KR-20260064298-A - Lithium sulfide synthesis process using lithium and sulfur powder

KR20260064298AKR 20260064298 AKR20260064298 AKR 20260064298AKR-20260064298-A

Abstract

The present invention provides a lithium sulfide synthesis process comprising: a first raw material including a lithium source; a second raw material including a sulfur source; a first raw material supply means for storing and supplying the first raw material under an inert gas atmosphere; a second raw material supply means for storing and supplying the second raw material; a first pulverization means for receiving the first raw material from the first raw material supply means and pulverizing it first through a blade mill; a cooling means for lowering the temperature of the first pulverization means; a second pulverization means for receiving the material that has passed through the first pulverization means and pulverizing it second; and a packaging means for packaging the material pulverized after passing through the second pulverization means. The process further comprises one or more of a sample inspection means, a centrifugation means, a wet stirring means, and an attrition mill between the first pulverization means and the second pulverization means, and a heating means including an electric heater is connected to one or more of the first pulverization means or the wet stirring means to heat the material.

Inventors

김은주
서창준
박성준

Assignees

주식회사 티앨씨

Dates

Publication Date: 20260507
Application Date: 20241031

Claims (12)

A first raw material (10) containing a lithium source; A second raw material (20) containing sulfur; A first raw material supply means (100) for storing and supplying the above first raw material under an inert gas atmosphere; A second raw material supply means (200) for storing and supplying the above second raw material; A first pulverization means (300) that receives a first raw material from the first raw material supply means and pulverizes it first through a blade mill; Cooling means (400) for lowering the temperature of the above first atomization means; A second micronization means (500) that receives the material that has passed through the first micronization means and performs a second micronization; and Packaging means (600) for packaging a substance that has been micronized by passing through the above second micronization means; and One or more of a sample inspection means (700), a centrifugation means (800), a wet stirring means (900), and an attrition mill (1000) are included between the first atomization means and the second atomization means, and A lithium sulfide synthesis process in which a heating means (1100) including an electric heater is connected to one or more of the above first atomization means or the above wet stirring means to heat.
In paragraph 1, A lithium sulfide synthesis process in which the first raw material comprises one or more of lithium metal or lithium oxide, and the second raw material comprises one or more of sulfur powder or hydrogen sulfide.
In paragraph 1, A lithium sulfide synthesis process in which, when the heating means is connected to the first atomization means, a sample inspection means and a centrifugation means are included between the first atomization means and the second atomization means.
In paragraph 1, A lithium sulfide synthesis process in which, when the heating means is connected to the wet stirring means, the wet stirring means and the attrition mill are included between the first atomization means and the second atomization means to perform wet milling.
In paragraph 2, When the heating means is connected to the first atomization means, the second raw material is supplied to the first atomization means and a reaction to synthesize lithium sulfide occurs. A lithium sulfide synthesis process in which, when the heating means is connected to the wet stirring means, the second raw material is supplied to the wet stirring means and synthesized into lithium sulfide.
In paragraph 1, A lithium sulfide synthesis process further comprising a solvent supply means for supplying a solvent to the above-mentioned wet stirring means.
In paragraph 5, A lithium sulfide synthesis process in which the lithium sulfide synthesized in the above wet stirring means is supplied to a second micronization means in a solvent-removed and dried state.
In paragraph 3, A lithium sulfide synthesis process in which lithium sulfide synthesized in the first micronization means is transferred to a centrifugation means when it meets a predetermined standard in a sample inspection means, and a first recovery procedure is carried out in which lithium sulfide, lithium, and sulfur that do not meet the standard are recovered, and in the centrifugation means, lithium sulfide and lithium are separated, and the lithium sulfide is transferred to a second micronization means, and a second recovery procedure is carried out in which lithium is recovered.
In paragraph 8, A lithium sulfide synthesis process in which lithium sulfide, lithium, and sulfur recovered through the above first and second recovery are reused in the process.
In paragraph 5, When the heating means is connected to the first atomization means, the ratio of the first raw material and the second raw material is 1:1 to 2:1, and A lithium sulfide synthesis process in which the ratio of the first raw material to the second raw material is 1:1 to 1:2 when the heating means is connected to the wet stirring means.
In paragraph 1, The above inert gas (30) is a lithium sulfide synthesis process comprising one or more inert gas supply means (1200) for storing and supplying inert gas to be used in any one or more of a first raw material preparation means, a second micronization means, and a packaging means.
In Paragraph 11, The above inert gas is connected to a cooling means to control the temperature in a lithium sulfide synthesis process.

Description

Lithium sulfide synthesis process using lithium and sulfur powder The present invention relates to a lithium sulfide synthesis process and provides a process for synthesizing lithium sulfide by selectively using multi-stage atomization and dry and wet means. Lithium sulfide (Li₂S) is an important material primarily used as a solid electrolyte or cathode material in energy storage devices such as lithium-ion batteries. Since the technology for synthesizing it with high purity directly affects battery performance, various synthesis methods are being researched. The background knowledge regarding the lithium sulfide synthesis technology related to the present invention is as follows. In addition, lithium sulfide can be obtained by directly reacting solid lithium with sulfur. While this method has the advantage of a simple process, the purity of the product and the reaction rate vary significantly depending on the reaction temperature and time. Furthermore, due to the risk of lithium oxidation and degradation at high temperatures, the reaction is often carried out in an inert gas atmosphere. In addition, the wet synthesis method, in which lithium and sulfur are dissolved in a solvent and reacted, allows for the reaction to take place at a lower temperature compared to solid-state reactions, thereby reducing the oxidation of lithium. Typically, lithium salts and hydrogen sulfide are dissolved in a solvent and reacted; by maintaining a specific temperature during this process, fine particles of lithium sulfide can be obtained. Wet synthesis has the advantage of being suitable for use as a battery electrode material because it facilitates uniform control of the reaction and is advantageous for controlling the particle size of the product. In addition, a method of producing lithium sulfide by reacting lithium metal with hydrogen sulfide (H₂S) gas at high temperatures is also widely used. While high-purity lithium sulfide can be obtained through a rapid reaction at high temperatures, safety is required when using highly toxic gases such as H₂S. This method is preferred for manufacturing materials for high-performance batteries because it allows for the synthesis of high-purity lithium sulfide within a short period of time at high temperatures. Korean Registered Patent Publication No. 10-2562588 relates to a method for producing high-purity lithium sulfide using a mixed organic solvent, comprising the step of a) raising a reaction solution containing lithium hydroxide (LiOH) and a mixed organic solvent to a temperature of 130°C or higher, and then injecting hydrogen sulfide (H2S) gas to react under a pressure higher than atmospheric pressure; wherein the mixed organic solvent is a mixture of an amide-based organic solvent and a sulfur-containing organic solvent, and the sulfur-containing organic solvent is one or more sulfite-based solvents selected from alkylene sulfite, dialkyl sulfite, diaryl sulfite, and alkyl aryl sulfite. Korean Registered Patent Publication No. 10-2562589 relates to a method for manufacturing high-purity lithium sulfide through wet and dry circulation processes, comprising: a) a step of heating a reaction solution containing lithium hydroxide (LiOH) and an organic solvent to 100°C or higher, then injecting hydrogen sulfide ( H₂S ) gas to react under a pressure higher than atmospheric pressure; b) a step of repeating the process of injecting hydrogen sulfide ( H₂S ) gas into the reaction solution and re-reacting at least once after the internal pressure of the reactor returns to atmospheric pressure following step a); c) a step of removing the organic solvent from the reaction solution after step b) to obtain a primary reaction product; d) a step of heating the primary reaction product to 100°C or higher, then injecting hydrogen sulfide ( H₂S ) gas into the reactor to react under a pressure higher than atmospheric pressure; and e) a step of using a vacuum pump to remove water and hydrogen sulfide ( H₂S ) gas generated as reaction by-products after step d). The present invention provides a method for producing lithium sulfide, comprising the steps of: a discharge step; and f) dehumidifying and filtering the water and hydrogen sulfide ( H₂S ) gas discharged through the vacuum pump, and then recirculating and reinjecting the hydrogen sulfide (H₂S) gas from which water has been removed back into the reactor and re-reacting it at least once, wherein the organic solvent is a mixed solvent comprising an aromatic organic solvent and a sulfur-containing organic solvent, wherein the volume ratio of the aromatic organic solvent to the sulfur-containing organic solvent in the mixed solvent is 1:0.1 to 10, and the sulfur-containing organic solvent is one or more sulfite-based solvents selected from alkylene sulfite, dialkyl sulfite, diaryl sulfite, and alkyl aryl sulfite. Korean Registered Patent Publication No. 10-2495178 relates to a method for manufacturing high-purity lithium sulfide through wet and dry