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Preparation method of battery-grade lithium sulfide

A lithium sulfide, battery-level technology, applied in battery electrodes, lithium batteries, secondary batteries, etc., can solve the problems of flammability, difficulty in control, and explosion of organic solvents, and achieve easy industrialization, low production costs, and low equipment requirements Effect

Pending Publication Date: 2022-05-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that organic solvents are flammable, explosive, volatile, serious environmental pollution, and not easy to recycle. The working conditions are highly dangerous and difficult to control
[0006] 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, it is necessary to explore low-cost, green and environmentally friendly Li 2 The S production method will have a profound impact on the development of the future energy battery field

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  • Preparation method of battery-grade lithium sulfide
  • Preparation method of battery-grade lithium sulfide
  • Preparation method of battery-grade lithium sulfide

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preparation example Construction

[0026] The design concept of the preparation method of battery-grade lithium sulfide proposed by the present invention is: in order to benefit the development of the energy battery field in the future, realize the industrialization of lithium sulfide production, produce as little waste as possible, reduce production costs, and be environmentally friendly. The main steps are: uniformly mixing metal magnesium and lithium source compound first, then calcining the mixture at high temperature to obtain the powder containing lithium sulfide. The calcined powder is impregnated and washed with an organic solvent to separate the insoluble matter, and the filtrate is crystallized and purified and then dried to obtain a crude lithium sulfide product, which can be further calcined at a high temperature to remove residual organic matter to obtain battery-grade lithium sulfide. In the present invention, lithium source compound adopts lithium sulfate, and the reaction that magnesium and lithi...

Embodiment 1

[0030] A preparation method of battery grade lithium sulfide, such as figure 1 As shown, the steps are: 0.233g magnesium powder (Mg) and 0.267g lithium sulfate (Li 2 SO 4 ) placed in a mortar (Mg and Li 2 SO 4 The molar ratio is 4:1), grind for 10 minutes, and mix the powder evenly; place the uniformly mixed magnesium powder and lithium sulfate mixture in a tube furnace, and calcinate at a high temperature of 550°C under an argon protective atmosphere, with a heating rate of 1°C / min, the temperature is maintained for 60 min; under the protection of argon atmosphere, the powder obtained by calcination is washed with absolute ethanol, and the insoluble matter (that is, the by-product MgO) is filtered out. ; Transfer the crude lithium sulfide product to a tube furnace, raise the temperature from room temperature at 5°C / min to 700°C under an argon protective atmosphere, and keep the temperature constant for 6 hours to obtain the lithium sulfide product. figure 2 It is powder...

Embodiment 2

[0032] A kind of preparation method of battery grade lithium sulfide, step is: with 0.367g magnesium powder (Mg) and 0.427g lithium sulfate (Li 2 SO 4 ) placed in a mortar (Mg and Li 2 SO 4 The molar ratio is 3.9:1), grind for 10min to mix the powder evenly; place the uniformly mixed magnesium powder and lithium sulfate mixture in a tube furnace, and calcinate at 600°C under an argon protective atmosphere with a heating rate of 5°C / min, and keep the temperature for 10 min; under the protection of argon atmosphere, wash the calcined powder with anhydrous isopropanol, filter out the insoluble matter, collect the clear liquid, and then evaporate the filtrate to crystallize and dry it to obtain the crude lithium sulfide product Transfer the crude lithium sulfide product to a tube furnace, raise the temperature from room temperature at 5°C / min to 600°C under an argon protective atmosphere, and keep the temperature constant for 12 hours to obtain the lithium sulfide product. im...

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Abstract

The invention discloses a preparation method of battery grade lithium sulfide, which mainly comprises the following steps: uniformly mixing metal magnesium and a lithium source compound, and calcining the mixture at high temperature to obtain powder containing lithium sulfide. And dipping and washing the powder obtained by calcining with an organic solvent, separating out insoluble substances, crystallizing and purifying the filtrate, drying to obtain a lithium sulfide crude product, and further calcining the lithium sulfide crude product at high temperature to remove residual organic matters to obtain the battery-grade lithium sulfide. According to the method, the battery-grade lithium sulfide is finally prepared, byproducts with high commercial value are separated in the preparation process, no waste is generated in the whole preparation process, in addition, a purification solvent in the synthesis process is not consumed and can be recycled, the concept of green chemistry is met, and good economical efficiency is achieved.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a preparation method and application of lithium sulfide. Background technique [0002] In recent years, the electric vehicle market has developed vigorously, but the range anxiety, long charging time, safety and other issues of vehicles have hindered the further expansion of its market share. The root of the above problems is the imperfect battery technology, so making a breakthrough in battery technology is the key to solving the problem. Lithium-sulfur batteries, lithium-oxygen batteries, all-solid-state batteries and other battery systems with high energy density are considered to be expected to solve the battery technical problems of electric vehicles and have attracted much attention. There are great advantages in all aspects, and the most commercial prospects; and lithium sulfide (Li 2 S) As a key material required for both battery systems—it can be used as t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/24H01M4/58H01M10/052H01M10/0562
CPCC01B17/24H01M4/5815H01M10/052H01M10/0562C01P2002/72C01P2002/85
Inventor 杨永安张欣
Owner TIANJIN UNIV