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Preparation of spinel type Li-Mn-oxide lithium ion screening materials by hydrothermal method

A technology of lithium manganese oxide and lithium ions, which is applied in the direction of manganese compounds, inorganic chemistry, chemical instruments and methods, etc., can solve the problems of expensive metal organics, unfavorable large-scale production, harsh process conditions, etc., and achieve high selectivity, Uniform composition and simple preparation process

Inactive Publication Date: 2005-11-30
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these existing technologies can control the particle size, morphology, composition and even microstructure of the product, the production process is relatively complicated and the process conditions are relatively harsh, which is not conducive to large-scale production; and the raw materials used generally require the use of more expensive metal organic compounds. , higher production cost

Method used

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  • Preparation of spinel type Li-Mn-oxide lithium ion screening materials by hydrothermal method
  • Preparation of spinel type Li-Mn-oxide lithium ion screening materials by hydrothermal method
  • Preparation of spinel type Li-Mn-oxide lithium ion screening materials by hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: Accurately weigh analytically pure (CMD) MnO2 8.6940g, analytically pure LiOH·H 2 O 4.1960g, after mixing the two, grind them with agate at room temperature and transfer them to a 50mL hydrothermal reaction kettle, add 25mL of distilled water, seal the hydrothermal reaction kettle after stirring vigorously for 5min, put it into a constant temperature oven at 160°C for 48h, take it out and cool it naturally After filtering, wash with distilled water until the filtrate PH=8, the obtained solid is dried at 100°C and sent to a high-temperature furnace for pre-calcination in an air atmosphere at 300°C for 2 hours, and then roasted in an air atmosphere at 600°C for 12 hours. Furnace cooling, the resulting product has uniform particle size, detected by XRD, its characteristic diffraction peak (see attached figure 2 ) and LiMn with spinel structure on the JCPDS diffraction card 2 o 4 The characteristic diffraction peaks are completely consistent and the peak in...

Embodiment 2

[0022] Embodiment 2: Accurately weigh analytically pure Mn 2 o 3 7.8940g, analytically pure LiOH·H 2 O 5.0352g, after the two are mixed, grind with agate at room temperature and then transfer to a 50mL hydrothermal reaction kettle, add 30mL of distilled water and stir vigorously for 5min, then seal the hydrothermal reaction kettle, and then send it to 140°C for 3

[0023] Insulate in a warm oven for 72 hours, take it out to cool naturally, filter, wash with distilled water until the filtrate pH = 7.5, dry the obtained solid at 105°C, send it to a high-temperature furnace for pre-calcination in an air atmosphere at 300°C for 2 hours, and then heat it at 700°C After roasting in the air atmosphere for 12 hours, the sample was cooled with the furnace, and the obtained product had a uniform particle size. The characteristic diffraction peaks (see attached image 3 ) and LiMn with spinel structure on the JCPDS diffraction card 2 o 4 The characteristic diffraction peaks are comp...

Embodiment 3

[0024] Example 3: Accurately weigh 8.7940 g of analytically pure γ-MnOOH, analytically pure LiOH·H 2 O 12.5880g, after mixing the two, grind them with agate at room temperature and transfer them to a 100mL hydrothermal reaction kettle, add 60mL of distilled water, seal the hydrothermal reaction kettle after stirring vigorously for 5min, put it into a constant temperature oven at 120°C for 24h, take it out and cool it naturally After filtration, wash with distilled water until the filtrate PH=8, the obtained solid is dried at 80°C and sent to a high-temperature furnace for pre-calcination in an air atmosphere at 300°C for 2 hours, and then roasted in an air atmosphere at 500°C for 8 hours. Furnace cooling, the resulting product has a uniform particle size, detected by XRD, characteristic diffraction peaks (see attached Figure 4 ) and LiMn with spinel structure on the JCPDS diffraction card 2 o 4 The characteristic diffraction peaks are completely consistent and the peak inte...

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Abstract

The invention relates to a hydrothermal production method of lithium ion bolting material of lithium-manganese oxide compound, which comprises the following steps: batching lithium oxidate and manganese oxidate with mole ratio of 0.5-3.0:1; delivering it to high-pressure hydrothermal autoclave after adequate mixing and grinding; adding distilled water to the mixture and processing it under 100-24 0 DEG C with 4-96h after full mixing; after filtering and rinshing to get colature of pH=7 to 8; drying it under 40-120 DEG C and processing preparatory roasting under 300 DEG C for 2h; roasting it under 300-800 DEG C in air atmosphere for 1-24h. The invention can get spinel structure lithium-manganese oxide of good crystal perfection, stable structure, and equal component. Said lithium-manganese oxide compound ionic screened material has the advantages of high selectivity and adsorption capacity when it is used to extract lithium resource from seawater and Salt Lake. The invention has the advantages of simple manufacturing process, mild conditioned response, cheap and available material and low cost of manufacture. Said lithium-manganese oxide compound can be used as electrode material of lithium ion secondary battery.

Description

technical field [0001] The invention relates to a method for preparing a lithium ion screening material by a hydrothermal method, in particular to a method for preparing a lithium manganese oxide lithium ion screening material by a hydrothermal method. Background technique [0002] Lithium resources are important strategic resources. It has great application prospects in energy conversion and aerospace technology. In recent years, with the development of lithium battery technology, the consumption of lithium has been increasing at a rate of 7-11% per year. According to statistics, in 2003, the world's total annual output of lithium exceeded 100,000 tons in terms of lithium carbonate. However, the total reserves of lithium in land ores are small. After hundreds of years of mining, they are on the verge of depletion, which is far from meeting the needs of industrial production. Therefore, the development of lithium resources from the resource-rich salt lake brine has become...

Claims

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Application Information

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IPC IPC(8): C01G45/00
Inventor 雷家珩杨顺林郭丽萍童辉
Owner WUHAN UNIV OF TECH
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