A kind of hexagonal flake manganese series lithium ion sieve adsorbent and preparation method thereof

A hexagonal flake, lithium ion technology, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve the problems of particle uniformity and dispersibility, and high energy consumption without using effective methods, and reduce the reaction time. Steps and the effects of preparation cost, good quality and high preparation efficiency

Active Publication Date: 2021-04-02
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing methods not only consume too much energy, but also do not use effective methods to control the uniformity and dispersion of particles and regulate their crystal growth process

Method used

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  • A kind of hexagonal flake manganese series lithium ion sieve adsorbent and preparation method thereof
  • A kind of hexagonal flake manganese series lithium ion sieve adsorbent and preparation method thereof
  • A kind of hexagonal flake manganese series lithium ion sieve adsorbent and preparation method thereof

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preparation example Construction

[0028] As an aspect of the technical solution of the present invention, what it relates to is a preparation method of a hexagonal plate-shaped manganese series lithium ion sieve adsorbent, comprising the following steps:

[0029] (1) adding manganese source and lithium source into water, stirring to obtain the first mixed solution;

[0030] (2) adding an organic amine compound into the first mixed solution, and stirring to obtain a second mixed solution;

[0031] (3) Place the second mixed solution in a microwave reactor, react at 150-180° C. for 20-45 minutes, and then perform solid-liquid separation on the solid and liquid in the second mixed solution to obtain LiMnO 2 particles;

[0032] (4) the resulting LiMnO 2 The particles were calcined at 450-600°C for 3-6 hours to obtain Li 1.6 mn 1.6 o 4 Hexagonal flaky manganese-based lithium ion sieve adsorbent.

[0033] In some embodiments, the manganese source includes any one or two or more of potassium permanganate, sodiu...

Embodiment 1

[0049] (1) Sodium permanganate and lithium chloride were added into deionized water at a ratio of 0.15:1, and magnetically stirred to obtain the first mixed solution.

[0050] (2) Add ethylenediamine to the first mixed solution, the ratio of ethylenediamine to sodium permanganate is 5:1, mix and magnetically stir to obtain the second mixed solution.

[0051] (3) Put the second mixed solution into a microwave reactor at a temperature of 150° C. and a reaction time of 20 minutes. After the reaction is completed, the solid and liquid mixtures are subjected to solid-liquid separation to obtain solids that are washed and dried to obtain pure LiMnO 2 particles.

[0052] (4) LiMnO will be obtained 2 Calcined at 450°C for 3 hours to obtain Li 1.6 mn 1.6 o 4 Lithium ion adsorbent.

[0053] (5) Li will be obtained 1.6 mn 1.6 o 4 The lithium-ion adsorbent was exchanged and washed three times with deionized water and ethanol.

[0054] The XRD diffraction pattern of the hexagonal...

Embodiment 2

[0057] (1) Potassium permanganate and anhydrous lithium hydroxide were added into deionized water at a ratio of 0.8:1, and magnetically stirred to obtain a first mixed solution.

[0058] (2) Add ethylenediamine to the first mixed solution, the ratio of ethylenediamine to potassium permanganate is 80:1, mix and magnetically stir to obtain the second mixed solution.

[0059] (3) Put the second mixed liquid into a microwave reactor at a temperature of 180° C. and a reaction time of 45 minutes. After the reaction is completed, the solid and liquid mixtures are subjected to solid-liquid separation, and the solids obtained are washed and dried to obtain pure LiMnO 2 , particles.

[0060] (4) LiMnO will be obtained 2 Calcined at 600°C for 6 hours to obtain Li 1.6 mn 1.6 o 4 Lithium ion adsorbent.

[0061] (5) Li will be obtained 1.6 mn 1.6 o 4 The lithium-ion adsorbent was exchanged and washed three times with deionized water and ethanol.

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Abstract

The invention discloses a hexagonal flaky manganese lithium ion sieve adsorbent and a preparation method thereof. The method includes: adding a manganese source and a lithium source into water, and stirring to obtain first mixed solution; adding an organic amine compound into the first mixed solution, and stirring to obtain second mixed solution; adding the second mixed solution into a microwave reactor, performing reaction for 20-45min at 150-180 DEG C, and subjecting solid and liquid in the second mixed solution to solid-liquid separation to obtain LiMnO2 particles; calcining the obtained LiMnO2 particles for 3-6h at 450-600 DEG C to obtain Li1.6Mn1.6O4 hexagonal flaky manganese lithium ion sieve adsorbent. A microwave hydrothermal reaction method is adopted for preparing the hexagonal flaky manganese lithium ion sieve adsorbent, organic amines are adopted as a reducing agent and a structural regulating agent for growth regulation, and simplicity of selected raw materials and a preparation process and high purity, high yield, particle size uniformity and stable performances of an obtained product are realized.

Description

technical field [0001] The invention relates to a lithium ion sieve adsorbent, in particular to a hexagonal sheet-shaped manganese series lithium ion sieve adsorbent and a preparation method thereof. Background technique [0002] Lithium exists in nature mainly in pegmatite ores such as spodumene and lepidolite, or in salt lake brine and seawater in the form of lithium ions. Lithium ion extraction methods in brine mainly include: precipitation method, evaporation crystallization method, solvent extraction method, calcination leaching method, salting out method, carbonization method, selective semipermeable membrane method, "Xu's" method, adsorption method, among which adsorption method The process is simple and the cost is low, and it is an ideal method for extracting lithium from the solution. Lithium-manganese spinel-type lithium adsorbent is the most widely studied and has the highest adsorption capacity, and is expected to be used for lithium extraction in high-magnesiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/04B01J20/28B01J20/30
CPCB01J20/04B01J20/28014
Inventor 刘忠钱方仁郭敏周永全钱志强李权吴志坚
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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