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Preparation method of high-purity nano-lithium oxide

A lithium oxide, high-purity technology, applied in the field of chemistry, can solve problems such as environmental pollution, potential safety hazards, and long distillation time, and achieve the effects of reducing production costs, reducing safety, and improving purity

Inactive Publication Date: 2019-02-15
天齐锂业(射洪)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned above, in existing literature, lithium hydroxide and hydrogen peroxide are roughly divided into two kinds of methods for raw material preparation lithium oxide: (1) add ethanol: improve the yield of lithium peroxide product with ethanol as dehydrating agent and cleaning agent and product purity, but the use of ethanol will increase the cost, and there are also potential safety hazards, which will pollute the environment
(2) No ethanol is added: Anhydrous lithium hydroxide and high-concentration hydrogen peroxide are used as raw materials. Carbon dioxide is easily introduced during the preparation of anhydrous lithium hydroxide, and the particle size also has certain requirements. Pressure distillation, long distillation time, high energy consumption, the whole process has certain restrictions on equipment and raw materials

Method used

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  • Preparation method of high-purity nano-lithium oxide
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  • Preparation method of high-purity nano-lithium oxide

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preparation example Construction

[0025] A kind of preparation method of high-purity nanoscale lithium oxide of the present invention, please refer to figure 1 , which includes the following process flow:

[0026] Mixing: adding hydrogen peroxide with a concentration of 30% into the reaction vessel and stirring, while stirring, slowly adding lithium hydroxide monohydrate with a purity of more than 99% into the reaction vessel to obtain a mixed solution, the mixed solution , calculated by weight percentage, hydrogen peroxide reacts stoichiometrically in excess of 3-20%;

[0027] Preliminary oxidation: place the reaction vessel in a vacuum drying oven, vacuumize, adjust the temperature to 80-120°C and keep it for the first predetermined time to obtain lithium peroxide containing crystal water;

[0028] Deep oxidation: continue vacuuming, adjust the temperature to 130-120°C and keep it for a second predetermined time to obtain lithium peroxide;

[0029] Thermal decomposition: continue vacuuming, adjust the temp...

Embodiment 1

[0037] Mixing: Add 2000mL of hydrogen peroxide with a concentration of 30% into the reaction vessel and stir, while stirring, slowly add 1.6kg of lithium hydroxide monohydrate with a purity of 99.9% into the reaction vessel, and continue stirring for 3 minutes after the addition is complete A well-mixed mixed solution was obtained, and the temperature was controlled at about 25° C. by means of an ice bath during the mixing process.

[0038] Preliminary oxidation: place the reaction vessel in a vacuum drying oven, evacuate to -0.01MPa, adjust the temperature to 80°C, and keep it warm for 4 hours to obtain lithium peroxide containing crystal water;

[0039]Deep oxidation: adjust the temperature in the vacuum drying oven to 130°C, keep the vacuum at -0.01MPa, and keep it warm for 4 hours to remove crystal water to obtain lithium peroxide.

[0040] Thermal decomposition: adjust the temperature in the vacuum drying oven to 350°C, keep the vacuum degree at -0.01MPa, and keep the tem...

Embodiment 2

[0046] Mixing: Add 5000mL of hydrogen peroxide with a concentration of 30% into the reaction vessel and stir, while stirring, slowly add 3.6kg of lithium hydroxide monohydrate with a purity of 99.5% into the reaction vessel, and continue stirring for 5 minutes after the addition is complete Obtain a well-mixed mixed solution, and use a water bath to control the temperature at about 45°C during the mixing process

[0047] Preliminary oxidation: put the reaction vessel in a vacuum drying oven, evacuate to -0.05MPa, adjust the temperature to 120°C, and keep it warm for 1 hour to obtain lithium peroxide containing crystal water;

[0048] Deep oxidation: adjust the temperature in the vacuum drying oven to 180°C, keep the vacuum at -0.05MPa, and keep it warm for 1 hour to remove crystal water to obtain lithium peroxide.

[0049] Thermal decomposition: adjust the temperature in the vacuum drying oven to 500°C, keep the vacuum degree at -0.05MPa, and keep the temperature for 1 hour to...

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Abstract

The invention provides a preparation method of high-purity nano-lithium oxide. The method comprises the following steps: mixing: hydrogen peroxide is added to a reactor and stirred, high-purity lithium hydroxide monohydrate is slowly added to the reactor during stirring, and a mixed solution is obtained; preliminary oxidation: the reactor is placed in a vacuum drying box and vacuumized, temperature is regulated to 80-120 DEG C and kept for a first predetermined duration, and lithium peroxide containing crystal water is obtained; deep oxidation: temperature in the vacuum drying box is regulatedto 130-120 DEG C and kept for a second predetermined duration, and lithium peroxide is obtained; thermal decomposition: the temperature in the vacuum drying box is regulated to 300-500 DEG C and keptfor a third predetermined duration, and lithium oxide is obtained; purification: the temperature in the vacuum drying box is regulated to 600-800 DEG C and kept for a fourth predetermined duration, and high-purity lithium oxide is obtained; milling and screening: high-purity lithium oxide obtained in the purification step is taken out and subjected to ball milling and screening, and nano-lithiumoxide is obtained.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of high-purity nano-scale lithium oxide. Background technique [0002] In recent years, lithium and lithium compounds have been more and more widely used in national life. As a new type of lithium-ion battery cathode material, it has attracted more and more attention and attention, and high-purity lithium oxide is a non- Water electrolyte, the battery made of it not only has the characteristics of general lithium battery, but also has the advantages of low cost and no pollution, which can be used in the manufacture of special glass and enamel, medicine, chemical industry and nuclear fusion reactor. [0003] At present, there are several methods for preparing lithium oxide at home and abroad: (1) metal lithium is heated to a molten state in a vacuum, and oxygen is introduced to oxidize to obtain lithium oxide. This method has a simple process and is easy t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/02B82Y40/00
CPCB82Y40/00C01D15/02C01P2004/62C01P2004/64C01P2006/80
Inventor 严新星邓红云陈格
Owner 天齐锂业(射洪)有限公司
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