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A lithium zirconate-coated manganese-based lithium ion sieve and its preparation and application

A technology of lithium ion and lithium zirconate, applied in the direction of manganate/permanganate, manganese compound, zirconium compound, etc., can solve the problems of poor structural stability, inability to take into account manganese dissolution loss and lithium adsorption capacity, etc., to reduce The effect of dissolution rate, reduction of manganese dissolution loss, and good adsorption performance

Inactive Publication Date: 2020-11-03
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the technical problems that existing lithium-ion sieves cannot take into account manganese dissolution loss and lithium adsorption capacity, and have poor structural stability, the present invention provides a lithium zirconate-coated manganese-based lithium-ion sieve (the present invention is also referred to as lithium-ion sieve) , designed to take into account manganese dissolution loss and lithium adsorption capacity, and also help to improve the stability of the material

Method used

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  • A lithium zirconate-coated manganese-based lithium ion sieve and its preparation and application
  • A lithium zirconate-coated manganese-based lithium ion sieve and its preparation and application
  • A lithium zirconate-coated manganese-based lithium ion sieve and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] (1) Preparation of lithium ion sieve precursor Li 1.6 Mn 1.6 O 4

[0086] Will electrolyze MnO 2 Calcined at 750℃ for 500min to generate Mn 2 O 3 , Weigh 22.6gLiOH·H 2 Dissolve O in 500mL deionized water, slowly add 20g Mn 2 O 3 Powder, control the Li / Mn molar ratio to 2.0:1, first 1700r·min -1 Stir at the rotating speed for 180min, then 800r·min -1 Stir for 60 min at the speed of rotation, then add the mixed solution into the autoclave and hydrothermally react at 250℃ for 17h to obtain LiMnO 2 , Then LiMnO 2 Calcined at 450℃ for 6h to obtain 25g precursor Li 1.6 Mn 1.6 O 4 .

[0087] (2) Preparation of coated Li 2 ZrO 3 Lithium ion sieve precursor

[0088] Weigh 1.12g zirconium nitrate pentahydrate and 0.38g lithium nitrate dissolved in 500mL ethanol solution (aqueous solution), the volume ratio of ethanol to water is 5:1, add 20g precursor Li 1.6 Mn 1.6 O 4 Disperse ultrasonically for 20h, place it in a constant temperature water bath at 70℃ and stir until ethanol is complete...

Embodiment 2

[0096] (1) Preparation of lithium ion sieve precursor Li 1.6 Mn 1.6 O 4

[0097] Will electrolyze MnO 2 Calcined at 650℃ for 500min to generate Mn 2 O 3 , Weighing 13·9gLiOH·H 2 Dissolve O in 500mL deionized water, slowly add 20gMn 2 O 3 Powder, control the Li / Mn molar ratio to 1.2:1, first 1500r·min -1 Stir at the speed of 240min, then 600r·min -1 Stir at a speed of 60 min at a high speed, then add the mixed solution into the autoclave and hydrothermally react at 200 ℃ for 20 h to obtain LiMnO 2 , Then LiMnO 2 Calcined at 350℃ for 10h to obtain 25g precursor Li 1.6 Mn 1.6 O 4 .

[0098] (2) Preparation of coated Li 2 ZrO 3 Lithium ion sieve precursor

[0099] Weigh 1.57g zirconium ethoxide and 0.89g lithium acetate and dissolve them in 300mL ethanol solution (aqueous solution), the volume ratio of ethanol to water is 5:1, add 20g precursor Li 1.6 Mn 1.6 O 4 , Disperse ultrasonically for 10 hours, place it in a constant temperature water bath at 70°C and stir until the ethanol is comp...

Embodiment 3

[0105] (1) Preparation of lithium ion sieve precursor Li 1.6 Mn 1.6 O 4

[0106] Will electrolyze MnO 2 Calcined at 800℃ for 500min to generate Mn 2 O 3 , Weigh out 17.0gLiOH·H 2 Dissolve O in 500mL deionized water, slowly add 20gMn 2 O 3 Powder, control the Li / Mn molar ratio to 1.5:1, first 2000r·min -1 Stir at the speed of 240min, then 700r·min -1 Stir at a speed of 60 min at a high speed, then add the mixed solution into the autoclave and hydrothermally react at 170℃ for 24h to obtain LiMnO 2 , Then LiMnO 2 Calcined at 500℃ for 6h to obtain 25g precursor Li 1.6 Mn 1.6 O 4 .

[0107] (2) Preparation of coated Li 2 ZrO 3 Lithium ion sieve precursor

[0108] Pipette 0.64 mL of 70% zirconium n-propoxide solution and 0.12 g of lithium hydroxide and dissolve in 400 mL of ethanol solution (aqueous solution). The volume ratio of ethanol to water is 5:1, and 20 g of precursor Li is added. 1.6 Mn 1.6 O 4 Disperse ultrasonically for 15h, place it in a constant temperature water bath at 80℃ an...

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Abstract

The invention belongs to the technical field of lithium adsorption materials and particularly discloses a lithium zirconate coated manganese lithium ion sieve. The lithium zirconate coated manganese lithium ion sieve has a core-shell structure, the core of the lithium zirconate coated manganese lithium ion sieve is made of H1.6Mn1.6O4, and the shell layer of the lithium zirconate coated manganeselithium ion sieve is made of Li2ZrO3. The invention also discloses a preparation method of the lithium ion sieve. Li1.6Mn1.6O4 is dispersed in a solution containing a Zr source and a lithium source, and then, a Li2ZrO3 lithium ion sieve precursor is obtained through solvent removal and calcination; the lithium zirconate coated manganese lithium ion sieve is obtained after the Li2ZrO3 lithium ion sieve precursor is subjected to Li removal treatment through acid leaching and then subjected to solid-liquid separation, washing and drying. The problems that the manganese lithium ion sieve has pooracid corrosion resistance, large manganese solution loss, instable structure, poor cycle performance and no adsorption capacity of a coating layer are solved. The lithium ion sieve product has high lithium adsorption capacity, is stable in structure and long in service life and is an efficient lithium extraction adsorbent for salt lake brine or seawater. The preparation process is simple and clean, no side reaction exists in the preparation process, the product performance is good, and the preparation process is suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of adsorption materials, and specifically relates to a manganese lithium ion sieve. [0002] technical background [0003] Lithium is an important strategic resource and one of the most ideal materials in the development of new energy. It is known as the "energy metal of the 21st century" and "the element that promotes the world's progress." And materials as an important emerging industry. With the increasing depletion and depletion of ore resources such as spodumene in recent years, the proportion of lithium extracted from salt lake brine in the current world's lithium salt production has risen to more than 90%. There are many salt lakes in our country, and lithium resources are abundant. However, the concentration of lithium in salt lake brines in my country is low, and the ratio of magnesium to lithium is high, making extraction difficult. The lithium ion sieve exchange method is the most practical method for extracting...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/30C01G45/12C01G25/00C22B26/12C22B3/24
CPCB01J20/04B01J20/06B01J20/28014C01G25/00C01G45/1221C22B3/24C22B26/12
Inventor 杨喜云王豪曹改芳徐徽石西昌
Owner CENT SOUTH UNIV