Preparation method and application of high-purity lithium sulfide

A lithium sulfide, high-purity technology, applied in chemical instruments and methods, inorganic chemistry, lithium compounds, etc., can solve problems such as large interface interaction, low product purity, and difficult purification, and achieve enhanced electronic conductivity and high electronic conductivity , the effect of improving economic efficiency

Active Publication Date: 2021-09-21
高能时代(珠海)新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, in method 1, the solid reacts with the solid, the interface effect is large, and the reaction can only be carried out on the solid surface, resulting in low product purity and containing a large amount of impurities. Method 2 NMP is easy to deteriorate under alkaline conditions and difficult to recycle.
The reaction conditions are harsh, the production of water will easily lead to the deterioration of lithium sulfide, and the purification is difficult. The method 3 lithium and sulfur react violently and easily explode, which is not easy to control and easily produces polysulfides

Method used

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  • Preparation method and application of high-purity lithium sulfide
  • Preparation method and application of high-purity lithium sulfide
  • Preparation method and application of high-purity lithium sulfide

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preparation example Construction

[0012] The invention provides a kind of preparation method of high-purity lithium sulfide, and this preparation method comprises the following steps:

[0013] Step 1: ball milling the defective lithium amide until the D50 remains below 50 microns to obtain lithium amide particle powder;

[0014] Step 2: Put the lithium amide particle powder in a reaction furnace with a stirring device, evacuate the reaction furnace to a vacuum degree of -0.1mpa, raise the temperature of the reaction furnace to 200-300°C, and then feed hydrogen sulfide into the reaction furnace Gas, keep the pressure of the reaction furnace at 0.1-0.15mpa, stir and react for 3-5 hours;

[0015] Step 3: Turn off the hydrogen sulfide gas, raise the temperature of the reaction furnace to 400-430°C, keep it warm for 0.5-1 hour, and vacuumize the reaction furnace to a vacuum degree of -0.1mpa after the heat preservation is completed;

[0016] Step 4: Introduce hydrogen sulfide gas again, keep the pressure of the re...

Embodiment 1

[0024] Step 1: ball milling the defective lithium amide until the D50 remains below 50 microns to obtain lithium amide particle powder;

[0025] Step 2: Put the lithium amide particle powder in a reaction furnace with a stirring device, evacuate the reaction furnace to a vacuum degree of -0.1mpa, raise the temperature of the reaction furnace to 200°C, and then pass hydrogen sulfide gas into the reaction furnace, Keep the reaction furnace pressure at 0.1mpa, stir and react for 5 hours;

[0026] Step 3: Turn off the hydrogen sulfide gas, raise the temperature of the reaction furnace to 430°C, and keep it warm for 0.5 hours. After the heat preservation is completed, evacuate the reaction furnace to a vacuum degree of -0.1mpa;

[0027] Step 4: Introduce hydrogen sulfide gas again to keep the pressure of the reactor at 0.1mpa, and raise the temperature to 430°C for 3 hours;

[0028] Step 5: The reacted lithium sulfide is ball milled and sieved, and the D50 is controlled to be 10-5...

Embodiment 2

[0030] Step 1: ball milling the defective lithium amide until the D50 remains below 50 microns to obtain lithium amide particle powder;

[0031] Step 2: Put the lithium amide particle powder in a reaction furnace with a stirring device, evacuate the reaction furnace to a vacuum degree of -0.1mpa, raise the temperature of the reaction furnace to 250°C, and then pass hydrogen sulfide gas into the reaction furnace, Keep the reaction furnace pressure at 0.13mpa, stir and react for 4 hours;

[0032] Step 3: Turn off the hydrogen sulfide gas, raise the temperature of the reaction furnace to 420°C, and keep it warm for 0.75 hours. After the heat preservation is completed, vacuum the reaction furnace to a vacuum degree of -0.1mpa;

[0033] Step 4: Introduce hydrogen sulfide gas again to keep the pressure of the reactor at 0.75mpa, and raise the temperature to 430°C for 4 hours;

[0034] Step 5: The reacted lithium sulfide is ball milled and sieved, and the D50 is controlled to be 10-...

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Abstract

The invention discloses a preparation method and application of high-purity lithium sulfide. Lithium sulfide is prepared by reacting a lithium amide defective product with hydrogen sulfide. Compared with metal lithium, lithium amide and by-products thereof are easier to react with hydrogen sulfide, so that lithium amide defective products react with hydrogen sulfide, on one hand, the progress of reaction between metal lithium and hydrogen sulfide is accelerated, and on the other hand, a small amount of lithium nitrogen compounds participating in the reaction have higher electron conductivity; and the prepared lithium sulfide is used as a sulfide electrolyte, and the performance of enhancing the electronic conductivity of the sulfide electrolyte can be achieved. Moreover, the economic benefit is also greatly improved by recycling lithium amide defective products.

Description

technical field [0001] The invention relates to the technical field of batteries, in particular to a preparation method and application of high-purity lithium sulfide. Background technique [0002] As the most important component of solid-state sulfide lithium-ion batteries with high energy and high safety performance, lithium sulfide is also the raw material for the preparation of solid-state sulfide electrolytes and the positive electrode material for high-capacity lithium-sulfur batteries. General attention and attention. Lithium amide is mainly used for synthesis and is mainly used in organic synthesis and pharmaceutical manufacturing. In industry, lithium metal and ammonia are commonly used to react with ammonia gas to prepare lithium amide. However, lithium hydride and lithium imide are easily produced if the production process is not well controlled. Impurities such as lithium nitride cause lithium amide purity to be not high, produce defective product (main content ...

Claims

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Application Information

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IPC IPC(8): C01D15/00H01M10/0563
CPCC01D15/00H01M10/0563C01P2002/72C01P2004/61C01P2006/80C01P2006/40Y02E60/10
Inventor 刘延成
Owner 高能时代(珠海)新能源科技有限公司
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