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A kind of preparation method of titanium series lithium ion sieve

A technology of lithium ion and titanium series, applied in the field of preparation of titanium series lithium ion sieve, can solve the problems of slow adsorption rate, unfavorable industrial application, poor adsorption capacity, etc., and achieve the effect of increasing adsorption capacity and enriching lithium ion channels

Active Publication Date: 2022-07-26
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] The commercially available 0.1-0.2 μm TiO 2 Take 2 g of the powder, press it into a test piece with a diameter of 20 mm and a thickness of 3 mm under 8 MPa, and sinter it at 600 °C for 3 hours in an argon atmosphere to obtain TiO 2 Audition. After tightly wrapping the test piece with molybdenum mesh, the thin 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, the cathodic polarization is 5 hours, and after the cathodic polarization is completed, the working electrode is anodically polarized, 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, calcined in air at 750°C for 2 hours, and soaked i...

Embodiment 2

[0017] The commercially available 0.1-0.2 μm TiO 2 Take 5 g of the powder, press it into two test pieces with a diameter of 20 mm and a thickness of 5 mm under 5 MPa, and sinter at 600° C. for 2 hours in an argon atmosphere. After the test piece was tightly wrapped with stainless steel mesh, the stainless steel wire was wound on the long stainless steel wire as the working electrode, the graphite rod was used as the counter electrode, and the mixture of LiCl and KCl with a molar ratio of 1:1 was used as the electrolyte. In the atmosphere, the temperature is 600°C, the voltage is 2.8V, the cathodic polarization is 4 hours, and after the cathodic polarization is completed, the working electrode is anodically polarized, the voltage is 2.0V, and the polarization time is 1 hour. After the liquid level was cooled to room temperature in the electrolytic cell, the product was taken out, washed with distilled water, dried in vacuum at 60°C, calcined in air at 600°C for 3 hours, and soa...

Embodiment 3

[0019] The commercially available 0.1-0.2 μm TiO 2 , take 0.5 g, press it into a test piece with a diameter of 5 mm and a thickness of 1 mm under 10 MPa, and sinter at 600 ° C for 3 hours in an argon atmosphere. The test piece was wound with molybdenum wire to make a working electrode, a graphite rod was used as the counter electrode, and a mixture of LiCl, KCl and NaCl in a molar ratio of 1:1:1 was used as the electrolyte. In an argon atmosphere, the temperature was 400 °C, and the voltage It is 3.2V, and the cathode is polarized for 5 hours. After the cathodic polarization is completed, the working electrode is anodically polarized. The voltage is 1.5V, and the polarization time is 1.5 hours. The product was taken out at room temperature, washed with distilled water, dried in a vacuum at 60°C, calcined at 850°C in air 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 materials were put into 20 ...

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Abstract

The invention discloses a preparation method of a titanium-based lithium ion sieve. 2 The powder or tablet is combined with a metal current collector as the working electrode, with graphite as the counter electrode, in an alkali metal halide, in an argon atmosphere, the temperature is 400 ~ 700 ° C, the voltage is 2.0 ~ 3.2V, and the cathode polarization is performed 1 ~5 hours, and then the working electrode was polarized at 1.0 ~ 2.6V, the polarization time was 0.5 ~ 2 hours, cooled to room temperature, taken out, then washed, and vacuum dried to obtain a polarized product; the obtained product was 600 in air. After burning at ~900℃ for 1~3 hours, then cooling, the obtained product is acid leached in 0.5~0.6mol / L hydrochloric acid for 24~48h to obtain a titanium-based lithium ion sieve with more abundant lithium ion channels, which effectively improves its adsorption. quantity.

Description

Technical field: [0001] The invention relates to a preparation method of a titanium-based lithium ion sieve. Background technique: [0002] At present, manganese-based ion sieves are mainly studied for lithium ion sieves, but manganese-based ion sieves have defects such as large manganese dissolution loss and few 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 slow elution, slow adsorption rate, uncontrollable particle size, and poor adsorption capacity, which are not conducive to industrial application. Therefore, new titanium-based lithium ion sieves are urgently needed. Invention content: [0003] The purpose of the present invention is to provide a preparation method of a titanium-based lithium ion sieve, which can realize controllable particle size, ensure batch stability, consistency ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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