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Magnetic separable metatitanic acid lithium ion sieve, preparation method and application of lithium ion sieve

A technology for magnetic separation and lithium ions, which is applied in chemical instruments and methods, lithium compounds, and other chemical processes, and can solve problems such as high ratio, complexity, and large amount of addition

Active Publication Date: 2018-06-29
JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the ion sieve has good dispersion and large specific surface, and can quickly separate the adsorbent from the solution, but Fe 3 o 4 The addition of a large amount of lithium ion sieve is high, the proportion of the lithium ion sieve is high, the adsorption capacity of the lithium ion sieve per unit mass is not high enough, and the preparation process requires a narrow channel impingement flow reactor and hydrothermal aging, which is relatively complicated

Method used

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  • Magnetic separable metatitanic acid lithium ion sieve, preparation method and application of lithium ion sieve
  • Magnetic separable metatitanic acid lithium ion sieve, preparation method and application of lithium ion sieve
  • Magnetic separable metatitanic acid lithium ion sieve, preparation method and application of lithium ion sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0069] A magnetically separable metatitanic acid lithium ion sieve with a molecular formula of H 2 Fe 0.074 Ti 0.926 o 3 , the particle size distribution of the lithium ion sieve is between 100-200nm, and the BET specific surface area is 58.42m 2 / g.

[0070] Prepare as follows:

[0071] According to the molar ratio of Li, Ti and Fe 2.2:1:0.08, lithium hydroxide, titanium dioxide and ferric oxide are mixed, fully ground until the mixture is uniform, and then the ground sample is placed in a crucible for compaction, and the lid is closed. The crucible was placed in a muffle furnace, heated to 600°C at a heating rate of 8°C / min, calcined at 600°C for 3 hours, and then cooled to room temperature. The cooled samples were washed with water and dried in an oven at 90°C. The dried sample was delithiated by acid leaching in 0.5 mol / L hydrochloric acid solution, and the acid leaching time was 24 hours. Then the solution after acid leaching was filtered, washed with distilled wat...

Embodiment 2

[0078] A magnetically separable metatitanic acid lithium ion sieve with a molecular formula of H 2 Fe 0.01 Ti 0.99 o 3 , the particle size distribution of the lithium ion sieve is between 60-170nm, and the BET specific surface area is 43.20m 2 / g.

[0079] Prepare as follows:

[0080] According to the molar ratio of Li, Ti and Fe 2:1:0.01, lithium carbonate, titanium dioxide and iron are mixed, fully ground until the mixture is uniform, and then the ground sample is placed in a crucible for compaction, and the covered crucible is placed In a muffle furnace, the temperature was raised to 350° C. at a heating rate of 0.1° C. / min, calcined at 350° C. for 0.5 hour, and then cooled to room temperature. The cooled samples were washed with water and dried in an oven at 90°C. The dried sample was delithiated by acid leaching in 0.01 mol / L sulfuric acid solution, and the acid leaching time was 48 hours. Then the solution after acid leaching was filtered, washed with distilled wa...

Embodiment 3

[0082] A magnetically separable metatitanic acid lithium ion sieve with a molecular formula of H 2 Fe 0.15 Ti 0.85 o 3 , the particle size distribution of the lithium ion sieve is between 110-200nm, and the BET specific surface area is 38.94m 2 / g.

[0083] Prepare as follows:

[0084] According to the molar ratio of Li, Ti and Fe 2.8:1:0.3, lithium acetate, tetrabutyl titanate and ferric sulfate were mixed, fully ground until the mixture was uniform, and then the ground sample was placed in a crucible for compaction, and the lid A good crucible is placed in a muffle furnace, heated to 1050°C at a heating rate of 10°C / min, calcined at 1050°C for 8 hours, and then cooled to room temperature. The cooled samples were washed with water and dried in an oven at 90°C. The dried sample was delithiated by acid leaching in 0.8 mol / L nitric acid solution, and the acid leaching time was 0.5 hours. Then the solution after acid leaching was filtered, washed with distilled water until...

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Abstract

The invention provides a metatitanic acid lithium ion sieve and a preparation method of the lithium ion sieve. A molecular formula of the lithium ion sieve is H2RxTi1xO3; R is a magnetic element; x isbetween 0.01 and 0.2; and the lithium ion sieve is formed by doping the magnetic element into an Li2TiO3 lattice, substituting part of titanium positions and removing lithium by pickling. A lithium ion sieve precursor is prepared by calcining a lithium source, a titanium source and a superparamagnetic substance and subjected to pickling and liquid-solid separation to form the magnetic separable metatitanic acid lithium ion sieve. The prepared metatitanic acid lithium ion sieve has the advantages of high adsorption capacity and leaching rate, low solution loss rate, stable structure and the like; the adsorption capacity of the lithium ion sieve is above 50mg / g; the leaching rate is greater than 99%; the solution loss rate is less than 0.1%; and the lithium ion sieve can be repeatedly usedfor many times. After adsorption, the lithium ion sieve can be separated from a lithium containing solution quickly by the action of an externally applied magnetic field, and the separation time is 1-10min.

Description

technical field [0001] The invention relates to the application field of a lithium ion sieve used for extracting lithium from a salt lake by an adsorption method, in particular to a magnetically separable metatitanic acid lithium ion sieve, a preparation method and an application thereof. Background technique [0002] Lithium is an important metal resource. Lithium and its compounds are widely used in metallurgy, medicine, glass ceramics, batteries, aerospace and other fields. With the rapid development of science and technology, the important position of lithium has become increasingly prominent, and the demand has increased rapidly. The lithium products of brine in various countries have increased year by year, and salt lake brine has gradually become the main source of lithium products. my country is a country with a large amount of lithium resources, and more than 80% of lithium resources exist in salt lake brine. The technology of extracting lithium from salt lake brine...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/28B01J20/30C02F1/28C01D15/00
CPCB01J20/041B01J20/06B01J20/28009B01J2220/4806C01D15/00C02F1/281
Inventor 李平王舒磊郑诗礼张懿
Owner JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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