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Method for preparing manganese-based lithium-ion sieve adsorbent

A lithium ion and adsorbent technology, which is applied in the field of preparation of manganese-based lithium ion sieve adsorbents, can solve the problems of low recycling rate of ion sieves, low purity of reaction products, unfavorable large-scale production, etc. Control, dissolution loss reduction effect

Inactive Publication Date: 2015-09-30
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are still some problems in the lithium ion sieve synthesized by the hydrothermal method, such as the low purity of the reaction product, the serious dissolution loss of manganese during the delithiation of the ion sieve precursor and the adsorption process, the low recycling rate of the ion sieve, and the stability of the ion sieve. Relatively poor, etc., not conducive to large-scale production

Method used

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  • Method for preparing manganese-based lithium-ion sieve adsorbent
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  • Method for preparing manganese-based lithium-ion sieve adsorbent

Examples

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Effect test

Embodiment 1

[0038] Accurately weigh 8.3920g of analytically pure lithium hydroxide monohydrate, add it to 60mL of ethanol solution with a volume fraction of 3%, and dissolve it, then add 24.5101g of manganese acetate tetrahydrate to it, and react at room temperature for 2 hours under the action of magnetic stirring to obtain a brick Red precipitated product, then drop 6.0mL of 30% H 2 o 2 solution, after reacting for 20 minutes, add 2.0980 g of lithium hydroxide monohydrate to it, stir and react for 12 hours, then transfer the cloudy solution to a polytetrafluoroethylene-lined reactor, and react at a constant temperature of 120°C for 12 hours. The resulting precipitate was filtered, washed, and dried to obtain a reddish-brown intermediate product, which was ground to uniform and fine particles, then placed in a muffle furnace at a rate of 10°C / min to 300°C, kept at a constant temperature for 5 hours, and then cooled naturally to room temperature, the spinel-type lithium-ion sieve precurs...

Embodiment 2

[0042] Accurately weigh 8.3920 g of analytically pure lithium hydroxide monohydrate, add it to 70 mL of ethanol solution with a volume fraction of 5% and dissolve it, then add 24.5101 g of manganese acetate tetrahydrate therein, and react at room temperature for 3 h under the action of a magnetic stirrer to obtain Brick red precipitation product, then drop 6.0mL mass fraction of 30% H into it at a speed of 1.0mL / min 2 o 2 solution, after reacting for 20 minutes, 3.1472 g of lithium hydroxide monohydrate was added thereto, stirred and reacted for 12 hours, then the cloudy solution was transferred to a polytetrafluoroethylene-lined reactor, and reacted at a constant temperature of 140°C for 12 hours. The resulting precipitate was filtered, washed, and dried to obtain a reddish-brown intermediate product, which was ground to uniform and fine particles, then placed in a muffle furnace at a heating rate of 10°C / min to 400°C, kept at a constant temperature for 5 hours, and then cool...

Embodiment 3

[0044] Accurately weigh 8.3920 g of analytically pure lithium hydroxide monohydrate and add it to 80 mL of ethanol solution with a volume fraction of 8% to dissolve it, then add 24.5101 g of manganese acetate tetrahydrate to it, and react at room temperature for 5 hours under the action of a magnetic stirrer to obtain a brick The red precipitate product was then dripped with 6.0mL H at a rate of 1.5mL / min 2 o 2 After 20 minutes of reaction, 4.1960 g of lithium hydroxide was added thereto, stirred for 12 hours, and then the cloudy solution was transferred to a polytetrafluoroethylene-lined reactor, and reacted at a constant temperature of 130° C. for 12 hours. The resulting precipitate was filtered, washed, and dried to obtain a reddish-brown intermediate product, which was ground to uniform and fine particles, then placed in a muffle furnace at a rate of 10°C / min to 500°C, kept at a constant temperature for 5 hours, and then cooled naturally to room temperature, the spinel li...

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Abstract

The invention discloses a method for preparing a manganese-based lithium-ion sieve adsorbent. The method comprises the following steps: adopting lithium hydroxide and divalent manganese salt as raw materials, dissolving the raw materials in an ethanol solution with volume fraction being 2-10%, stirring uniformly, adding H2O2 and lithium hydroxide, synthesizing an intermediate through the low-temperature hydrothermal method, obtaining lithium-ion sieve precursor through low-temperature roasting, and performing solvent dipping on the precursor to elute lithium ions so as to obtain the corresponding lithium-ion sieve adsorbent. According to the invention, the lithium-ion sieve precursor is ordered in structure and uniform in particle; hydrochloric acid and persulfate are adopted as a dipping agent of the precursor, so that the elution effect to lithium ions is good, and the manganese dissolution loss rate is greatly reduced. The whole preparation process is mild in condition and easy to control; the obtained ion sieve is high in purity and adsorbing capacity and excellent in stability, and has excellent application prospects.

Description

technical field [0001] The invention relates to a preparation method of a manganese-based lithium ion sieve adsorbent, in particular to a method for preparing a manganese oxide lithium ion sieve by a hydrothermal method. Background technique [0002] Lithium metal, lithium alloys and lithium salts are widely used in electronics, chemical industry, metallurgy, energy, nuclear energy, aerospace and other fields due to their excellent performance, and are known as "industrial monosodium glutamate", "energy metals that promote world progress" and so on. With the development of high-tech, the demand for lithium resources is increasing day by day, and the lithium resources on land are far from meeting the needs of society. However, there are huge lithium resources in seawater, and how to effectively extract lithium from seawater has become an urgent problem to be solved. [0003] At present, in the research of lithium extraction from seawater, solvent extraction method and adsorb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/04B01J20/28B01J20/30
Inventor 沈江南杨珊珊周玛丽侯震东林溪赵严
Owner ZHEJIANG UNIV OF TECH
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