Preparation method of nanotube-shaped manganite lithium ion sieve absorbent

A manganese oxide and lithium ion technology is applied in the field of preparation of nano-tubular manganese oxide lithium ion sieve adsorbent, which can solve the problems of single adsorbent shape, low adsorption capacity, small specific surface area, etc., and achieve high-efficiency cycle Utilize performance, reduce production costs, and source a wide range of effects

Inactive Publication Date: 2018-12-25
QINGHAI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Based on the above-mentioned problems that the current spinel-type manganese oxide lithium ion sieve adsorbent has a single shape and a small specific surface area, resulting in low adsorption capacity and slow adsorption rate, the present invention discloses a simple inorganic material (KMnO 4 Manganese source, iron salt and dilute hydrochloric acid), using hydrothermal method, high temperature calcination method and ion exchange technology to obtain nanotube-shaped spinel lithium ion sieve adsorbent, which has strong ion selectivity and is environmentally friendly and recyclable Lithium ion sieve adsorbent

Method used

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  • Preparation method of nanotube-shaped manganite lithium ion sieve absorbent

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Embodiment 1

[0028] A preparation method of a nanotubular manganese oxide lithium ion sieve adsorbent, comprising the steps of:

[0029] (1) Preparation of γ-MnOOH

[0030] Weigh 0.50 g KMnO respectively 4 and 0.334g FeSO 4Dissolve in a mixed solution of 65mL of secondary water and 5mL of ethanol, stir to mix evenly; pour the mixed solution into the lining of a 100mL reactor, and react at 140°C for 20 hours after the reactor is installed. After the reaction was finished, the reaction kettle was taken out, allowed to cool down to room temperature naturally, and the product was suction filtered, washed with water, and then washed with ethanol, and washed twice repeatedly. Put the solid product in a drying oven with a temperature of 55°C to dry the moisture;

[0031] (2) Synthesis of LiMnO 2

[0032] Weigh 0.62g of γ-MnOOH prepared in step (1) and slowly add it to 70mL of LiOH solution with a concentration of 2mol / L. After mixing evenly, place the solution in the lining of a 100mL reacto...

Embodiment 2

[0039] (1) Preparation of γ-MnOOH

[0040] Weigh 1.1g KMnO respectively 4 and 0.684g (NH 4 ) 2 Fe(SO 4 ) 2 Dissolve in a mixed solution of 65mL of secondary water and 5mL of ethanol, stir to mix evenly; pour the mixed solution into the lining of a 100mL reactor, and react at 158°C for 26 hours after the reactor is installed. After the completion, take out the reaction kettle, allow it to cool down to room temperature naturally, then filter the product with suction, wash with water, then wash with ethanol, and wash repeatedly for 3 times, put the solid product in a drying oven with a temperature of 60°C, and dry the water;

[0041] (2) Synthesis of LiMnO 2

[0042] Weigh 0.94g of γ-MnOOH prepared in step (1) and slowly add to 70mL of LiOH·H with a concentration of 2mol / L 2 O solution, after mixing evenly, place the solution in a 100mL reaction kettle lining, and react at a temperature of 120°C for 14 hours after the reaction kettle is installed. Suction filtration, wash...

Embodiment 3

[0049] (1) Preparation of γ-MnOOH

[0050] Weigh 1.5g KMnO respectively 4 and 1.024g NH 4 FePO 4 Dissolve in a mixed solution of 65mL of secondary water and 5mL of ethanol, stir to mix evenly; pour the mixed solution into the lining of a 100mL reactor, and react at 180°C for 30 hours after the reactor is installed. After the completion, the reaction kettle was taken out, allowed to cool naturally to room temperature, and the product was subjected to suction filtration, washed with water, and then washed with ethanol, and washed repeatedly for 4 times, and the solid product was placed in a drying oven at a temperature of 75°C to dry the water;

[0051] (2) Synthesis of LiMnO 2

[0052] Weigh 1.35 g of γ-MnOOH prepared in step (1) and slowly add it to 70 mL of LiOH·H with a concentration of 2 mol / L 2 O solution, after mixing evenly, place the solution in a 100mL reactor lining, and react at a temperature of 130°C for 20 hours after the reactor is installed. After the react...

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Abstract

The invention relates to the field of preparation of inorganic materials (manganese oxide series), in particular to a preparation method of a nanotube-shaped manganite lithium ion sieve absorbent. Thepreparation method comprises the following four steps: preparing gamma-MnOOH; synthesizing LiMnO2; preparing a lithium ion sieve precursor Li4Mn5O12; and preparing a lithium ion sieve absorbent H4Mn5O12. The preparation method is simple, and the production cost for an existing method used at present can be reduced. The prepared lithium ion sieve adsorber H4Mn5O12 has a nanotube-shaped morphology,regular thorn-shaped substances grow on the surface of the lithium ion sieve adsorber H4Mn5O12, the specific surface area is large and is 90.979-92.997 m<2> / g, the lithium ion sieve adsorber with thespecial morphology has large adsorption capacity to lithium ions and high adsorption rate, wherein the adsorption capacity is 14.0-37.0 mg / g, the nanotube-shaped manganite lithium ion sieve absorbentis environmentally friendly, and has high-efficiency recycling property, and industrialized production is easy to realize. The preparation method of the nanotube-shaped manganite lithium ion sieve absorbent can be used for extracting lithium ions in an alkali metal competition system such as a salt lake.

Description

technical field [0001] The invention relates to the field of preparation of inorganic materials (manganese oxide series), in particular to a preparation method of a nanotube manganese oxide lithium ion sieve adsorbent. Background technique [0002] my country's salt lake Li + Abundant resources, research on how to extract and isolate Li from salt lakes + The significance is very significant. Currently for Li + The separation and extraction of resources mainly include precipitation, ion exchange, solvent extraction and adsorption. The precipitation method has the characteristics of simple operation, high efficiency and high purity, but it needs to evaporate a large amount of water in the early brine treatment process, which leads to high time cost, high energy consumption and complicated process, and it is not easy to treat brine containing a large amount of alkaline earth metals, especially Not suitable for treating low-concentration lithium-containing brine. The ion ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/04B01J20/28B01J20/30
CPCB01J20/04B01J20/28014B01J20/28059B01J20/30
Inventor 许乃才刘忠史丹丹李武董亚萍
Owner QINGHAI NORMAL UNIV
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