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Preparation method of lithium sulfide powder

A technology for lithium sulfide and powder, applied in the field of preparing lithium sulfide powder, can solve the problems of low purity of lithium sulfide, difficult industrial production, energy consumption, etc., and achieve the effect of easy industrial implementation and environmental friendliness

Inactive Publication Date: 2015-05-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the lithium sulfide produced by this method has disadvantages such as low purity, poor batchability, and energy consumption, and is not easy for industrial production.

Method used

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  • Preparation method of lithium sulfide powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The sulfur powder was dried in a vacuum oven at 100 °C for 12 h. Under the protection of an argon atmosphere, uniformly mix 0.32g of sulfur powder and 0.16g of lithium hydride powder and add them into a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 20:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 400r / min for 8 hours, and the obtained powder was lithium sulfide powder. figure 1 Its corresponding XRD diffraction pattern, compared with the standard card, shows that the obtained product is a pure phase lithium sulfide, and no other impurities exist.

Embodiment 2

[0030] The sulfur powder was dried in a vacuum oven at 60 °C for 24 h. Under the protection of a nitrogen atmosphere, 5.1 g of sulfur powder and 2.4 g of lithium hydride powder were uniformly mixed and then added to a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 60:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 350r / min for 12 hours, and the obtained powder was lithium sulfide powder.

Embodiment 3

[0032] The sulfur powder was dried in a vacuum oven at 80 °C for 6 h. Under the protection of an argon atmosphere, uniformly mix 9.6g of sulfur powder and 3.6g of lithium hydride powder and add them into a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 40:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 480r / min for 6 hours, and the obtained powder was lithium sulfide powder.

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Abstract

The invention discloses a preparation method of lithium sulfide powder. The preparation method comprises the following steps: (1) drying sulfur powder; (2) under inert atmosphere protection, mixing the dried sulfur powder with lithium hydride powder in a mole ratio of 1:(1-3), adding the obtained mixture into a sealed ball-milling tank, and carrying out ball-milling on the mixture for 1-24 h under the condition that the rotating speed is 100-500 r / min at room temperature; and (3) after the ball-milling reaction is completed, under inert atmosphere, taking the powder out of the ball-milling tank, so that the lithium sulfide powder is obtained. The preparation method of lithium sulfide powder disclosed by the invention has the characteristics of simple process, low cost, and easiness for industrialized production.

Description

(1) Technical field [0001] The invention relates to a method for preparing lithium sulfide powder. (2) Background technology [0002] Lithium sulfide is an inorganic compound whose chemical formula is Li 2 S, belonging to the cubic crystal system, anti-fluorite structure, space group is , easily deliquescent in the air. At present, there are few preparation methods for lithium sulfide, and the most common preparation methods mainly include the following two types: the first method is to put sulfur powder into lithium triethylborohydride (LiBEt) 3 H) in tetrahydrofuran (THF) solution, after fully reacting, the solid powder is separated from the liquid to obtain lithium sulfide; the second method is to add sulfur powder and metal lithium powder to liquid ammonia, and after fully reacting, the solid The powder is separated from the liquid to obtain lithium sulfide. The above-mentioned two types of methods all need solvents. After the solid-liquid separation process, the ef...

Claims

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Application Information

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IPC IPC(8): C01B17/22
CPCC01B17/22C01P2002/72
Inventor 梁初梁升夏阳张文魁黄辉陶新永甘永平
Owner ZHEJIANG UNIV OF TECH
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