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Preparation method of lithium sulfide

A technology of lithium sulfide and lithium element, applied in chemical instruments and methods, inorganic chemistry, lithium compounds, etc., can solve the problems of high production cost of lithium sulfide, harsh process requirements, long preparation process time, etc., and achieves low production cost and process. The effect of simple requirements and short preparation process

Pending Publication Date: 2022-04-26
SHENZHEN INST OF ADVANCED TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the problems of high production cost, long preparation process time and strict process requirements in the prior art, the purpose of the present invention is to provide a preparation method of lithium sulfide, which has the advantages of low production cost, simple process requirements, and safety High, short preparation process, simple product purification advantages

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  • Preparation method of lithium sulfide
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  • Preparation method of lithium sulfide

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preparation example Construction

[0028] The embodiment of the present invention provides a kind of preparation method of lithium sulfide, comprises the following steps:

[0029] S1. Dissolving the simple substance of lithium in the cyclic ether containing benzene series to obtain solution A; wherein, the mass ratio of the simple substance of lithium to the benzene series is 1: (1-10), when the simple substance of lithium and the benzene series When the mass ratio of lithium is in the range of 1: (1-10), the lithium element can completely react with the benzene series. The mass ratio of the lithium element to the benzene series can be, for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1: 9 or 1:10.

[0030] Specifically, the lithium element is selected from at least one of lithium strips, lithium sheets, lithium butyl, and lithium powder; the benzene series is selected from at least one of naphthalene, tetralin, and biphenyl; the ring The ether is at least one selected from tetrahydrofuran and dioxolane. ...

Embodiment 1

[0043] Carry out the following process steps in an anhydrous and oxygen-free argon glove box:

[0044] S1. Dissolve 0.6 g of butyl lithium in 10 mL of tetrahydrofuran solution with a concentration of 0.2 g / mL of naphthalene, stir until the butyl lithium is completely dissolved, and the solution turns dark green to black, and solution A is obtained.

[0045] S2. Dissolve 1.39g of sulfur powder in 8mL of carbon disulfide, stir until completely dissolved, and obtain solution B.

[0046] S3. In the condition of a cold water bath at 5°C, under the condition of stirring, add the solution A to the solution B, and the solution B does not boil; after the addition is completed, continue to stir for 60 minutes to obtain a suspension .

[0047] S4. The suspension is subjected to solid-liquid separation by centrifugation, and the solid phase is collected and washed twice with a tetrahydrofuran solution, and then dried to obtain a solid-phase lithium sulfide powder.

[0048] as the picture ...

Embodiment 2

[0052] Carry out the following process steps in an anhydrous and oxygen-free argon glove box:

[0053] S1. Dissolve 1.0 g of lithium powder in 10 mL of dioxolane solution with a biphenyl solubility of 0.6 g / mL, stir until the lithium butyl is completely dissolved, and the solution turns dark green to black, and solution A is obtained.

[0054] S2. Dissolve 1.39g of sulfur powder in 8mL of dimethyl sulfoxide, stir until completely dissolved, and obtain solution B.

[0055] S3. In the condition of a cold water bath at 10°C, under the condition of stirring, add the solution A to the solution B, and the solution B does not boil; after the dropwise addition, continue to stir for 60 minutes to obtain a suspension .

[0056] S4. The suspension is subjected to solid-liquid separation by centrifugation, and the solid phase is collected and washed twice with a dioxolane solution, and then dried to obtain a solid-phase lithium sulfide powder.

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Abstract

The preparation method of the lithium sulfide provided by the invention comprises the following steps carried out under the protection of an inert atmosphere: S1, dissolving a lithium elementary substance in cyclic ether containing benzene series to obtain a solution A; wherein the mass ratio of the lithium elementary substance to the benzene series is 1: (1-10); s2, dissolving elemental sulfur in an organic solvent to obtain a solution B; wherein the concentration of the elemental sulfur in the organic solvent is 0.01 g / mL to 0.3 g / mL; s3, mixing the solution A and the solution B according to the mass ratio of lithium elementary substance to sulfur elementary substance of (2-5): 1 to obtain a suspension; and S4, carrying out solid-liquid separation on the turbid liquid to obtain a solid-phase lithium sulfide product. The preparation method of lithium sulfide provided by the invention has the advantages of low production cost, simple process requirements, high safety, short preparation flow and simple product purification.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery materials, in particular to a preparation method of lithium sulfide. Background technique [0002] Safety is one of the key requirements for electric vehicles, next-generation portable electronic devices, and large-scale energy storage devices. Compared with the current commercial organic electrolyte-based lithium-ion batteries (LIBs), all-solid-state lithium batteries (ASSLBs) are expected to break through the development bottleneck of the existing liquid electrolyte LIBs due to their higher energy density and safety. However, during the development of early solid-state electrolytes, ASSLBs did not have any advantages in competing with LIBs in organic electrolytes due to their relatively low ionic conductivity. Recent studies have found that sulfide solid electrolytes have high ionic conductivity, and the room temperature lithium ion conductivity has reached or even exceeded that of ...

Claims

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Application Information

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IPC IPC(8): C01D15/00H01M10/052H01M10/0562
CPCC01D15/00H01M10/0562H01M10/052C01P2002/72C01P2004/03Y02E60/10
Inventor 韩金龙陆子恒杨春雷
Owner SHENZHEN INST OF ADVANCED TECH