Lithium ion sieve doped with IIIA element as well as preparation method and application thereof

A technology of ion sieve and elements, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problems of reduced cycle performance, high energy consumption, easy loss of manganese, etc., and achieve high industrial feasibility , Excellent product performance and low equipment requirements

Inactive Publication Date: 2020-04-14
HUNAN BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, during the pickling process, manganese is easy to lose, which affects the structural stability of ion sieves and reduces the cycle performance. These problems have always hindered the industrial application of ion sieves.
[0006] In this patent, on the one hand, the preparation cycle of the two-step roasting + hydrothermal method is too long, resulting in high energy consumption, and the organic materials involved are not conducive to storage and transportation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of ion sieve, comprising the following steps:

[0037] 1) 5.0014g MnO 2 Mix and grind with 1.3781g LiOH evenly;

[0038] 2) Weigh 2.7423g of Na 2 B 4 o 7 10H 2 O, mix into 1) the ground powder, add 10% alcohol to wet grind and grind evenly, put it in a vacuum drying oven for 4 hours at 100°C;

[0039] 3) 2) the mixed raw material that obtains is ground into powder, is transferred in the tube furnace, O 2 In the atmosphere stage, the temperature is raised to 700°C for 4 hours, in which the first stage is raised to 400°C for 1 hour, the second stage is heated to 600°C for 1 hour, and the third stage is heated to 700°C. The samples obtained by roasting are washed and dried for later use;

[0040] 4) Weigh 5.0024 g of the sample obtained by roasting, pickle with 0.5 mol / L hydrochloric acid for 4 h, filter and dry to obtain an ion sieve;

[0041] Use 0.5g / L lithium solution to detect the lithium extraction performance of the ion sieve:

[0042] T...

Embodiment 2

[0045] A preparation method of ion sieve, comprising the following steps:

[0046] 1) 9.9995g MnO 2with 4.2504g Li 2 CO 3 Mix and grind evenly;

[0047] 2) Weigh 1.9167g of Al according to the molar ratio Al / Mn=0.05 2 (SO 4 ) 3 18H 2 O, mix into 1) the ground powder, add 10% alcohol to wet grind and grind evenly, put it in a vacuum drying oven for 4 hours at 100°C;

[0048] 3) 2) the mixed raw material that obtains is ground into powder, is transferred in the tube furnace, O 2 In the atmosphere stage, the temperature was raised to 800°C for 4 hours, in which the first stage was raised to 400°C for 1 hour, the second stage was raised to 600°C for 1 hour, and the third stage was heated to 800°C. The samples obtained by roasting were washed and dried for later use;

[0049] 4) Weigh 3.2075 g of the sample obtained by roasting, pickle with 0.5 mol / L hydrochloric acid for 4 h, filter and dry to obtain an ion sieve;

[0050] Use 0.5g / L lithium solution to detect the lithium...

Embodiment 3

[0054] A preparation method of ion sieve, comprising the following steps:

[0055] 1) 5.0011g MnO 2 Mix and grind with 1.3783g LiOH evenly;

[0056] 2) Weigh 5.0648g of GaCl 3 , mix into 1) the ground powder, add 10% alcohol to wet grind and grind evenly, put it in a vacuum drying oven for 4 hours at 100°C;

[0057] 3) 2) the mixed raw material that obtains is ground into powder, is transferred in the tube furnace, O 2 In the atmosphere stage, the temperature was raised to 800°C for 4 hours, in which the first stage was raised to 400°C for 1 hour, the second stage was raised to 600°C for 1 hour, and the third stage was heated to 800°C. The samples obtained by roasting were washed and dried for later use;

[0058] 4) Weigh 5.0006 g of the sample obtained by roasting, pickle with 0.5 mol / L hydrochloric acid for 4 h, filter and dry to obtain an ion sieve;

[0059] Use 0.5g / L lithium solution to detect the lithium extraction performance of the ion sieve:

[0060] The manganes...

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Abstract

The invention discloses a lithium ion sieve doped with an IIIA element as well as a preparation method and application thereof. The method comprises the following steps: mixing a manganese source anda lithium source, and uniformly grinding; adding a salt or elementary substance of the IIIA element, uniformly grinding, and then drying; carrying out dry grinding on the dried raw materials to obtainpowder, carrying out segmented roasting for 0.5-16 hours at 300-800 DEG C in an oxygen or air atmosphere, and cooling to obtain an ion sieve precursor; pickling the ion sieve precursor for 4-12 hours, filtering and drying to obtain the ion sieve; and the salt or elementary substance of the IIIA element is more than one of Na2B4O7.10H2O, boron powder, aluminum sulfate, aluminum hydroxide, galliumchloride, gallium nitrate, indium hydroxide or thallium trifluoroacetate. The 4h adsorption capacity of the ion sieve product prepared by the method is close to 20mg / g, and the acid pickling manganeseloss is reduced by one time compared with that of lambda-MnO2 serving as an ion sieve and is superior to the adsorption performance of the ion sieve prepared by taking LiMn2O4 as a precursor.

Description

technical field [0001] The invention relates to a lithium ion sieve doped with IIIA elements, a preparation method and application thereof. Background technique [0002] Lithium resources are widely used in batteries, metallurgy and other industries. my country's solid ore lithium resources are poor, but liquid lithium resources are abundant. Lithium extraction from salt lake brine and seawater has attracted the attention of researchers. The traditional precipitation method, solvent extraction method, calcination and other methods can achieve a lithium recovery rate of 80-90%, but it is difficult to recover low-concentration lithium. The ion sieve adsorption method uses the ion sieve to have the characteristics of screening and memory effect on lithium ions, and extracts and recovers lithium in high-salt and low-lithium solutions, which has high economic value. [0003] The currently studied lithium ion sieves are mainly manganese oxide ion sieves with a spinel structure. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/04B01J20/30C02F1/28
CPCB01J20/04C02F1/281
Inventor 杨鼎乔延超陈若葵阮丁山孙颉段金亮李强谌志新
Owner HUNAN BRUNP RECYCLING TECH
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