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A method for preparing lithium oxide or single crystal lithium hydroxide

A technology of lithium hydroxide monohydrate and lithium hydroxide, which is applied in the field of materials, can solve the problems of long reaction time, long process flow, and low productivity, and achieve the effects of low production cost, simple and practical process flow, and good storage

Active Publication Date: 2016-01-13
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for producing lithium oxide include: metal lithium is heated to a molten state in vacuum, and oxygen is directly oxidized to obtain lithium oxide. This method has a simple process and is easy to operate, but the yield is low; high-purity lithium carbonate is heated to 700 ℃ heat preservation for 50h, this method has a long reaction time and high energy consumption; anhydrous lithium hydroxide can be heated and decomposed under vacuum to obtain 98% lithium oxide, but anhydrous lithium hydroxide is easy to react with carbon dioxide in the air and is not easy Preservation; Lithium hydroxide monohydrate first reacts with hydrogen peroxide to produce lithium peroxide, and then heats lithium peroxide under vacuum conditions to produce lithium oxide. This method can prepare relatively pure lithium oxide, but the process flow is long and the productivity is low. lower

Method used

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  • A method for preparing lithium oxide or single crystal lithium hydroxide
  • A method for preparing lithium oxide or single crystal lithium hydroxide
  • A method for preparing lithium oxide or single crystal lithium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A device for preparing lithium oxide or single crystal lithium hydroxide such as image 3 As shown, the crucible 3 for placing the reaction material is located in the iron crucible 13, and the inside of the iron crucible 13 is communicated with the vacuum pipeline 7 through a vacuum bellows 6, the vacuum pipeline 7 is communicated with the cold trap 11, and the cold trap 11 is communicated with the vacuum pump 12;

[0036] The vacuum pipeline 7 is provided with a resistance gauge 8 and a resistance vacuum gauge 9;

[0037] A diaphragm valve 5 is provided on the vacuum bellows 6 between the inside of the iron crucible 10 and the vacuum pipeline 7;

[0038] The iron crucible 10 is located in the resistance furnace 4, and the resistance furnace 4 is also provided with a thermocouple 2 and a temperature controller 1; the temperature measured by the thermocouple 2 is the temperature at the outer wall of the iron crucible 13;

[0039] Using the above device, put lithium hydr...

Embodiment 2

[0047] The device for preparing lithium oxide or single crystal lithium hydroxide is the same as in Example 1;

[0048] Put lithium hydroxide monohydrate in a corundum crucible, cover the corundum crucible cover; place the corundum crucible in an iron crucible, cover the top cover of the iron crucible, and seal it with bolts; evacuate to 50~150Pa by a vacuum pump;

[0049] The material of the corundum crucible used is alumina with a weight purity ≥ 99%;

[0050] Heat lithium hydroxide monohydrate to 120°C through a resistance furnace, keep it warm for 2 hours, and remove free water;

[0051] Under the condition of vacuum degree of 50~150Pa, heat the material in the corundum crucible to 250°C, keep it warm for 2 hours, and remove the crystal water;

[0052] Under the condition of vacuum degree of 50~150Pa, heat the material in the corundum crucible to 1000℃ at a speed of 5~15℃ / min, and keep it warm for 4h;

[0053] After the heat preservation is over, under the condition of v...

Embodiment 3

[0056] The device for preparing lithium oxide or single crystal lithium hydroxide is the same as in Example 1;

[0057] Put lithium hydroxide monohydrate in a corundum crucible, cover the corundum crucible cover; place the corundum crucible in an iron crucible, cover the top cover of the iron crucible, and seal it with bolts; evacuate to 50~150Pa by a vacuum pump;

[0058] The material of the corundum crucible used is alumina with a weight purity ≥ 99%;

[0059] Heat lithium hydroxide monohydrate to 100°C through a resistance furnace, keep it warm for 2.5 hours, and remove free water;

[0060] Under the condition of vacuum degree of 50~150Pa, heat the material in the corundum crucible to 220°C, keep it warm for 2.5h, and remove the crystal water;

[0061]Under the condition of vacuum degree of 50~150Pa, heat the material in the corundum crucible to 900℃ at a speed of 5~15℃ / min, and keep it warm for 6h;

[0062] After the heat preservation is over, under the condition of vacu...

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Abstract

A method for preparing lithium oxide or single crystal lithium hydroxide, which belongs to the field of material technology and is carried out according to the following steps: (1) Place lithium hydroxide monohydrate in a crucible, and then heat it to 90 under a vacuum of 50~150Pa ~120℃, keep for 2~3h; (2) Heat the lithium hydroxide monohydrate with free water removed to 200~250℃ under a vacuum of 50~150Pa, keep it for 2~3h, and then heat it at 5~15℃ / min Raise the temperature to 700~1000℃ at a fast speed and keep it warm for 4~10h; (3) Under the condition of vacuum degree of 50~150Pa, cool the material in the crucible to 70~100℃ with the furnace, and then place the crucible in the glove box to At room temperature, lithium oxide or single crystal lithium hydroxide is obtained. Compared with the traditional method, the method of the present invention has the advantages that the raw materials used are easy to obtain and easy to preserve, the process flow adopted is simple and practical, the production cost is relatively low, and the equipment investment is small; the obtained product has high purity, high yield, and high quality. Stablize.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a method for preparing lithium oxide or single crystal lithium hydroxide. Background technique [0002] In recent years, lithium and lithium compounds have been more and more widely used in national life. For example, lithium-ion secondary batteries are widely used in notebook computers, mobile communications, and electric tools. Lithium oxide is one of the main raw materials for preparing electrode materials in lithium batteries. In addition, lithium oxide also has important applications in glass industry, ceramic industry, metallurgical industry and other fields. [0003] At present, the methods for producing lithium oxide include: metal lithium is heated to a molten state in vacuum, and oxygen is directly oxidized to obtain lithium oxide. This method has a simple process and is easy to operate, but the yield is low; high-purity lithium carbonate is heated to 700 ℃ heat pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B1/10C30B29/10
Inventor 高炳亮王兆文张世镖石忠宁胡宪伟于江玉
Owner NORTHEASTERN UNIV LIAONING