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The preparation method of lithium sulfide

A technology of lithium sulfide and lithium thiosulfate, applied in the directions of alkali metal sulfide/polysulfide, electrochemical generator, electrical components, etc., can solve the problems of high temperature and high energy consumption, and meet the requirements of safe operation and energy consumption. Low, batch production stable effect

Active Publication Date: 2022-04-15
天齐锂业(江苏)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing lithium sulfide preparation and synthesis methods are mainly divided into two categories: synthesis method and pyrolysis method. Among them, high temperature pyrolysis method includes: lithium sulfide precursor (lithium sulfate, lithium sulfite, lithium bisulfate, lithium dithionate One or more) and related reducing agents are prepared by reacting at high temperature, such as patents CN106229487A, CN108400327A, etc. Although lithium sulfide can be obtained by these methods, due to the high temperature required, the energy consumption is relatively high

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preparation example Construction

[0019] The preparation method of lithium sulfide of the present invention, its steps are as follows successively:

[0020] a. Grinding and mixing: mix and grind the sulfur source and the lithium source, add hydrazine hydrate while grinding, finish the grinding after adding, and obtain the reaction material; wherein, the sulfur source is sulfur powder, lithium thiosulfate or lithium sulfite ; The lithium source is lithium hydroxide, lithium thiosulfate or lithium sulfite;

[0021] b. Vacuum defoaming: put the reaction materials into a vacuum defoaming bucket, and vacuumize. After the bubbles are eliminated, keep the vacuum state for 1 to 4 hours, and then change the air pressure to normal pressure to obtain a lithium sulfide solution;

[0022] c. Drying: Lithium sulfide solution is dried to obtain lithium sulfide.

[0023] The method of the present invention adopts mixed grinding of sulfur source and lithium source to ensure that the raw materials can be fully contacted, and r...

Embodiment 1

[0038] Mole ratio Li 2 O:S:N 2 h 4 ·H 2Weigh lithium hydroxide monohydrate, sulfur powder and hydrazine hydrate in a ratio of O→1:2:4, mix lithium hydroxide monohydrate and sulfur powder and grind evenly, then slowly add hydrazine hydrate into the mixed powder, Grind while adding until the hydrazine hydrate is added completely. The obtained reaction material is put into a vacuum defoaming barrel, vacuumed to below 0.1MPa, and the reaction is continued until the bubbles are no longer generated, and then the vacuum state is maintained for 1 hour, and the valve of the vacuum defoaming barrel is opened until the air pressure reaches normal pressure. Transfer to a vacuum freeze dryer, carry out vacuum freeze drying at a low temperature of -50°C and a pressure below 100 Pa for 4 hours, vacuum cap the dried material and take it out to obtain the lithium sulfide product YP-1.

[0039] The composition parameter of gained product is shown in Table 1, and its XRD diffraction pattern ...

Embodiment 2

[0041] Mole ratio Li 2 O:S:N 2 h 4 ·H 2 Weigh lithium hydroxide monohydrate, sulfur powder and hydrazine hydrate in a ratio of O→1:1:2, mix and grind lithium hydroxide monohydrate and sulfur powder evenly, then slowly add hydrazine hydrate into the mixed powder, and add While grinding, until the hydrazine hydrate is added completely. The obtained reaction material is put into a vacuum defoaming barrel, vacuumed to below 0.1MPa, and the reaction is continued until the bubbles are no longer generated, and then the vacuum state is maintained for 4 hours. The valve of the vacuum defoaming barrel is opened until the air pressure reaches normal pressure, and the mixed liquid Transfer to a vacuum freeze dryer, carry out vacuum freeze drying at a low temperature of -60°C and a pressure below 100 Pa for 6 hours, vacuum cap the dried material and take it out to obtain the lithium sulfide product YP-2.

[0042] The composition parameter of gained product is shown in Table 1, and its ...

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Abstract

The invention relates to a preparation method of lithium sulfide, belonging to the technical field of lithium ion battery materials. The technical problem solved by the present invention is to provide a preparation method of lithium sulfide. The method uses mixed grinding of sulfur source and lithium source to ensure that the raw materials can be fully contacted. Under the condition of the reducing agent hydrazine hydrate, redox reaction occurs, and the conversion rate of lithium sulfide can reach more than 80%. Defoaming treatment, its operation is simple, the generated gas is processed by vacuum defoaming equipment, and after drying, lithium sulfide is purified, and the product purity can reach more than 95%. Therefore, using this method to prepare lithium sulfide has simple process and operability Strong, low energy consumption, low raw material requirements for equipment, stable batch production, no toxic gas, no secondary pollution, and can meet the requirements of safe operation and commercial lithium sulfide.

Description

technical field [0001] The invention relates to a preparation method of lithium sulfide, belonging to the technical field of lithium ion battery materials. Background technique [0002] With the development of modern science and technology, energy, environment and information technology have become the three most important areas of human society in the 21st century. The development of new energy has become an important task for the sustainable development of human beings. At present, various energy conversion and storage devices such as solar cells, fuel cells, lithium-ion batteries, and supercapacitors have been developed. Among them, lithium-ion batteries have been widely used in various portable electronic products because of their high operating voltage, long cycle life and stable discharge performance. [0003] With the emergence of new technologies, new energy vehicle technology has attracted more and more attention. People have put forward higher requirements on the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/24H01M10/056
CPCY02E60/10
Inventor 周复杨柳陈格邓红云徐川黄建成杨艳辉高宜宝
Owner 天齐锂业(江苏)有限公司
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