vacuum tube furnace, and connecting the Kaipu generator at the interface of the quartz sintered tube;

[0042] 3) Pass hydrogen gas into the quartz sintered tube and heat the quartz sintered tube to react to prepare the lithium sulfide.

[0043]Wherein, the anhydrous lithium sulfate, hard carbon and glucose were mixed in a mass ratio of 5:1.5:5, and were ground for 7.5 hours at room temperature in a planetary ball mill whose model was SK2-4-12PC3, and the ball milling speed was 200 rpm , the particle size of the anhydrous lithium sulfate, glucose and hard carbon after grinding is 13 microns; the preheating temperature of the quartz sintered tube is 260...

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Abstract

The invention discloses a preparation method of lithium sulfide. The preparation method comprises the following steps of 1) grinding, mixing and transferring anhydrous lithium sulfate, glucose and hard carbon into a quartz sintering tube of a vacuum tubular furnace; 2) per-heating the quartz sintering tube, vacuumizing the vacuum tubular furnace, and connecting a kipp gas generator to a pipe opening of the quartz sintering tube; 3) introducing hydrogen to the quartz sintering tube, heating the quartz sintering tube, and performing reaction to prepare the lithium sulfide, wherein the mass ratioof the anhydrous lithium sulfate, the hard carbon and the glucose is (1:2:5)-(10:1:5). The purity of the lithium sulfide prepared by the preparation method of the lithium sulfide reaches 99.9% or above, the lithium sulfide is low in production cost, simple in preparation method and process, short in preparation period and simple in preparation equipment and is easy to operate, the preparation process is high in safety, the raw material which is used is non-toxic, industrial production on a large scale is facilitated, the glucose is tightly combined with lithium sulfate after carbonization, and the conversion efficiency of the lithium sulfide can be improved.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a preparation method of lithium sulfide. Background technique [0002] In recent years, there has been an increasing demand for high-performance lithium secondary batteries used in portable information terminals, portable electronic devices, small household power storage devices, motorcycles powered by motors, electric vehicles, and hybrid electric vehicles. High-purity lithium sulfide is a commonly used electrolyte material in lithium-ion batteries. Lithium-sulfur batteries have become one of the research hotspots for next-generation lithium batteries due to their high specific energy, cheap battery materials, and environmental friendliness. However, lithium sulfide is extremely sensitive to water, so that the production, storage, and preparation processes are subject to many restrictions, and eventually the price of lithium sulfide is extremely expensive, which gr...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCH01M4/5815Y02E60/10
Inventor 罗发洪朱辰
Owner 北京天工新材科技发展有限公司
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