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Method for preparing spherical lithium titanate from inorganic titanium sources

A technology of inorganic titanium and lithium titanate, applied in the direction of inorganic chemistry, chemical instruments and methods, titanium compounds, etc., to achieve the effects of convenient industrial production, good appearance, and superior electrochemical performance

Active Publication Date: 2011-08-17
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, there is no report on the preparation of spherical lithium titanate from inorganic titanium sources

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  • Method for preparing spherical lithium titanate from inorganic titanium sources
  • Method for preparing spherical lithium titanate from inorganic titanium sources
  • Method for preparing spherical lithium titanate from inorganic titanium sources

Examples

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Embodiment 1

[0039] The titanium source is 15g of chemically pure titanium sulfate, which is dissolved in water. In the experiment, 10wt.% ammonia water is used to adjust the pH to 3, and the titanium precipitate is obtained by filtration; the precipitate is beaten with distilled water, and hydrogen peroxide solution is added. The molar ratio of hydrogen peroxide and titanium is The ratio is 1. During the reaction process, use 0.5mol / L ammonia water to adjust the pH of the solution to 7, then react in a stirred reactor at 20°C, filter to obtain a titanium solution after 10 minutes, and then pour it into a 1000ml beaker; Lithium hydroxide solution was added to the solution, and the molar ratio of lithium hydroxide to titanium was 4:5; the solution was stirred for 10 minutes and then spray-dried. A precursor of lithium titanate, a negative electrode material for lithium ion batteries, is obtained; the precursor is calcined at 600° C. for 12 hours in an argon atmosphere to obtain lithium titan...

Embodiment 2

[0041] The titanium source is ilmenite at 120°C, the ratio of acid to mineral is 1.2:1, 5g of hydrolyzed high-titanium slag after hydrochloric acid leaching for 2 hours, beat the titanium slag with distilled water, add hydrogen peroxide solution, and the molar ratio of hydrogen peroxide to titanium It is 6: 1, and the pH of the solution is adjusted to 10.5 with 30wt.% ammonia water in the experiment, and then reacted in a stirred reactor at 35°C for 50 minutes, filtered to obtain a titanium solution, and poured into a beaker with a volume of 1000ml; Add lithium hydroxide solution, the molar ratio of lithium hydroxide to titanium is 4:5; stir for 10 minutes, spray and dry under the conditions of inlet air temperature 140°C, outlet air temperature 120°C and feed rate 100ml / h to obtain a lithium ion battery The precursor of the material lithium titanate; the precursor is calcined at 900° C. for 5 hours in an argon atmosphere to obtain lithium titanate, a negative electrode materia...

Embodiment 3

[0043] The titanium source is 10g of chemically pure titanium tetrachloride, which is dissolved in water. In the experiment, 0.1mol / L sodium hydroxide solution is used to adjust the pH to 4, and the titanium precipitate is obtained by filtration; the titanium precipitate is beaten with distilled water, and hydrogen peroxide is added. Solution, the molar ratio of hydrogen peroxide and titanium is 10: 1, adjust the pH of the solution with 20wt.% ammonia water to be 12, react in a stirred reactor at 80°C, react for 360min, filter to obtain the solution of titanium; Lithium acetate solution was added to the solution, and the molar ratio of lithium to titanium was 4:5; stirred for 10 minutes, and spray-dried at an inlet air temperature of 200°C, an outlet air temperature of 140°C and a feed rate of 1000ml / h to obtain a lithium-ion battery The precursor of the material lithium titanate; the precursor is calcined at 800° C. for 12 hours in a nitrogen atmosphere to obtain lithium titan...

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Abstract

The invention discloses a method for preparing spherical lithium titanate from inorganic titanium sources. The method comprises the following steps: pulping the titanium precipitate prepared from titanic acid or ilmenite and industrial titanic solution with water, adding a coordinating agent to the pulp according to the molar ratio of the coordinating agent to titanium being (1.0:1)-(20:1), adjusting the pH value to be 7-14 with alkali, then carrying out reaction in a stirred reactor at the temperature of 10-80 DEG C for 5-720min and filtering the reactant to obtain titanium solution; adding lithium sources to the solution according to the molar ratio of lithium to titanium being 4:5; and then carrying out spray drying on the mixed solution to obtain a lithium titanate precursor and calcining the precursor in the inert atmosphere at the temperature of 550-900 DEG C for 1-72 hours to obtain lithium titanate, the cathode material of lithium ion batteries. The method has the characteristics of wide raw material range, simple process flows, low energy consumption, low cost, good product particle size and morphology, high purity and excellent electrochemical property.

Description

Technical field: [0001] The invention relates to a method for preparing lithium titanate, a negative electrode material of a lithium ion battery, in particular to a method for preparing spherical lithium titanate from an inorganic titanium source. Background technique: [0002] Lithium-ion batteries are a new generation of green and environmentally friendly batteries that were put on the market after the 1990s. They are widely used in portable appliances because of their advantages such as high working voltage, high specific energy, long cycle life, low self-discharge power, no memory effect, and no pollution. and electric vehicles. The anode material of lithium ion battery is one of the key factors restricting its overall performance. The negative electrode materials used in the earliest commercialized lithium-ion batteries are almost all carbon / graphite materials, but because the electrode potential of carbon is very close to that of lithium, when the battery is overcharg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00
Inventor 吴飞翔李新海王志兴郭华军彭文杰贺振江熊训辉胡启阳张云河
Owner CENT SOUTH UNIV
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