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Preparation method of titanium-based lithium ion sieve

A lithium-ion and titanium-based technology, applied in the field of preparation of titanium-based lithium-ion sieves, can solve the problems of unfavorable industrial application, slow adsorption rate, uncontrollable particle size, etc., and achieve the effect of enriching lithium ion channels and increasing adsorption capacity.

Active Publication Date: 2021-07-16
GUANGDONG INST OF RARE METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the titanium-based lithium ion sieves prepared by the existing preparation methods usually have defects such as elution, slow adsorption rate, uncontrollable particle size, and poor adsorption capacity, which are not conducive to industrial applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Commercially available 0.1-0.2μm TiO 2 Take 2g of the powder, press it into a test piece with a diameter of 20mm and a thickness of 3mm under 8MPa, and sinter at 600°C for 3 hours in an argon atmosphere to obtain TiO 2 Audition. After the test piece was tightly wrapped with molybdenum mesh, the fine molybdenum wire was wound on the long molybdenum wire as the working electrode, the graphite rod was used as the counter electrode, and the mixture of LiCl and NaCl with a molar ratio of 2:1 was used as the electrolyte. In the atmosphere, the temperature is 500°C, the voltage is 3.2V, and the cathode is polarized for 5 hours. After the cathode polarization is completed, the anodic polarization is performed on the working electrode, the voltage is 2.6, and the polarization time is 0.5 hours. After cooling to room temperature in the electrolytic cell, the product was taken out, washed with distilled water, dried in vacuum at 60°C, burned in air at 750°C for 2 hours, soaked in...

Embodiment 2

[0017] Commercially available 0.1-0.2μm TiO 2 Take 5g of the powder, press it under 5MPa to form two test pieces with a diameter of 20mm and a thickness of 5mm, and sinter at 600°C for 2 hours in an argon atmosphere. After the test piece is tightly wrapped with stainless steel mesh, stainless steel wire is wound on the long stainless steel wire as the working electrode, graphite rod is used as the counter electrode, and the mixture of LiCl and KCl with a molar ratio of 1:1 is used as the electrolyte. In the atmosphere, the temperature is 600°C, the voltage is 2.8V, and the cathode is polarized for 4 hours. After the cathode polarization is completed, the anodic polarization is performed on the working electrode. The voltage is 2.0V, and the polarization time is 1 hour. After cooling to room temperature in the electrolytic tank, the product was taken out, washed with distilled water, dried in vacuum at 60°C, burned in air at 600°C for 3 hours, and soaked in 0.5mol / L hydrochlori...

Embodiment 3

[0019] Commercially available 0.1-0.2μm TiO 2 , take 0.5g, press under 10MPa to form a test piece with a diameter of 5mm and a thickness of 1mm, and sinter at 600°C for 3 hours in an argon atmosphere. The test piece is wound with molybdenum wire to make the working electrode, the graphite rod is used as the counter electrode, and the mixture of LiCl, KCl and NaCl with a molar ratio of 1:1:1 is used as the electrolyte, in an argon atmosphere, the temperature is 400 °C, the voltage 3.2V, cathodic polarization for 5 hours, after the cathodic polarization is completed, anodic polarization is performed on the working electrode, the voltage is 1.5V, and the polarization time is 1.5 hours. The product was taken out after room temperature, washed with distilled water, dried in vacuum at 60°C, burned in air at 850°C for 1 hour, and soaked in 0.5mol / L hydrochloric acid for 24 hours to obtain a titanium-based lithium ion sieve material. The above material was put into 20mL lithium chlor...

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Abstract

The invention discloses a preparation method of a titanium-based lithium ion sieve, which comprises the following steps of: compounding TiO2 powder or a tablet with a metal current collector to serve as a working electrode, taking graphite as a counter electrode, carrying out cathode polarization for 1-5 hours in alkali metal halide in an argon atmosphere at the temperature of 400-700 DEG C and the voltage of 2.0-3.2 V, carrying out anode polarization on the working electrode at the voltage of 1.0-2.6 V for 0.5-2 hours, cooling to normal temperature, taking out, washing, and carrying out vacuum drying to obtain a polarization product; and burning the obtained product in air at 600-900 DEG C for 1-3 hours and then cooling, acid-leaching the obtained product in 0.5-0.6 mol / L hydrochloric acid for 24-48 hours to obtain the titanium lithium ion sieve. The titanium-based lithium ion sieve has richer lithium ion channels, and the adsorption capacity of the titanium-based lithium ion sieve is effectively improved.

Description

Technical field: [0001] The invention relates to a preparation method of a titanium series lithium ion sieve. Background technique: [0002] At present, manganese-based ion sieves are mainly researched on lithium-ion sieves, but manganese-based ion sieves have defects such as large manganese dissolution loss and low number of cycles. The titanium-based lithium ion sieve has the advantages of less dissolution loss and stable structure. However, the titanium-based lithium ion sieves prepared by the existing preparation methods usually have defects such as elution, slow adsorption rate, uncontrollable particle size, and poor adsorption capacity, which are not conducive to industrial application. Therefore, there is an urgent need for new titanium-based lithium ion sieves. Invention content: [0003] The purpose of the present invention is to provide a preparation method of titanium-based lithium ion sieve, which can realize controllable particle size, ensure batch stability...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/04B01J20/30C22B3/24C22B26/12
CPCB01J20/06B01J20/041B01J20/3078B01J20/3085C22B3/24C22B26/12
Inventor 李伟刘志强王东兴朱薇陶进长高远
Owner GUANGDONG INST OF RARE METALS
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