Zirconium dioxide-coated manganese lithium ion sieve as well as preparation method and application thereof

A technology of zirconium dioxide and lithium ions, applied in chemical instruments and methods, inorganic chemistry, manganese compounds, etc., can solve problems such as poor cycle performance, large manganese dissolution loss, poor acid corrosion resistance, etc.

Inactive Publication Date: 2017-11-24
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the technical deficiencies of the existing manganese-based lithium ion sieve such as poor acid corrosion resistance, large manganese dissolution loss, unstable structure, and poor cycle performance. The present invention provides a zirconia with a core-shell coating structure Coated manganese-based lithium-ion sieve, designed to improve the stability of manganese-based lithium-ion sieve

Method used

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  • Zirconium dioxide-coated manganese lithium ion sieve as well as preparation method and application thereof
  • Zirconium dioxide-coated manganese lithium ion sieve as well as preparation method and application thereof
  • Zirconium dioxide-coated manganese lithium ion sieve as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (1) Preparation of lithium ion sieve precursor Li 1.6 mn 1.6 o 4

[0068] electrolytic MnO 2 Calcined at 750°C for 500min to generate Mn 2 o 3 , Weigh 22.6gLiOH.H 2 O was dissolved in 500 mL of deionized water and slowly added 20 g of Mn 2 o 3 Powder, control the Li / Mn molar ratio to 2.0:1, first 300r.min -1 Stir for 30min at a constant speed, then 1700r.min -1 Stir at 180min at a constant speed, and finally 800r.min -1 Stir at the speed of 60min, and then put the mixed solution into the autoclave for hydrothermal reaction at 250°C for 17h to obtain LiMnO 2 , then the LiMnO 2 Calcined at 450°C for 6h to obtain 25g of precursor Li 1.6 mn 1.6 o 4 .

[0069](2) Preparation of coated ZrO 2 Li-ion sieve precursor

[0070] Weigh 2.1 g of zirconium nitrate pentahydrate and dissolve it in 500 mL of ethanol solution (aqueous solution), the volume ratio of ethanol to water is 5:1, add 20 g of precursor Li 1.6 mn 1.6 o 4 , ultrasonically dispersed for 20 hours,...

Embodiment 2

[0078] (1) Preparation of lithium ion sieve precursor Li 1.6 mn 1.6 o 4

[0079] electrolytic MnO 2 Calcined at 650°C for 500min to generate Mn 2 o 3 , weighed 13.9g LiOH·H 2 O was dissolved in 500 mL of deionized water and slowly added 20 g of Mn 2 o 3 Powder, control the Li / Mn molar ratio to 1.2:1, first 200r·min -1 Stir at 1500r·min for 30min -1 Stir at 240min at a constant speed, and finally 600r·min -1 Stir at a high speed for 60 minutes, then add the mixed solution into the autoclave and react for 20 hours at 200 ° C to obtain LiMnO 2 , then the LiMnO 2 Calcined at 350 °C for 10 h to obtain 25 g of precursor Li 1.6 mn 1.6 o 4 .

[0080] (2) Preparation of coated ZrO 2 Li-ion sieve precursor

[0081] Weigh 1.96 g of zirconium ethoxide and dissolve it in 300 mL of ethanol solution (aqueous solution), the volume ratio of ethanol to water is 5:1, add 20 g of precursor Li 1.6 mn 1.6 o 4 , ultrasonically dispersed for 10 h, placed in a constant temperature ...

Embodiment 3

[0087] (1) Preparation of lithium ion sieve precursor Li 1.6 mn 1.6 o 4

[0088] electrolytic MnO 2 Calcined at 800°C for 500min to generate Mn 2 o 3 , Weigh 17.0gLiOH·H 2 O was dissolved in 500 mL of deionized water and slowly added 20 g of Mn 2 o 3 Powder, control the Li / Mn molar ratio to 1.5:1, first 300r min -1 Stir at room temperature for 30min, then 2000r·min -1 Stir at 240min at a constant speed, and finally 700r·min -1 Stir at a high speed for 60 minutes, then add the mixed solution into the autoclave and react for 24 hours at 170 ° C to obtain LiMnO 2 , then the LiMnO 2 Calcined at 500 °C for 6 h to obtain 25 g of precursor Li 1.6 mn 1.6 o 4 .

[0089] (2) Preparation of coated ZrO 2 Li-ion sieve precursor

[0090] Pipette 0.8mL of 70% zirconium n-propoxide solution and dissolve in 400mL 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 , ultrasonically dispersed for 15 hours, plac...

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Abstract

The invention provides a zirconium dioxide-coated manganese lithium ion sieve which has a core-shell structure, wherein a core is made of H1.6Mn1.6O4, and a shell layer is made of ZrO2. In addition, the invention further discloses a preparation method which comprises the following steps: dispersing Li1.6Mn1.6O4 into solution containing a Zr source, removing a solvent and roasting, so as to obtain a ZrO2 lithium ion sieve precursor; removing Li from the ZrO2 lithium ion sieve precursor, then performing solid-liquid separation, washing and drying, so as to obtain the zirconium dioxide-coated manganese lithium ion sieve. According to the zirconium dioxide-coated manganese lithium ion sieve, the problems that a manganese lithium ion sieve is poor in acid corrosion resistance, large in manganese solution loss, unstable in structure and poor in cycling performance are solved. The obtained lithium ion sieve product is high in adsorption capacity of lithium ions, stable in structure and long in service life, so that the lithium ion sieve provided by the invention is an efficient lithium extraction adsorbent of salt lake brine or sea water. The zirconium dioxide-coated manganese lithium ion sieve is simple and clean in preparation processes, free of side reaction in a preparation process and good in product performance, thereby being suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a manganese-based lithium ion sieve, in particular to a method for coating and modifying the lithium ion sieve; it belongs to the technical field of chemical product preparation. technical background [0002] There are many salt lakes in the central and western parts of my country, which are rich in lithium, sodium, potassium, magnesium and other resources, and have great economic value. Extracting lithium from salt lake brine has become a research hotspot for scientific and technological workers. Salt lake brine is characterized by low lithium concentration and high ratio of magnesium to lithium. Ion sieve exchange method is the most practical method for extracting lithium from dilute solution. The technical key of this method is to find an exchange agent with specific selectivity for lithium ions. Spinel-type lithium manganese oxide ion sieve has good selectivity, relatively low cost, large adsorptio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/04B01J20/30C02F1/28C01G45/12
CPCB01J20/0211B01J20/0222B01J20/04C01G45/1242C02F1/281
Inventor 杨喜云王豪尹周澜徐徽石西昌
Owner CENT SOUTH UNIV
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