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A kind of preparation method of spinel structure lithium titanate

A technology of structural lithium titanate and spinel, applied in titanate, alkali metal titanate, chemical instruments and methods, etc., can solve the problems of shortening calcination time, low tap density, and reducing particle sintering, etc. The effect of saving energy consumption, low cost and improving utilization efficiency

Active Publication Date: 2018-08-28
YUNNAN GANG FENG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition of calcined seeds (rutile seeds) in metatitanic acid shortens the calcination time, reduces particle sintering and overcomes the shortcoming of low tap density when metatitanic acid is directly used as a titanium source

Method used

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  • A kind of preparation method of spinel structure lithium titanate
  • A kind of preparation method of spinel structure lithium titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation of spinel structure lithium titanate includes the following steps:

[0032] (1) Take metatitanic acid with an iron content of 65mg / kg after the second water washing in the sulfuric acid method titanium dioxide production process, and add deionized water to make the concentration 350g / L (with TiO 2 Calculated) of slurry A;

[0033] (2) Take 3.0L slurry A, add 1.05L concentration to 100g / L (with TiO 2 Calculate the calcined seed crystal, stir for 3h, filter and wash with water until the pH value is greater than 1.8, stop washing, add deionized water to filter cake to make 200g / L (with TiO 2 Calculate) the slurry B;

[0034] (3) Add lithium carbonate powder to slurry B according to the ratio of Li / Ti=0.88 (molar ratio), and stir for 6 hours to prepare slurry C;

[0035] (4) The slurry C is sent to a rotary calcining kiln with a specification of φ150x2000 for dehydration, desulfurization and calcination. The control parameters of the rotary kiln are 320°C at the kiln...

Embodiment 2

[0038] The preparation of spinel structure lithium titanate includes the following steps:

[0039] (1) Take metatitanic acid with an iron content of 28mg / kg after the second water washing in the production process of sulfuric acid method titanium dioxide, add deionized water to make the concentration of 500g / L (with TiO 2 Calculated) of slurry A;

[0040] (2) Take 2.0L slurry A, add 0.4L with a concentration of 50g / L (with TiO 2 Calculate the calcined seed crystals), stir for 2h, filter and wash with water until the pH value is greater than 1.8, stop washing, and add deionized water to the filter cake to make 400g / L 2 Calculate) the slurry B;

[0041] (3) In accordance with the ratio of Li / Ti=0.97 (molar ratio), a lithium acetate solution with a concentration of 300g / L (calculated as lithium acetate) was added to slurry B, and stirred for 4 hours to prepare slurry C;

[0042] (4) The slurry C is sent to a rotary calcining kiln with a specification of φ150x2000 for dehydration, desulfur...

Embodiment 3

[0045] The preparation of spinel structure lithium titanate includes the following steps:

[0046] (1) Take metatitanic acid with an iron content of 80mg / kg after the second water washing in the sulfuric acid method titanium dioxide production process, add deionized water to make the concentration 250g / L (with TiO 2 Calculated) of slurry A;

[0047] (2) Take 4.0L slurry A, add 0.8L concentration 250g / L (with TiO 2 Calculate the calcined seed crystals), stir for 2h, filter and wash with water until the pH value is greater than 1.8, stop the water washing, add deionized water to the filter cake to make 200g / L (with TiO 2 Calculate) the slurry B;

[0048] (3) Add lithium sulfate powder to slurry B according to the ratio of Li / Ti=0.82 (molar ratio), and stir for 6 hours to prepare slurry C;

[0049] (4) The slurry C is sent to a rotary calcining kiln with a specification of φ150x2000 for dehydration, desulfurization and calcination. The control parameters of the rotary kiln are 400°C at th...

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Abstract

The invention provides a preparation method of spinel-structure lithium titanate. The preparation method comprises the following steps: 1, taking metatitanic acid produced in a process of producing titanium dioxide with a sulfuric acid method; preparing the metatitanic acid into slurry A with de-ionized water; 2, adding calcining seed crystals, which are widely used in a process of producing rutile-type titanium dioxide with the sulfuric acid method, into the slurry A, wherein the mass ratio of TiO2 in the calcining seed crystals to TiO2 in the slurry A is (2 to 20) to 100; after uniformly stirring, filtering and washing with water; stopping water washing when the pH (Potential of Hydrogen) value is greater than 1.8; adding de-ionized water into a filter cake to prepare slurry B with the TiO2 concentration of 200g / L to 400g / L; 3, adding a lithium source into the slurry B according to the mole ratio of Li to Ti of 0.82 to 0.97; sufficiently and uniformly stirring to obtain slurry C; 4, conveying the slurry C into a rotary kiln; heating and calcining to finish dehydration, desulfurization and crystal form transformation to prepare the spinel-structure lithium titanate. According to the preparation method provided by the invention, all the methods are slurry processes, and dry-method crushing and grinding do not need to be carried out before the crystal form transformation is finished by heating so that energy consumption is low; a titanium source is cheap and easy to obtain.

Description

Technical field [0001] The invention belongs to the field of preparation of inorganic non-metallic materials, and in particular relates to a preparation method of spinel structure lithium titanate. Background technique [0002] Lithium titanate (Li 4 Ti 5 O 12 ) Used as a negative electrode material for lithium-ion batteries, it has the following outstanding performance: Lithium titanate with spinel structure hardly changes its lattice constant during the process of lithium insertion and removal, so it is called a "zero strain" material; its theory The lithium insertion potential is 1.55V ((VS.Li + / Li), although lithium titanate (Li 4 Ti 5 O 12 ) Has a high platform potential, but its advantage is to ensure that it can be charged and discharged within the potential range where the organic electrolyte does not decompose, and it is not easy to form an SEI film, and there is no precipitation of lithium metal, which greatly improves safety; in addition, its theory The specific capac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00
CPCC01G23/005C01P2002/32C01P2002/72C01P2004/61C01P2006/11C01P2006/12C01P2006/80
Inventor 廖向阳朱贤荣谢宏伟王玲
Owner YUNNAN GANG FENG NEW MATERIAL CO LTD
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