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Hydrothermal synthesis method of micro-emulsion of nano lithium titanate

A nano-lithium titanate, hydrothermal synthesis technology, applied in the direction of titanium compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex synthesis route, poor sample dispersibility, high synthesis cost, and achieve simple process, low cost, The effect of increasing crystallinity

Inactive Publication Date: 2013-09-04
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods often have complex synthetic routes, high synthetic costs, low yields, and the prepared samples usually have poor dispersion and serious agglomeration.

Method used

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  • Hydrothermal synthesis method of micro-emulsion of nano lithium titanate
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  • Hydrothermal synthesis method of micro-emulsion of nano lithium titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Mix the raw materials cetyltrimethylammonium bromide, n-hexanol, cyclohexane and deionized water to prepare two identical microemulsions. Wherein the concentration of cetyltrimethylammonium bromide is 0.01-1.2 mol / liter, the concentration of cyclohexane is 3-7 mol / liter, and the amount of deionized water is the same as that of cetyltrimethylammonium bromide. The ratio of the amount of substance of ammonium bromide is: 10-80, the ratio of the amount of substance of n-hexanol to the amount of substance of cetyltrimethylammonium bromide is: 2-30;

[0028] (2) Lithium hydroxide and titanium tetraisopropoxide were added to the above two microemulsions respectively, stirred at room temperature for 5-30 minutes, and microemulsions containing lithium hydroxide and titanium tetraisopropoxide were prepared respectively. Wherein the concentration of lithium hydroxide is 0.1-1.2 mol / liter, and the concentration of titanium tetraisopropoxide is 0.15-1.5 mol / liter;

[0029] (3) ...

Embodiment 2

[0032] (1) Mix the raw materials cetyltrimethylammonium bromide, n-hexanol, cyclohexane and deionized water to prepare two identical microemulsions. Wherein the concentration of cetyltrimethylammonium bromide is 0.05-1.0 mol / liter, the concentration of cyclohexane is 3-6 mol / liter, and the amount of deionized water is the same as that of cetyltrimethylammonium bromide. The ratio of the amount of substance of ammonium bromide is: 12-75, and the ratio of the amount of substance of n-hexanol to the amount of substance of cetyltrimethylammonium bromide is: 3-60;

[0033] (2) Lithium acetate and titanium tetraisopropoxide were added to the above two microemulsions respectively, stirred at room temperature for 10-30 minutes, and microemulsions containing lithium acetate and titanium tetraisopropoxide were prepared respectively. Wherein the concentration of lithium hydroxide is 0.2-0.7 mol / liter, and the concentration of titanium tetraisopropoxide is 0.25-0.9 mol / liter;

[0034] (3)...

Embodiment 3

[0037] (1) Mix raw materials sodium lauryl sulfate, n-hexanol, cyclohexane and deionized water to prepare two identical microemulsions. Wherein the concentration of sodium lauryl sulfate is 0.06-0.8 mole / liter, the concentration of cyclohexane is 3.5-6 mole / liter, and the amount of substance of deionized water is equal to the amount of substance of sodium lauryl sulfate The ratio is: 15-70, the ratio of the amount of substance of n-hexanol to the amount of substance of sodium lauryl sulfate is: 2-70;

[0038] (2) Lithium nitrate and tetrabutyl titanate were added to the above two microemulsions respectively, stirred at room temperature for 5-30 minutes, and microemulsions containing lithium nitrate and tetrabutyl titanate were prepared respectively. Wherein the concentration of lithium hydroxide is 0.1-1.0 mol / liter, the concentration of tetrabutyl titanate is 0.12-1.3 mol / liter;

[0039] (3) After mixing the above two microemulsions, continue to stir for 10-30 minutes, then ...

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Abstract

The invention discloses a hydrothermal synthesis method of a micro-emulsion of nano lithium titanate. According to the method disclosed by the invention, the micro-emulsion is prepared from cetyltrimethylammonium bromide, n-hexanol, cyclohexane and a water phase, and tetrabutyl titanate and lithium hydroxide are used as reaction materials. The method comprises the steps of: (1) preparing the 0.02-2.0 mol / L lithium hydroxide micro-emulsion and 0.025-2.5 mol / L titanium tetraisopropoxide micro-emulsion respectively; and (2) mixing the micro-emulsions in two concentrates, stirring for 5-120 minutes at the room temperature, then transferring a mixture into a 50 ml high-pressure reactor which is lined with polytetrafluoroethylene, carrying out hydrothermal reaction at the temperature of 60-240 DEG C for 1-70 hours, and then carrying out centrifugal separation, washing, drying and thermal treatment on a reactant to obtain spinel type lithium titanate. The method has the characteristics of controllable grain size, controllable morphology, simple process, simple equipment and the like.

Description

technical field [0001] The invention relates to a preparation method of an inorganic functional material, in particular to a method for preparing lithium ion battery negative electrode material nano lithium titanate by using a microemulsion-hydrothermal method, and belongs to the technical field of inorganic advanced nano material preparation technology. Background technique [0002] Lithium-ion batteries have been used more and more widely because of their advantages such as high energy density, high output voltage, long service life and low environmental pollution. With the development of the electric vehicle industry, higher requirements are placed on the charging and discharging performance and safety of lithium-ion batteries. Traditional carbon anode materials can no longer meet the requirements of high-power lithium-ion batteries due to their low theoretical capacity, poor rate performance, and safety issues. Therefore, it is urgent to develop anode materials with exce...

Claims

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Application Information

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IPC IPC(8): C01G23/00H01M4/485
CPCY02E60/10
Inventor 刘光印王慧远戚文杨治政王邦勇
Owner JILIN UNIV
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