Preparation method of high-purity lithium sulfide

A lithium sulfide, high-purity technology, applied in the direction of alkali metal sulfide/polysulfide, etc., can solve the problems of no index control and many impurities.

Active Publication Date: 2021-04-20
天齐锂业(江苏)有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

There are serious authenticity problems in this method. The lithium sulfide obtained according to the method of this patent is not high-purity lithium sulfide, but a mixture containing lithium sulfide, because after the method is calcined by a simple reduction reaction, the calcined product is more or less The problem of excessive carbon is rarely present, and there may also be side reaction impurities such as lithium carbonate. Therefore, there are more impurities, and it does not provide corresponding index control (comprising index type and index content) in the embodiments. At the same time We have proved through a large number of experiments that the method and steps of this patent cannot obtain 99.9% of lithium sulfide products

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[0026] The preparation method of high-purity lithium sulfide of the present invention, its steps are as follows successively:

[0027] a. Mixing materials: lithium sulfide precursor and sugar reducing agent according to Li 2 The molar ratio of O and C is mixed at 1:2.5~6 to obtain a mixed material; wherein, the lithium sulfide precursor is at least one of lithium sulfate, lithium sulfite, lithium bisulfate, and lithium dithionate;

[0028] b. Heating reaction: under the protection of vacuum or inert gas, react the mixed material at 200-300°C for 2-6h; then react at 400-600°C for 2-6h; then react at 675-775°C for 2-6h, cool to obtain reacted material;

[0029] c. Leaching, filtering and drying: add the reacted material to anhydrous alcohols, then filter, and the filtrate is dried to obtain high-purity lithium sulfide.

[0030] By adopting the method of the invention, high-purity lithium sulfide can be prepared, the purity of which is more than or equal to 99.9%, and the metho...

Embodiment 1

[0046] 1) Take 60g of AR grade anhydrous lithium sulfate and 49.1g of AR grade sucrose, mix and grind to 200-300 mesh;

[0047] 2) Melt-coat the uniformly ground material obtained in the previous step at 200°C for 4 hours under the protection of an inert gas or in a vacuum environment;

[0048] 3) Continue to carbonize and coat the molten coating material obtained in the previous step at 400°C for 6 hours under inert gas protection or vacuum environment;

[0049] 4) Continue to reduce and calcinate the carbonized coated material obtained in the previous step at 775°C for 2 hours under the protection of an inert gas or in a vacuum environment;

[0050] 5) After the material obtained in the previous step is cooled to normal temperature, it is dissolved in absolute ethanol at a mass solid-to-liquid ratio of 1:200, and then filtered, and the filtrate is kept for use, and the filter residue is washed with 5% hydrogen peroxide.

[0051] 6) The filtrate obtained in the previous step...

Embodiment 2

[0053] 1) Take 300g of AR grade lithium sulfite and 320g of AR grade glucose and mix and grind to 300-400 mesh;

[0054] 2) Melt-coat the uniformly ground material obtained in the previous step at 250°C for 3 hours under the protection of an inert gas or in a vacuum environment;

[0055] 3) Continue to carbonize and coat the molten coating material obtained in the previous step at 500°C for 3 hours under the protection of an inert gas or in a vacuum environment;

[0056] 4) Continue to reduce and calcinate the carbonized coated material obtained in the previous step at 750°C for 3 hours under the protection of inert gas or in a vacuum environment;

[0057] 5) After the material obtained in the previous step is cooled to normal temperature, it is dissolved in anhydrous methanol according to the mass solid-to-liquid ratio of 1:250, and then filtered, and the filtrate is kept for use, and the filter residue is washed with 10% hydrogen peroxide.

[0058] 6) The filtrate obtained ...

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Abstract

The invention relates to a preparation method of high-purity lithium sulfide, and belongs to the technical field of preparation of lithium sulfide. The technical problem to be solved by the invention is to provide the preparation method of the high-purity lithium sulfide. The method mainly comprises the following steps: reacting a lithium sulfide precursor (one or more of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate) with a related reducing agent at high temperature to prepare a lithium sulfide-containing substance, and leaching and purifying the lithium sulfide in the mixture; and finally, carrying out spray drying to obtain a lithium sulfide product with purity of 99.9% or above and controllable morphology. The method is simple and easy to operate, free of toxic organic solvents, safe and environmentally friendly, the purity of the obtained lithium sulfide is high and can reach 99.9% or above, the morphology is controllable, and the degree of sphericity is high.

Description

technical field [0001] The invention relates to a method for preparing high-purity lithium sulfide, and belongs to the technical field of lithium sulfide preparation. Background technique [0002] With the rapid development of new energy vehicles, the demand for power batteries of new energy vehicles is mainly concentrated in two aspects of long battery life and high safety. At present, the energy density of liquid lithium-ion battery cells can reach 240-260kw h / kg, which is close to the limit of 300kw h / kg. [0003] In recent years, there have been many electric vehicle fire accidents at home and abroad. The main reason is the power battery itself. Since the liquid lithium-ion battery uses a low flash point electrolyte and a high energy density ternary cathode material, it is prone to safety hazards. [0004] How to solve the contradiction between high energy density and high safety is imminent. Lithium sulfide (Li2S) is used as a cathode material for lithium-sulfur batte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/22
CPCY02E60/10
Inventor 周复陈格杨柳邓红云徐川黄建成何霞高宜宝
Owner 天齐锂业(江苏)有限公司
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