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Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4

A li1.6mn1.6o4, ion sieve technology, applied in chemical instruments and methods, other chemical processes, inorganic chemistry, etc., can solve the problems of complex synthesis of MnOOH, instability of MnOOH, high operating conditions, etc., and it is easy to achieve product ratio Controlled, stable properties, wide range of effects

Active Publication Date: 2013-05-29
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

[0004] The manganese dioxide ion sieve with the largest adsorption capacity reported so far is MnO 2 0.5H 2 O, its synthesis method is relatively simple, all of which are first synthesized by LiMnO 2 , then the LiMnO 2 Precursor obtained by calcination in air atmosphere
The existing synthesis methods generally use MnOOH as the manganese source to synthesize LiMnO 2 , and the synthesis of MnOOH itself is relatively complicated, requiring high operating conditions, and MnOOH is unstable in the air, which is not conducive to industrial production
At the same time, there are also the problems of high lithium-manganese ratio of raw materials (generally greater than 10), and long hydrothermal reaction time.

Method used

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  • Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4
  • Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4
  • Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4

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preparation example Construction

[0031] Manganese series ion sieve adsorbent MnO of the present invention 2 0.5H 2 The preparation method of O and precursor thereof, comprises the steps:

[0032] (1) Add 0.1-0.3mol / L potassium permanganate solution and 3.0-5.0mol / L lithium hydroxide solution into 2-4mol / L manganese chloride solution at a flow rate of 3-10mL / min while stirring , wherein the molar ratio of manganese chloride to potassium permanganate is (3.8-4.5):1, and the molar ratio of lithium hydroxide to potassium permanganate is (12-25):1;

[0033] (2) Transfer the brown solution obtained in step (1) to a 1L polytetrafluoroethylene hydrothermal kettle, and conduct a hydrothermal reaction at 120-200°C for 6-24 hours to obtain the intermediate product LiMnO 2 ;

[0034] (3) LiMnO 2 After washing with water and suction filtration, dry at 60-100°C for 3-6 hours, and then calcinate at 300-500°C for 4-48 hours in an oxidizing atmosphere (air atmosphere or oxygen atmosphere) to obtain a lithium adsorbent pr...

Embodiment 1

[0039] Add 0.1mol / L potassium permanganate solution and 5.0mol / L lithium hydroxide solution to 2mol / L manganese chloride solution at a flow rate of 3mL / min under vigorous stirring, wherein the added manganese chloride and permanganese The molar ratio of potassium permanganate is 4:1, and the molar ratio of lithium hydroxide and potassium permanganate is 25:1; the obtained brown solution is hydrothermally reacted at 180°C for 6 hours in a 1L polytetrafluoroethylene hydrothermal kettle , to obtain the intermediate product LiMnO 2 , the XRD pattern of the product is shown in figure 1 (a), SEM image see figure 2 (a); by figure 1 (a), 2(a), it can be seen that the pure phase LiMnO can be obtained under the hydrothermal conditions adopted 2 , and the particle size of the product is relatively uniform, and the particle size is about 100nm. LiMnO 2 After washing with 30 times the volume of deionized water, suction filtration, drying at 80°C for 6 hours, and calcination at 450°C ...

Embodiment 2

[0042] Add 0.1mol / L potassium permanganate solution and 5.0mol / L lithium hydroxide solution into 2mol / L manganese chloride solution at a flow rate of 3mL / min under vigorous stirring, wherein the manganese chloride and potassium permanganate The molar ratio was 4.5:1, and the molar ratio between lithium hydroxide and potassium permanganate was 16.5:1; the obtained brown solution was transferred to a 1L polytetrafluoroethylene hydrothermal kettle, and hydrothermally reacted at 160°C for 12 hours to obtain Intermediate product LiMnO 2 ; the LiMnO 2 After washing with 30 times the volume of deionized water, suction filtration, drying at 80°C for 6 hours, and calcination at 350°C in air atmosphere for 24h, the lithium adsorbent precursor Li 1.6 mn 1.6 o 4 . Take the precursor 0.8g Li 1.6 mn 1.6 o 4 Add 200mL of 0.1mol / L HCl solution, put it into a constant temperature water bath shaker to oscillate at a frequency of 130rpm, control the temperature at 30°C, and react for 12h ...

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Abstract

The invention discloses a method for preparing a lithium ion sieve adsorbent MnO2.0.5H2O and a precursor thereof Li1.6Mn1.6O4. The method comprises the following steps: carrying out one-step hydrothermal synthesis on raw materials inorganic manganese salt and lithium salt to obtain an intermediate, and roasting at low temperature to obtain the required precursor Li1.6Mn1.6O4; and carrying out acid treatment on the precursor to extract Li so as to obtain an H-type ion sieve, washing with water, filtering, and drying to obtain the ion sieve adsorbent MnO2.0.5H2O which has a screening effect on lithium ions. The invention has the advantages of simple process route and mild preparation conditions; and the obtained ion sieve has the advantages of low solution loss, high adsorption rate and high adsorption capacity.

Description

technical field [0001] The invention relates to a preparation method of a lithium adsorbent, in particular to a method for preparing a manganese-based ion sieve adsorbent MnO 2 0.5H 2 O and its precursor Li 1.6 mn 1.6 o 4 Methods. Background technique [0002] Lithium is the lightest metal in the world and is widely used in many fields due to its special physical and chemical properties. Most of the lithium resources in the world are stored in salt lakes (seawater). How to effectively extract lithium from salt lakes or seawater has become an urgent problem to be solved. [0003] my country is a resource-rich country with abundant reserves of lithium resources, especially liquid lithium resources. The methods for extracting and separating lithium from salt lake brine mainly include precipitation method, solvent extraction method and adsorption method. From the environmental and economic point of view, the adsorption method has greater advantages than other methods, esp...

Claims

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Application Information

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IPC IPC(8): C01G45/02C01G45/00B01J20/06C22B26/12C22B3/24
Inventor 孙淑英肖伽励周龙生李超宋兴福李平于建国
Owner EAST CHINA UNIV OF SCI & TECH
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