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Green preparation method of lithium sulfide

A lithium sulfide, green technology, applied in the direction of alkali metal sulfide/polysulfide, electrochemical generator, positive electrode, etc., can solve the problem of increasing the reaction process and subsequent processing steps, increasing the research burden in the field of lithium sulfide, and complicating the preparation process and other problems, to achieve the effect of facilitating purification, realizing large-scale continuous preparation, and simple process

Active Publication Date: 2021-03-19
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(2) In the research of solid-state electrolytes for lithium-sulfur batteries, due to the rise of LPSCl solid-state electrolytes, lithium sulfide is used as a raw material for this solid-state electrolyte, and the demand for it in relevant laboratories has increased significantly. At present, high-purity lithium sulfide is mainly Purchased through Aladdin, Alpha and other reagent websites, the price per gram of lithium sulfide exceeds 100 yuan, which increases the research burden in the field of lithium sulfide
However, the preparation process of this method is complicated, and a large amount of aromatic and ether organic solvents need to be consumed. Most of these solvents are toxic, and will produce a large amount of waste liquid pollution, and the cost is high; High-purity lithium metal, high-purity sulfur element, using ether or aromatic hydrocarbons as solvents to obtain lithium sulfide at high temperature, but this method uses high temperature and high pressure, requires a large amount of organic solvent, and the reaction process is complicated. The reaction process and subsequent processing steps are greatly increased, and a large amount of waste liquid and gas will be generated at the same time, which seriously affects the environment

Method used

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  • Green preparation method of lithium sulfide

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Effect test

Embodiment 1

[0027] In a glove box filled with argon atmosphere, lithium amide and elemental sublimed sulfur were weighed according to the molar ratio of 2:1, ground evenly by hand, then transferred to a heating tube, vacuumed, and 30 bar hydrogen gas was introduced. Heat to 300°C at a heating rate of 2°C / min, keep it warm for 5 hours, after the reaction is completed, the temperature of the reactor drops to room temperature, vacuumize, transfer the reactor to a glove box with argon atmosphere, open the reactor, and take out the powder sample That is the required lithium sulfide powder. figure 1 It is the X-ray diffraction pattern corresponding to the product, and the obtained product is lithium sulfide.

Embodiment 2

[0029] In a glove box filled with argon atmosphere, weigh imide lithium and elemental sublimed sulfur according to the molar ratio of 2:1, grind them evenly by hand, then transfer them to a heating tube, vacuumize, and inject 50bar hydrogen. Heat up to 500°C at a heating rate of 5°C / min, keep warm for 1h, after the reaction is completed, the reactor temperature drops to room temperature, vacuumize, transfer the reactor to an argon atmosphere glove box, open the reactor, and take out the powder sample That is the required lithium sulfide powder.

Embodiment 3

[0031] In a glove box filled with a helium atmosphere, lithium amide and elemental sublimed sulfur were weighed according to a molar ratio of 2:1, ground evenly by hand, then transferred to a heating tube, vacuumed, and 10 bar hydrogen gas was introduced. Heat up to 200°C at a heating rate of 5°C / min, keep it warm for 20 hours, after the reaction ends, the reactor temperature drops to room temperature, vacuumize, transfer the reactor to a glove box with a helium atmosphere, open the reactor, and take out the powder sample That is the required lithium sulfide powder.

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Abstract

The invention belongs to the field of material synthesis, and particularly relates to a green preparation method of lithium sulfide. Aiming at the problems that high-purity lithium sulfide is high inprice inAladdin and Alpha reagent websites, the research burden in the field of lithium sulfide research is increased and the like, the invention discloses the green preparation method of lithium sulfide, and lithium sulfide powder can be obtained through simple processes such as solid-solid mixing, heating, heat preservation and the like. The method has the advantages of simple preparation method, easy realization of industrial production, low preparation cost, high product purity, realization of large-batch continuous preparation, and meeting of the requirements of the current research fieldon lithium sulfide.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a green preparation method of lithium sulfide. Background technique [0002] Lithium sulfide, molecular formula: Li 2 S, for lithium sulfide. It is an important part of the current lithium-ion battery research field, and is mainly used for the research of lithium-ion battery cathode materials and the research of lithium-sulfur battery solid electrolyte. (1) As a popular electrode material, the theoretical discharge mass specific capacity of lithium sulfide is 1166mAh / g, which is much higher than the capacity of lithium cobalt oxide batteries (<150mAh / g) widely used in commerce. The content is high, and the matching negative electrode material can even choose a lithium-free material, thereby ensuring the safety of the battery. (2) In the research of solid-state electrolytes for lithium-sulfur batteries, due to the rise of LPSCl solid-state electrolytes, lithium ...

Claims

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Application Information

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IPC IPC(8): C01B17/22H01M4/58H01M10/0525H01M10/0562
CPCC01B17/22H01M4/5815H01M10/0525H01M10/0562H01M2004/028C01P2002/72Y02E60/10
Inventor 梁初王凯李嘉辉甘永平黄辉张文魁张俊夏阳
Owner ZHEJIANG UNIV OF TECH
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