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Manganese series lithium ion sieve adsorbent and preparation method of precursor thereof

A technology of lithium ion and adsorbent, which is applied in the field of preparation of manganese-based lithium ion sieve-type adsorbent and precursor, can solve problems such as difficult to meet industrialization requirements, long process flow, complicated process, etc., and achieve low raw material prices and low process flow Short, high adsorption selectivity effect

Active Publication Date: 2012-05-30
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the existing synthetic precursor Li by methods such as soft chemical method 1.6 mn 1.6 o 4 The process flow is long, the process is complicated, and it will produce a large amount of waste water, causing environmental pollution, and it is difficult to meet the problems and deficiencies of industrialization requirements. A preparation of lithium ion sieve adsorbent MnO 2 0.5H 2 A new method for O, which can be adapted to the industrial production of lithium adsorption from salt lake brine or seawater with low lithium concentration

Method used

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  • Manganese series lithium ion sieve adsorbent and preparation method of precursor thereof
  • Manganese series lithium ion sieve adsorbent and preparation method of precursor thereof
  • Manganese series lithium ion sieve adsorbent and preparation method of precursor thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Take MnO 2 Calcined at 680°C for 6h under air atmosphere to obtain Mn 2 o 3 .

[0028] (2) Take Mn 2 o 3 15.78g, LiOH·H 2 O 8.8g (lithium-manganese molar ratio 1.05: 1), using acetone as a dispersion medium, ground in a ball mill for 2 hours; after the mixture was dried, put it into a corundum crucible, and roast it under an inert atmosphere (nitrogen or argon) . After the temperature was raised to 800°C, the temperature was kept constant for 12 hours. After the synthesis, the sample was cooled with the furnace to obtain LiMnO 2 , its XRD pattern is attached figure 2 shown.

[0029] (3) put LiMnO 2Put it into a corundum crucible, place it in a furnace, and bake it at 450°C for 5 hours in an air atmosphere, and then cool it naturally to obtain the cubic lithium ion sieve precursor Li 1.6 mn 1.6 o 4 . The lithium ion sieve precursor Li 1.6 mn 1.6 o 4 Lithium ion sieve MnO was obtained after acid leaching with 0.5mol / L HCl for 2h, filtered and dried. ...

Embodiment 2

[0032] (1) Take Mn 2 o 3 15.78g, Li 2 CO 3 7.97g (lithium-manganese mol ratio 1.08: 1), with dehydrated alcohol as dispersion medium, grinds 2 hours in ball mill machine; After the mixture after grinding is dried, put into corundum crucible, under inert atmosphere (nitrogen or argon gas ) Roasting. After the temperature rises to 750°C, keep the temperature for 12 hours. After the synthesis, the sample is cooled with the furnace to obtain LiMnO 2 .

[0033] (2) put LiMnO 2 Put it into a corundum crucible, place it in a furnace, and bake it at 500°C for 5 hours in an air atmosphere, and then cool it naturally to obtain the cubic lithium ion sieve precursor Li 1.6 mn 1.6 o 4 . The lithium ion sieve precursor Li 1.6 mn 1.6 o 4 Lithium ion sieve MnO was obtained after acid leaching with 0.5mol / L sulfuric acid for 2h, filtered and dried. 2 0.5H 2 O. The adsorption analysis of the ion sieve is the same as (4) in Example 1.

Embodiment 3

[0035] (1) Take Mn 2 o 3 15.78g, Li 2 CO 3 7.97g (lithium-manganese molar ratio 1.08: 1), with absolute ethanol as dispersion medium, grind in ball mill for 2 hours; After the mixture after grinding is dried, put into corundum crucible, under inert atmosphere (nitrogen or argon) Roasting. After the temperature was raised to 500°C, the temperature was kept constant for 24 hours. After the synthesis, the sample was cooled with the furnace. LiMnO can be obtained after roasting 2 .

[0036] (2) put LiMnO 2 Put it into a corundum crucible, place it in a furnace, and bake it at 600°C for 5 hours in an air atmosphere, and then cool it naturally to obtain the cubic lithium ion sieve precursor Li 1.6 mn 1.6 o 4 . The lithium ion sieve precursor Li 1.6 mn 1.6 o 4 Lithium ion sieve MnO was obtained after acid leaching with 0.5mol / L HCl for 2h, filtered and dried. 2 0.5H 2 O. Lithium ion sieve MnO 2 0.5H 2 The adsorption and analysis process of O is the same as step (4...

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Abstract

The invention discloses a method for preparing a manganese series lithium ion sieve adsorbent, and relates to a method for preparing an inorganic adsorbent for adsorbing lithium from liquid lithium resources such as brine of salt lake, seawater and the like. In the method, a cubic crystal ion sieve precursor Li1.6Mn1.6O4 is prepared from Mn2O3 and LiOH or Li2CO3 serving as raw materials by using two sections of solid-phase reactions, wherein the precursor also can be used as an anode material of a lithium ion battery. The precursor is acidized to obtain a lithium ion sieve adsorbent MnO2.0.5H2O (or expressed as H1.6Mn1.6O4), and the ion sieve is the lithium adsorbent which has high selectivity on lithium. The method has the advantages of simple and readily available raw materials, simple process, high adsorption capacity of the ion sieve, low cost, high purity of products and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a manganese-based lithium ion sieve-type adsorbent and a preparation method of its precursor, in particular to a method for the preparation of lithium ions in lithium-containing solutions such as salt lake brine, seawater, and groundwater with high selectivity and high adsorption capacity. Lithium adsorbent MnO with good cycle performance 2 0.5H 2 O preparation method. Background technique [0002] Lithium and lithium salts have a very wide range of uses in lithium batteries, aerospace, nuclear reactions and other fields, and are known as "energy metals and metals that push the world forward". With the continuous high consumption of lithium resources, the original lithium ore resources mainly based on hard rock raw materials are gradually exhausted, and the extraction of lithium and its compounds from lithium-containing liquid resources such as salt lake brine, seawater, and geothermal water will gradually become an important...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/04B01J20/30C01G45/02
Inventor 石西昌周定方张志兵徐徽陈白珍陈亚杨喜云
Owner CENT SOUTH UNIV
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