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Synthesis method of lithium extraction adsorbent

A synthesis method and lithium adsorption technology, applied in chemical instruments and methods, adsorption water/sewage treatment, titanium compounds, etc., can solve the problems of difficult control of mass transfer in solid phase reactions, difficulty in ensuring uniform mixing, etc., and achieve structural stability and reduction Small agglomeration, high selectivity effect

Inactive Publication Date: 2020-04-10
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Purpose of the invention: The purpose of the invention is to provide a synthetic method for extracting lithium adsorbent, dissolving the lithium source in a solvent containing a certain amount of additives, then adding the titanium source to form a solid-liquid mixed state, and drying the slurry to obtain a precursor After calcination, the solid powder has regular shape and uniform particle size, which can effectively solve the problem that the mass transfer of solid-phase reaction is difficult to control in solid-phase synthesis, and it is difficult to ensure complete mixing and uniformity.

Method used

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  • Synthesis method of lithium extraction adsorbent
  • Synthesis method of lithium extraction adsorbent
  • Synthesis method of lithium extraction adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Dissolve 6.1835g of lithium hydroxide monohydrate in 100ml of an aqueous solution containing 5% cetyltrimethylammonium bromide, and add 4.0338g to it under stirring (Li / Ti molar ratio is 2.80:1) Anatase-type titanium dioxide, continue to stir for 24h, the obtained slurry is spray-dried at a feed rate of 5ml / min under stirring, and the spray temperature is 120°C to obtain a solid powder;

[0029] 2. The obtained solid powder was calcined in a muffle furnace at a temperature of 5°C / min to 700°C for 72h to obtain the metatitanic acid lithium ion sieve precursor Li 2 TiO 3 ;

[0030] 3. Put the precursor body into 2 TiO 3 Add the powder into 0.3mol / L hydrochloric acid solution (solid-to-liquid ratio is 6g / L), magnetically stir at 50°C for 6h to remove lithium, filter, wash, and dry to obtain the metatitanic acid lithium ion sieve adsorbent H 2 TiO 3 ;

[0031] 4. Add the ion sieve to a solution with a pH of 10 and a lithium concentration of 500 mg / L, and magnetical...

Embodiment 2

[0034] 1. Dissolve 8.2440g of lithium acetate dihydrate in 80ml of absolute ethanol, add 4.0338g of rutile titanium dioxide (Li / Ti molar ratio is 1.60:1) to it under stirring, continue stirring for 0.5h, and the resulting slurry is stirred In the state, the feed rate is 3ml / min, and the inlet air temperature is 110°C for flash drying to obtain a solid powder;

[0035] 2. The obtained solid powder was calcined in a muffle furnace at a rate of 1°C / min to 550°C for 12 hours to obtain the metatitanic acid lithium ion sieve precursor Li 2 TiO 3 ;

[0036] 3. Put the precursor body into 2 TiO 3 Add the powder into 0.01mol / L hydrochloric acid solution (solid-to-liquid ratio is 0.5g / L), magnetically stir at 90°C for 8 hours to remove lithium, filter, wash, and dry to obtain the metatitanic acid lithium ion sieve adsorbent H 2 TiO 3 ;

[0037] 4. Add the ion sieve to a solution with a pH of 11 and a lithium concentration of 1 g / L, and magnetically stir at 55°C for 12 hours, and t...

Embodiment 3

[0039] 1. Dissolve 4.4794g of lithium chloride in 800ml of an aqueous solution containing 20% ​​polyvinylpyrrolidone, add 4.0338g of rutile titanium dioxide (Li / Ti molar ratio is 2.05:1) to it under stirring, and continue stirring for 48h to obtain Slurry is under stirring state with the feed rate of 20ml / min, and vacuum degree is 60kPa, and shaft speed is 10rpm and carries out vacuum drying with steam heating, obtains solid powder;

[0040] 2. The obtained powder was calcined in a muffle furnace at a rate of 5°C / min to 800°C for 9 hours to obtain the metatitanate lithium ion sieve precursor Li 2 TiO 3 ;

[0041] 3. Put the precursor body into 2 TiO 3 Add the powder into 1mol / L nitric acid solution (solid-to-liquid ratio is 50g / L), stir magnetically at 45°C for 0.15h to delithiate, filter, wash, and dry to obtain the metatitanic acid lithium ion sieve adsorbent H 2 TiO 3 ;

[0042] 4. Add the ion sieve to a solution with a pH of 10 and a lithium concentration of 200 mg / L...

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Abstract

The invention discloses a synthesis method of a lithium extraction adsorbent. The preparation method comprises the following steps: dissolving a lithium source in a solvent containing a certain amountof additive, then adding a titanium source into the solvent to be uniformly mixed to form a solid-liquid mixed state, and carrying out drying treatment to assist synthesis, so that the raw materialsare rapidly dried, fully mixed and calcined to obtain a lithium-ion sieve precursor Li2TiO3 with uniformly distributed particle sizes. A metatitanic acid type lithium ion sieve H2TiO3 obtained after acid pickling and lithium removal of the precursor Li2TiO3 has a remarkable adsorption effect. The method is simple and easy to implement, and the lithium ion sieve H2TiO3 is mainly used for extractinglithium from salt lake brine, oil field brine, seawater and other water bodies and has huge potential in the aspect of liquid lithium extraction.

Description

technical field [0001] The invention relates to the technical field of adsorbent materials, in particular to a synthesis method of an adsorbent for extracting lithium. Background technique [0002] Lithium is closely related to people's lives. Lithium is the alkali metal with the smallest atomic radius and the lightest metal known so far. It is called energy material and strategic resource, and it has a wide range of applications in many aspects such as glass, ceramics, medicine, aerospace vehicles, nuclear industry and the most well-known lithium battery industry. Especially in recent years, with the development of new energy vehicles, the demand for lithium resources is increasing day by day. [0003] The total amount of lithium resources in China ranks fourth in the world, accounting for about 13.21% of the total lithium reserves in the world. However, more than 79% of China's lithium resources exist in the brine of salt lakes and underground brines of oil fields in liq...

Claims

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Application Information

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IPC IPC(8): B01J20/06C01G23/00C02F1/28C22B26/12B01J20/30C02F101/10
CPCB01J20/06B01J20/041C22B26/12C01G23/00C02F1/281C02F2101/10B01J2220/42
Inventor 杨刚仵档孙朋飞
Owner NANJING UNIV OF TECH
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