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Doped lithium titanate adsorption agent and preparation method thereof

A technology of heterolithic lithium titanate and adsorbent, which is applied in the field of doped lithium titanate adsorbent and its preparation, can solve the problems of complex potential process of the system, high cost of external oxidant, and fast performance decay, etc., to achieve improved microporous structure, Improve lithium adsorption capacity and selectivity, low titanium dissolution rate

Active Publication Date: 2019-02-12
四川泛宇锂能新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the cost of adding an oxidant is high, and the process of adjusting the potential of the system by an external circuit is complicated.
In patent CN108212074A, magnetic elements (iron, cobalt, nickel) are mixed into lithium metatitanate to replace part of the titanium, and then the lithium is eluted with acid to obtain a magnetically separable titanium-based adsorbent. It can be quickly separated by the action of an external magnetic field, but there are problems such as large dissolution rate during desorption, fast performance decay, and long adsorption time.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] LiOH·H 2 O, SnC 2 o 4 and H 2 TiO 3 According to the molar ratio of 4.05:0.09:4.91 mixed, 55.0g LiOH·H 2 O (analytical pure), 6.1g SnC 2 o 4 (chemically pure) and 156.3g H 2 TiO 3 (Chemically pure) Add 435g of deionized water at a solid-to-liquid ratio of 1:2 and stir in a 60°C water bath for 3h; the obtained slurry is air-dried at 110°C for 5h, finely ground, calcined at 750°C for 15h, cooled, and finely ground , get Li 4 sn 0.02 Ti 4.91 o 12 Adsorbent precursors. Take 100g of the Li 4 sn 0.09 Ti 4.91 o 12 Place in 3.0L of HCl with a concentration of 1.0mol / L, stir and soak for 4h, and obtain a hydrogen-type lithium ion adsorbent after filtration. Then take 1000mL of bittern as shown in Table 1, adjust the pH to 8.0 with 0.1mol / L NaOH solution, add 42g (dry weight) of the hydrogen-type lithium ion adsorbent, soak for 60min under stirring, and filter to obtain the adsorption mother liquor L 1 , to determine its Li + , Mg 2+ content, to obtain filter ...

Embodiment 2

[0028] C 2 h 3 o 2 Li, Zr(NO 3 ) 4 ·5H 2 O and rutile TiO 2 According to the molar ratio of 4.04:1.2:3.8 mixed, 78.5gC 2 h 3 o 2 Li (analytically pure), 151.7g Zr (NO 3 ) 4 ·5H 2 O (analytically pure) and 89.4g rutile TiO 2 (Analytical pure) Add 480g of deionized water according to the solid-to-liquid ratio of 1:1.5, and stir at 25°C for 8h; the obtained slurry is air-dried at 120°C for 4h, finely ground, calcined at 800°C for 16h, cooled, and ground Fine, get Li 4 Zr 1.2 Ti 3.8 o 12 Adsorbent precursors. Take 100g of the Li 4 Zr 1.2 Ti 3.8 o 12 Soak in 1.8L of HCl with a concentration of 1.5mol / L for 5h, filter to obtain a hydrogen-type lithium ion adsorbent, then take 1000mL of brine (pH=9.5) with the composition shown in Table 2, and add the hydrogen-type lithium ion adsorbent 70g (dry weight), soak 80min under stirring, filter, obtain the adsorption mother liquor L 3 , to determine its Li + , Mg 2+ content, to obtain filter cake S 3 That is, the lo...

Embodiment 3

[0032] Li 2 CO 3 , Ce(NO 3 ) 3 ·6H 2 O and anatase TiO 2 According to the molar ratio of 2.03:0.05:4.95 mixed, 48.7gLi 2 CO 3 (analytical pure), 7.0g Ce(NO 3 ) 3 ·6H 2 O (analytically pure) and 128.3g TiO 2 (Analytical pure) Add 460g of deionized water according to the solid-to-liquid ratio of 1:2.5 and stir in a 50°C water bath for 4h; the obtained slurry is air-dried at 105°C for 8h, finely ground, calcined at 700°C for 18h, cooled, and finely ground , get Li 4 Ce 0.05 Ti 4.95 o 12 Adsorbent precursors. Take 100g of the Li 4 Ce 0.05 Ti 4.95 o 12 Soak in 1.0L of HCl with a concentration of 3.0mol / L for 6h, filter to obtain a hydrogen-type lithium ion adsorbent, then take 200mL of brine with the composition shown in Table 3 (pH>14), add the hydrogen-type lithium ion adsorbent 45g (dry weight), soaked under stirring for 70min, filtered to obtain the adsorption mother liquor L 5 , to determine its Li + , Mg 2+ content, to obtain filter cake S 5 That is, th...

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PUM

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Abstract

The invention relates to an adsorption material for separating and extracting lithium from brine, in particular to a doped lithium titanate adsorption agent and a preparation method thereof. The dopedlithium titanate adsorption agent HxLi4-xMyTi5-yO12 is obtained by doping M into crystal lattices of Li4Ti5O12 to form precursors Li4MyTi5-yO3 and then removing lithium by acid pickling, where M is one or a mixture of several of Ce, Sn, Nb, Zr, Mo, Ta, W, Mn and Hf; the value range of x is 0.0 to 4.0; the value range of y is 0.0 to 2.0. A titanium source, the lithium source and M salts are uniformly mixed, dried, roasted, cooled and are subjected to acid pickling to obtain the doped lithium titanate adsorption agent. The doped lithium titanate adsorption agent prepared by the method is used for performing adsorption lithium extraction on brine with the magnesium-lithium ratio being greater than 100; the lithium absorption rate is greater than 75 percent; the magnesium removal rate is greater than 99 percent; the stripping liquid acidity is high; the lithium enriching times is about 1 to 7 times; the titanium dissolution damage rate is low; the industrialized application prospects arerealized.

Description

technical field [0001] The invention relates to an adsorbent material for separating and extracting lithium from brine, in particular to a doped lithium titanate adsorbent and a preparation method thereof. Background technique [0002] With the widespread application of lithium batteries in automobiles, wind power, IT and other fields, the demand for lithium and its compounds, the key raw material, has increased dramatically. At present, the demand for lithium products in the international market continues to grow at an average rate of more than 10% per year, resulting in a doubling of the market price of lithium products. More than 60% of the world's lithium resources are stored in salt lakes, and lithium extraction from salt lake brine has become the main way to produce lithium salts at home and abroad. my country's salt lake brine resources are rich, ranking second in the world's proven reserves of lithium resources, of which liquid ore lithium resources account for abou...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/30C01G23/00C01G25/00
CPCB01J20/0251B01J20/041B01J20/06C01G23/002C01G25/006
Inventor 钟辉赖先熔南近山王诗诗
Owner 四川泛宇锂能新材料科技有限公司
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