Lithium sulfide preparation method capable of realizing continuous production

A technology of lithium sulfide and lithium salt, which is applied in the direction of alkali metal sulfide/polysulfide, structural parts, electrical components, etc., can solve problems such as authenticity to be verified, and achieve the effect of promoting kinetics, reducing production costs, and shortening the process route effect

Active Publication Date: 2022-04-05
湖南恩捷前沿新材料科技有限公司
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  • Description
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Problems solved by technology

There is neither characteristic bulging of anti-oxidation film nor other impurity peaks in this drawing, so its authenticity needs to be verified.

Method used

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  • Lithium sulfide preparation method capable of realizing continuous production

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preparation example Construction

[0028] A kind of preparation method of the lithium sulfide that can realize continuous production that the present invention develops, main steps are as follows:

[0029] (1) Mix sulfur-containing lithium salt, organic carbon source and carbon material in proportion, disperse in organic solvent and wet mix;

[0030] (2) Press filter the resulting material and press it into a block in a mold, put the pressed material into a crucible, and use a tube furnace to sinter at a high temperature under the protection of fluid nitrogen, wherein sulfur powder is placed in the low temperature area, and sulfur powder is placed in the high temperature area. place materials;

[0031] (3) After the sintered material is crushed, it is dissolved in an alcohol solvent, and the solvent is removed in a vacuum oven to obtain lithium sulfide.

[0032] Step (1) is a material mixing process, mixing sulfur-containing lithium salt, organic carbon source and carbon material in proportion, and dispersing ...

Embodiment 1

[0043] Take 40g of lithium sulfate monohydrate, 5g of polyvinylpyrrolidone, and 5g of conductive carbon black and disperse in isopropanol, and use a high-speed mixer to mix at 1400rpm for 15min;

[0044] After the suspension is filtered, the filtrate is recovered, the filter cake is pressed into a square block in a mold and put into a crucible, the crucible is placed in the right temperature zone of the tube furnace, and the crucible containing a small amount of sulfur powder is placed in the left temperature zone;

[0045] Nitrogen gas is introduced from the left end of the tube furnace until the oxygen content in the tube furnace is less than 30ppm, the nitrogen flow rate is 100mL / min, the high temperature zone starts to heat up, and the nitrogen flow rate remains unchanged from the beginning of the temperature rise to the tube furnace cooling down to room temperature;

[0046] Heat the temperature in the high temperature zone to 250°C for 6 hours;

[0047] Heat the temperat...

Embodiment 2

[0055] Take 70g of lithium sulfate monohydrate, 15g of polydopamine, and 4g of conductive carbon black and disperse them in ethanol, and use a ball mill to mix the materials at 400rpm for 30min;

[0056] After the suspension is filtered, the filtrate is recovered, the filter cake is pressed into a square block in a mold and put into a crucible, the crucible is placed in the right temperature zone of the tube furnace, and the crucible containing a small amount of sulfur powder is placed in the left temperature zone;

[0057] Nitrogen gas is introduced from the left end of the tube furnace until the oxygen content in the tube furnace is less than 30ppm, the nitrogen flow rate is 300mL / min, the high temperature zone starts to heat up, and the nitrogen flow rate remains unchanged from the beginning of the temperature rise to the tube furnace cooling down to room temperature;

[0058] Heat the temperature in the high temperature zone to 280°C for 7 hours;

[0059] Heat the temperat...

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Abstract

The invention discloses a lithium sulfide preparation method capable of realizing continuous production. According to the method, lithium sulfide is prepared by adopting a lithium sulfide precursor and a carbon high-temperature pyrolysis reduction method. The lithium sulfide precursor coats the carbon to promote the reaction, meanwhile, a sulfur atmosphere in the furnace is provided by adopting a sulfur powder evaporation mode, sulfur volatilization of the lithium sulfide precursor at a high temperature is inhibited, and flowing nitrogen is adopted for atmosphere protection. The method does not need vacuumizing or negative pressure protection, can be continuously carried out at normal pressure, and can realize continuous production by selectively using a roller kiln or a pushed slab furnace during amplification, so that the production cost of lithium sulfide is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of production of lithium sulfide, and in particular relates to a preparation method of lithium sulfide capable of realizing continuous production. Background technique [0002] With the world's requirements for "carbon peaking and carbon neutrality", new energy vehicles have begun to be favored by governments around the world. However, because traditional lithium-ion batteries require the injection of electrolyte, the electrolyte is very likely to leak when the battery is impacted and squeezed, which may lead to fire or even explosion. The all-solid-state battery has received widespread attention because its electrolyte is in an all-solid form and its safety performance has been greatly improved. [0003] Most of the current lithium-ion batteries use lithium iron phosphate system or ternary system as the positive electrode, and match with graphite negative electrode. As the demand for energy density of lit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/26H01M4/1397H01M4/58
CPCY02E60/10
Inventor 刘芳洋杜岳勇张宗良
Owner 湖南恩捷前沿新材料科技有限公司
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