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A kind of preparation method of lithium ion sieve adsorbent and its product and application

A lithium ion and adsorbent technology, applied in the field of materials, can solve the problems of porous fibrous lithium ion sieves, low lithium ion adsorption efficiency, and weakened lithium ion adsorption capacity, etc., to improve chemical stability and reusability Excellent, the effect of increasing the contact area

Active Publication Date: 2021-08-27
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titanium-based lithium-ion sieves prepared by traditional solid-phase synthesis methods are fine particles, which are prone to aggregation in water, which greatly weakens its adsorption capacity for lithium ions.
Although some supports (including carbon materials, polymer nanofibers) are used to load ion sieve particles, the use of supports hinders the diffusion of lithium ions and covers some adsorption sites, resulting in low lithium ion adsorption efficiency.
Prior to this, porous fibrous Li-ion sieves have not been reported

Method used

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  • A kind of preparation method of lithium ion sieve adsorbent and its product and application
  • A kind of preparation method of lithium ion sieve adsorbent and its product and application
  • A kind of preparation method of lithium ion sieve adsorbent and its product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Porous nanofibrous Li 4 Ti 5 o 12 (P-LTO-NF) preparation

[0023] 7g porogen (PVP), 5g lithium salt (LiAc) and 105mL mixed solvent (80mL EtOH, 10mLHAc and 15mLDMF) were mixed, then stirred at room temperature for 1h; then added 25g butyl titanate (TBOT), and then continued to Stir for 2h to obtain spinning solution. Put the electrospinning solution into the solution loading device of the electrospinning machine, set the electrospinning voltage to 14kV, and then perform electrospinning to obtain a nanofiber membrane.

[0024] After the nanofibrous membrane was dried at room temperature, it was calcined at 650° C. for 3 h in an air environment to obtain a porous nanofibrous titanium-based lithium ion sieve precursor (P-LTO-NF).

[0025] (2) Lithium ion sieve adsorbent H 4 Ti 5 o 12 (P-HTO-NF) preparation

[0026] Put 1 g of P-LTO-NF into 100 mL of 0.2 M hydrochloric acid and stir for 1 h, and dry the solid at room temperature to obtain H 4 Ti 5 o 12 (P-HTO-...

Embodiment 2

[0030] (1) Porous nanofibrous Li 4 Ti 5 o 12 -Fe 2 o 3 (P-LFTO-NF) preparation

[0031] 7g porogen (PVP), 5g lithium salt (LiAc), 5g iron salt (FeAc 2 ) and 105mL mixed solvent (80mL EtOH, 10mLHAc and 15mLDMF) were mixed, then stirred at room temperature for 1h; then 25g of butyl titanate (TBOT) was added, and then stirred at room temperature for 2h to obtain a spinning solution. Put the spinning solution into the solution loading device of the electrospinning machine, set the electrospinning voltage to 14kV, and then perform electrospinning to obtain nanofibers.

[0032] After the nanofibers were dried at room temperature, they were calcined at 650° C. for 3 h in an air environment to obtain a porous nanofibrous titanium-based lithium ion sieve precursor (P-LFTO-NF).

[0033] (2) Lithium ion sieve adsorbent H 4 Ti 5 o 12 (P-HFTO-NF) preparation

[0034] Put 1 g of P-LFTO-NF into 100 mL of 0.2 M hydrochloric acid and stir for 1 h, and dry the solid at room temperatur...

Embodiment 3

[0039] (1) Porous nanofibrous Li 4 Ti 5 o 12 -ZrO 2 (P-LZTO-NF) Preparation

[0040] 7g porogen (PVP), 5g lithium salt (LiAc), 5g zirconium salt (ZrOCl 2 ) and 105mL mixed solvent (80mL EtOH, 10mL HAc and 15mL DMF) were mixed, then stirred at room temperature for 1h; then added 25g of butyl titanate, and then continued to stir at room temperature for 2h to obtain a spinning solution. Put the spinning solution into the solution loading device of the electrospinning machine, set the electrospinning voltage to 14kV, and then perform electrospinning to obtain nanofibers.

[0041] After the nanofibers were dried at room temperature, they were calcined at 650° C. for 3 h in an air environment to obtain a porous nanofibrous titanium-based lithium ion sieve precursor (P-LZTO-NF).

[0042] (2) Lithium ion sieve adsorbent H 4 Ti 5 o 12 -ZrO 2 (P-HZTO-NF) preparation

[0043] Put 1g of P-LFTO-NF into 100mL of 0.2M hydrochloric acid and stir for 1h, and dry the solid at room tem...

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Abstract

The invention discloses a preparation method, product and application of a lithium ion sieve adsorbent, comprising the following steps: placing a porogen, a lithium salt, and an auxiliary metal salt in a solvent, stirring and mixing, and then adding tetrabutyl titanate , continue to stir until the solution is uniformly mixed to obtain a spinning solution; place the spinning solution in the solution storage device of the electrospinning machine, set the process parameters of the electrospinning, and then perform electrospinning to obtain nanofibers; After drying, calcining is carried out under the air atmosphere. After the calcining is completed, a lithium ion sieve precursor is obtained; the lithium ion sieve precursor is stirred and reacted in an inorganic acid, and after the reaction is completed, a lithium ion sieve adsorbent is obtained. The porous nanofibrous lithium ion sieve adsorbent prepared by the invention has a very large specific surface area, increases the contact area between the adsorbent and the solution, and can improve its adsorption capacity for lithium ions. The porous fibrous lithium ion sieve has an ion sieve structure as a whole, which has high selectivity for lithium ion adsorption.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of a lithium-ion sieve adsorbent and its product and application. Background technique [0002] With the rapid development of clean energy, the demand for lithium is increasing. The process of extracting lithium from lithium ore is complex and costly. Lithium-containing saline lake water is an important source of lithium, but saline lake water contains high concentrations of sodium, magnesium, and potassium ions. Traditional methods such as solvent extraction, ion exchange, precipitation and membrane separation are difficult to separate lithium with high selectivity. Lithium ion sieve can effectively and selectively adsorb and separate lithium ions. Manganese-based lithium-ion sieves are commonly used, but manganese-based lithium-ion sieves have manganese dissolution loss, especially in acidic environments, the dissolution loss of manganese i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/04B01J20/28B01J20/30
CPCB01J20/04B01J20/28009B01J20/28023
Inventor 刘承斌唐艳红韦淑丹魏元峰罗胜联
Owner HUNAN UNIV