Method of preparing and purifying lithium sulfide

A lithium sulfide and lithium sulfate technology, applied in chemical instruments and methods, sulfur compounds, alkali metal sulfides/polysulfides, etc., can solve the problems of poor controllability of composite material morphology, difficulty in preparing lithium sulfide, and unstable product quality and other problems, to achieve the effect of easy industrial implementation, high yield and low equipment requirements

Inactive Publication Date: 2020-11-10
TIANJIN UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

The disadvantage is that the process technology still needs to be optimized and perfected, the product quality is unstable, and the controllability of the shape of the composite material is poor.
[0007] It is precisely because of the above-mentioned problems in the existing lithium sulfide preparation methods that the industrial production of lithium sulfide is difficult and the cost remains high. Therefore, the development of low-cost large-scale preparation and purification of lithium sulfide is the key to promoting sulfide electrolytes and sulfide solid-state batteries. The key to practicality

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  • Method of preparing and purifying lithium sulfide
  • Method of preparing and purifying lithium sulfide

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[0022] The method for preparing and purifying lithium sulfide provided by a typical embodiment of the present invention includes

[0023] Step 1, dissolving lithium sulfate and soluble carbon source in deionized water in proportion, and then spray-drying and granulating to obtain powder.

[0024] The ratio of lithium sulfate and soluble carbon source is Li 2 SO 4 +2C=Li 2 S+2CO 2 Weighing, excess carbon source 3-5%.

[0025] Preferably, in step 1, the soluble carbon source is one or a combination of sucrose, glucose and citric acid.

[0026] Step 2: Calcining the granulated powder under the protection of an inert atmosphere.

[0027] Preferably, in step 2, the inert atmosphere is nitrogen, argon or hydrogen-argon mixed gas. The calcination temperature is 750~900℃, and the calcination time is 5~15h.

[0028] Step 3: In a dehumidifying and drying environment, the calcined powder is washed with absolute ethanol to filter out insoluble lithium sulfate and carbon powder, and...

Embodiment 1

[0032] According to Li 2 SO 4 +2C=Li 2 S+2CO 2 For the reaction, lithium sulfate and sucrose were dissolved in deionized water in proportion (excess sucrose 5%), and then spray-dried and granulated; under the protection of nitrogen, the granulated powder was calcined in a tube furnace at 750°C for 15 hours; In a water anaerobic glove box (both water and oxygen content is lower than 1ppm), the calcined powder is washed with absolute ethanol to filter out insoluble lithium sulfate and carbon powder, and then the filtrate is evaporated, crystallized, purified and dried to obtain lithium sulfide , with a purity of 99.4%.

Embodiment 2

[0034] According to Li 2 SO 4 +2C=Li 2 S+2CO 2 Reaction, dissolve lithium sulfate and citric acid in proportion (5% citric acid excess) in deionized water, then spray dry and granulate; under the protection of hydrogen and argon mixed gas, the granulated powder is 900°C in a tube furnace Calcination for 5 hours; in the dehumidification and drying room (water content less than 100ppm), the calcined powder is washed with absolute ethanol to filter out insoluble lithium sulfate and carbon powder, and then the filtrate is evaporated, crystallized, purified and dried to obtain lithium sulfide , with a purity of 99.5%.

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Abstract

The invention relates to a method for preparing and purifying lithium sulfide, which comprises the following steps: proportionally dissolving lithium sulfate and a soluble carbon source in deionized water, and carrying out spray drying granulation to obtain powder; calcining the powder obtained by granulation under the protection of an inert atmosphere; and in a dehumidifying and drying environment, washing the powder obtained by calcining with absolute ethyl alcohol, filtering out insoluble lithium sulfate and carbon powder, crystallizing and purifying the filtrate, and drying the solid to obtain lithium sulfide. The yield of lithium sulfide obtained by calcining after drying granulation is high (higher than 93%), wherein high-purity lithium sulfide is obtained after purification with absolute ethyl alcohol. The method has the advantages of simple preparation and purification processes, low equipment requirements, cyclic utilization of the purification solvent, environmental friendliness and easiness in industrial implementation.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a method for large-scale preparation and purification of lithium sulfide at low cost. Background technique [0002] Lithium-ion batteries have been widely used in digital products, electric vehicles, energy storage power stations and other fields. Due to the use of liquid electrolyte in traditional lithium-ion batteries, the safety problem cannot be completely solved. Solid-state batteries, including all-solid-state batteries, can effectively solve the problem of battery safety due to the use of non-flammable solid-state electrolytes. Among the developed solid-state electrolytes, sulfide solid-state electrolytes have the highest ionic conductivity and have attracted extensive attention. The main raw material for the synthesis of sulfide electrolytes is lithium sulfide. The existing preparation methods of lithium sulfide can be roughly divided into ball milling meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/26C01B17/36H01M4/58H01M10/0525
CPCC01B17/26C01B17/36C01P2006/80H01M4/5815H01M10/0525Y02E60/10
Inventor 宋大卫涂芳源张洪周张联齐
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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