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Preparation of three-dimensional macropore-mesopore lithium ion sieve

A three-dimensional macroporous, lithium ion technology, applied in the field of nanomaterials, can solve the problems of increased mass transfer resistance, decreased adsorption capacity, and decreased adsorption rate, and achieves the effects of increasing adsorption capacity, increasing adsorption rate, and large specific surface area.

Inactive Publication Date: 2017-11-07
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, commonly used titanium sources are prone to hydrolysis, and there are relatively few studies on the structure-activity relationship of lithium titanate.
The titanium-based lithium ion sieves prepared at this stage are mainly bulk materials, and the exposed lithium ion vacancies on the surface are few, while the granulation or film casting process further increases the mass transfer resistance, reduces the adsorption rate, and reduces the adsorption capacity.

Method used

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  • Preparation of three-dimensional macropore-mesopore lithium ion sieve
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  • Preparation of three-dimensional macropore-mesopore lithium ion sieve

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Embodiment 1

[0038] Preparation of Opal Polystyrene Hard Templates

[0039] Add 0.45 g of sodium dodecylbenzenesulfonate and 0.6 g of potassium persulfate into a three-necked round-bottomed flask filled with 150 ml of water and 270 ml of ethanol, and dissolve under magnetic stirring at room temperature. After the solid was dissolved, the temperature of the solution was raised to 71 °C under the protection of nitrogen, and then 36 ml of styrene was quickly injected into the three-necked flask with a needle (the styrene needs to be washed with 0.5 mol / L NaOH solution first to remove the polymerization inhibitor), Stir evenly to generate a vortex, and reflux at 71 °C for 19 h to obtain a milky white solution. The obtained solution was filtered with absorbent cotton to remove large agglomerates, and bottled for preservation. Add the prepared polystyrene emulsion into a beaker, the height of the solution is preferably 1-2 cm, and place the beaker in an oven at 70 °C until the solvent evaporate...

Embodiment 2

[0041] Three-dimensional macroporous-mesoporous lithium titanate 3DM-Li 4 Ti 5 o 12 Precursor preparation

[0042] Add 1.32 g of anhydrous lithium acetate, 0.55 g of P123, 17 mL of glacial acetic acid, and 37 mL of isopropanol into a round bottom flask, stir magnetically until the solids dissolve, then pipette 7.4 mL of isopropyl titanate In the round bottom flask, continue stirring for 10 min to obtain a light yellow homogeneous solution.

Embodiment 3

[0044] Three-dimensional macroporous-mesoporous lithium titanate 3DM-Li 4 Ti 5 o 12 preparation of

[0045] The prepared lithium titanate precursor solution was injected into the block polystyrene template, and after it was completely wetted, it was placed in an oven at 70 °C for 24 h at room temperature after the solvent evaporated. Using the step-by-step calcination method, the bulk product was first calcined in a muffle furnace at 200 °C for 2 h with a heating rate of 1 °C / min, and then the temperature was raised to 600 °C for 6 h with a heating rate of 1 °C / min .

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Abstract

The invention relates to the preparation and application of a lithium ion sieve with a three-dimensional macropore-mesoporous structure. The lithium-ion sieve uses polystyrene microsphere arrays as a template, and isopropyl titanate and anhydrous lithium acetate as titanium and lithium sources, and obtains titanic acid with a three-dimensional macroporous-mesoporous structure by infusion and calcination. Lithium 3DM‑Li4Ti5O12. Finally, 3DM‑Li4Ti5O12 was delithiated by acid leaching to obtain a three-dimensional macroporous‑mesoporous lithium ion sieve 3DM‑H4Ti5O12. The macropore structure in the lithium ion sieve is arranged regularly, and the pores are connected through mesopores, forming a three-dimensional macropore-mesopore structure in which the channels are interconnected. Compared with other materials, the unique pore structure of the lithium ion sieve is conducive to the entry of lithium ions into the pores from all directions, reducing the internal diffusion resistance of lithium ions, reducing the adsorption-desorption equilibrium time of lithium ions, and increasing the adsorption capacity of lithium ions. The above many advantages make the lithium ion sieve can be used as a good lithium adsorption material.

Description

technical field [0001] The invention relates to a three-dimensional macroporous-mesoporous lithium ion sieve and a preparation method thereof, belonging to the field of nanomaterials. Background technique [0002] As a new type of energy metal, lithium metal is widely used in many fields. The demand for lithium resources is increasing day by day. However, the output of lithium metal is in short supply. Lithium resources mainly exist in lithium ore, salt lakes and seawater. However, lithium ore resources are limited, and even the most mature ore lithium extraction process has disadvantages such as high energy consumption, high equipment requirements, high cost, and low recovery rate, which cannot meet the market's demand for metal lithium. 69% of the world's lithium reserves come from salt lakes. At present, the methods for extracting lithium from salt lakes mainly include evaporation, crystallization, precipitation, solvent extraction and adsorption. Adsorption is consider...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/30C22B26/12C01D15/00
CPCB01J20/06B01J20/28014B01J20/28083B01J20/28085B01J20/3057B01J20/3085C01D15/00C22B26/12
Inventor 王灵芝李娜甘凯峰卢德力张金龙
Owner EAST CHINA UNIV OF SCI & TECH
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