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Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof

A lithium ion and adsorbent technology, applied in the field of preparing lithium ion sieve H4Mn5O12 and its precursor, can solve the problems of unfavorable large-scale production, complex process, harsh conditions, etc., and achieve easy control of product ratio, good cycle stability, The effect of large adsorption capacity

Inactive Publication Date: 2011-03-16
CENT SOUTH UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the synthesis of these two materials mostly adopts the intermediate product synthesized by hydrothermal method, which has complicated process, harsh conditions, high production cost and small output, which is not conducive to large-scale production.

Method used

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  • Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof
  • Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof
  • Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof

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Embodiment 1

[0026] According to attached figure 1 As shown in the synthesis process, accurately weigh 4.0808 g of lithium acetate and 12.255 g of manganese acetate, add distilled water to dissolve, and obtain a mixed solution. The mixed solution was added dropwise into a citric acid solution containing 18.912 g of citric acid, and reacted in a constant temperature water bath at 80° C. for 1 h. Then the reaction product was dried in an oven at 120° C. to obtain a yellow solid. Grind the yellow solid and put it into a box furnace at a rate of 5°C / min to 400°C for 12 hours, then cool naturally to obtain the spinel lithium ion sieve precursor Li 4 mn 5 o 12 ,Such as figure 2 shown. The lithium ion sieve precursor Li 4 mn 5 o 12 Use 0.5mol / L HCl acid leaching for 24h to obtain lithium ion sieve 4 mn 5 o 12 ,Such as figure 2 shown. image 3 and Figure 4 Respectively, the obtained lithium ion sieve precursor Li 4 mn 5 o 12 SEM images before and after acid leaching. Weigh 0.3...

Embodiment 2

[0028] according to figure 1 As shown in the synthesis process, accurately weigh 4.0808 g of lithium acetate and 12.255 g of manganese acetate, add distilled water to dissolve, and obtain a mixed solution. The mixed solution was added dropwise into a citric acid solution containing 9.456 g of citric acid, and reacted in a constant temperature water bath at 80° C. for 1 h. Then the reaction product was dried in an oven at 120° C. to obtain a yellow solid. After grinding the yellow solid, put it into a box furnace at a rate of 5°C / min to 350°C for 12 hours, then cool it naturally to obtain the lithium ion sieve precursor Li 4 mn 5 o 12 . The lithium ion sieve precursor Li 4 mn 5 o 12 With 0.7mol / L HCl acid leaching for 24h, the lithium ion sieve H 4 mn 5 o 12 . Weigh 0.3g lithium ion sieve H 4 mn 5 o 12 Put in 30ml containing Li + 250mg / L in a certain salt lake brine, after 24 hours of adsorption equilibrium, the measured adsorption capacity is 10mg / g.

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Abstract

The invention provides a method for preparing a manganese series lithium-ion sieve adsorbent H4Mn5O12 and a precursor thereof, relating to a preparation method of an inorganic adsorbent for absorbing lithium from liquid lithium resources such as salt brine, seawater, geothermal water and the like. In the preparation method, manganese salts and lithium salts with low melting points are taken as raw materials, organic carboxylic acid is used as an ingredient, the precursor Li4Mn5O12 is obtained through soft chemical synthesis and low-temperature roasting; acid treatment is carried out on the precursor, and Li in the precursor is extracted to be converted to an H-type ion sieve represented by H4Mn5O12 or MnO2.0.31H2O; and the H-type ion sieve H4Mn5O12 is filtered, washed and dried to obtain the adsorbent capable of sieving lithium ions. The method of the invention has simple process, and the obtained ion sieve has the advantages of small dissolving loss, fast adsorption rate and high adsorption capacity.

Description

technical field [0001] The present invention relates to a kind of preparation method of lithium ion sieve adsorbent, especially preparation lithium ion sieve H 4 mn 5 o 12 (or MnO 2 0.31H 2 O) and methods of its precursors. Background technique [0002] Lithium and its compounds are widely used in metallurgy, pharmaceuticals, chemical power sources, alloy materials, nuclear fusion power generation and other fields, and the market demand is strong. However, the world's lithium ore reserves are far from meeting the market demand, and they are increasingly depleted. Salt lake brine, groundwater, and seawater contain huge lithium resources, which have become the focus of development and research in the lithium industry at home and abroad in recent years. Liquid lithium mineral resources will become the main resource for lithium extraction. [0003] my country is a country with a large amount of salt lake resources, and it is of great significance to study the comprehensive...

Claims

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Application Information

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IPC IPC(8): B01J20/04B01J20/30C01G45/02
Inventor 石西昌马立文陈白珍徐徽陈亚杨喜云
Owner CENT SOUTH UNIV
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