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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 low tap density, reduce particle sintering, shorten calcination time, etc. The effect of low cost, energy saving and lithium consumption reduction

Active Publication Date: 2017-05-24
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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  • Preparation method of spinel-structure lithium titanate
  • Preparation method of spinel-structure lithium titanate
  • Preparation method of spinel-structure lithium titanate

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specific Embodiment approach

[0027] The present invention will be further described in detail below in conjunction with specific embodiments, which are explanations of the present invention rather than limitations.

[0028] The calcined seed crystal used in the present invention is the rutile crystal seed, specifically refers to the hydrated titanium dioxide colloidal particles added in the metatitanic acid bleaching process or salt treatment process in the production process of sulfuric acid titanium dioxide, which can promote the conversion of rutile crystal form.

[0029] Metatitanic acid is commonly known as hydrated titanium dioxide, therefore, when the present invention carries out the metering of metatitanic acid, all use TiO 2 count.

Embodiment 1

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

[0032] (1) get the metatitanic acid that iron content is 65mg / kg after secondary water washing in the sulfuric acid method titanium dioxide production process, add deionized water and make concentration be 350g / L (with TiO 2 meter) slurry A;

[0033] (2) Take 3.0L of slurry A, add 1.05L of slurry A with a concentration of 100g / L (using TiO 2 Calcined seed crystals), stirred for 3 hours, filtered, and washed with water until the pH value was greater than 1.8, the water washing was stopped, and the filter cake was made into 200g / L by adding deionized water (using TiO 2 meter) slurry B;

[0034] (3) According to the ratio of Li / Ti=0.88 (molar ratio), lithium carbonate powder was added to slurry B, and slurry C was obtained after stirring for 6 hours;

[0035] (4) Send slurry C into a rotary calciner with a specification of φ150x2000 for dehydration, desulfurization and calcination. The control p...

Embodiment 2

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

[0039] (1) Get the metatitanic acid that iron content is 28mg / kg after secondary water washing in the sulfuric acid method titanium dioxide production process, add deionized water and make concentration be 500g / L (with TiO 2 meter) slurry A;

[0040] (2) Take 2.0L of slurry A, add 0.4L of slurry A with a concentration of 50g / L (using TiO 2Calcined seed crystals), stirred for 2 hours, filtered, and washed with water until the pH value was greater than 1.8, the water washing was stopped, and the filter cake was made into 400g / L by adding deionized water (using TiO 2 meter) slurry B;

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

[0042] (4) Send the slurry C into a rotary calciner with a specification of φ150x2000 for dehydratio...

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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, in particular to a preparation method of spinel lithium titanate. Background technique [0002] Lithium titanate (Li 4 Ti 5 o 12 ) is used as a negative electrode material for lithium-ion batteries, and has the following outstanding properties: Lithium titanate with a spinel structure is called a "zero-strain" material because its lattice constant hardly changes during the lithium intercalation and desorption process; its theoretical The lithium intercalation potential is 1.55V ((VS.Li + / Li), although lithium titanate (Li 4 Ti 5 o 12 ) has a higher 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, it is not easy to form an SEI film, and there is no precipitation of lithium metal, which greatly improves the safety; in addition, its theory The spe...

Claims

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Application Information

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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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