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Method for synthesizing lithium titanate/titanium dioxide compound nano polycrystalline powder material by utilizing high-temperature and high-pressure mixed solvent thermal system

A technology for synthesizing lithium titanate and mixed solvents, which is applied in the growth of polycrystalline materials, chemical instruments and methods, nanotechnology for materials and surface science, etc., to achieve the effect of simplifying the synthesis steps, fast reaction process, and not easy to agglomerate

Active Publication Date: 2018-07-24
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching, it is found that there is no synthesis of (Li 4 Ti 5 o 12 / TiO 2 ) Relevant literature on composite nano-polycrystalline powder materials

Method used

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  • Method for synthesizing lithium titanate/titanium dioxide compound nano polycrystalline powder material by utilizing high-temperature and high-pressure mixed solvent thermal system
  • Method for synthesizing lithium titanate/titanium dioxide compound nano polycrystalline powder material by utilizing high-temperature and high-pressure mixed solvent thermal system
  • Method for synthesizing lithium titanate/titanium dioxide compound nano polycrystalline powder material by utilizing high-temperature and high-pressure mixed solvent thermal system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Ingredients:

[0045] Mix 70ml of methanol and 30ml of ultrapure water evenly, and then disperse 0.8392g of lithium hydroxide monohydrate and 7.45ml of titanium isopropoxide into the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0046] 2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0047] Put the sealed reaction vessel into a muffle furnace, heat it to 380°C (the pressure inside the vessel reaches 31.5MPa), and keep the temperature constant for 2 hours.

[0048] 3. Cooling:

[0049] The reaction kettle was naturally cooled to room temperature (20-25° C.), and the reaction kettle was taken out from the muffle furnace.

[0050] 4. Washing:

[0051] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.45 nm in a...

Embodiment 2

[0058] 1. Ingredients:

[0059] Mix 70ml of methanol and 30ml of ultrapure water evenly, and then disperse 0.8392g of lithium hydroxide monohydrate and 7.45ml of titanium isopropoxide into the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0060] 2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0061] Put the sealed reaction vessel into a muffle furnace, heat it to 340°C (the pressure inside the vessel reaches 22.3MPa), and keep the temperature constant for 2 hours.

[0062] 3. Cooling:

[0063] The reactor was cooled to room temperature (20-25° C.) at a cooling rate of 10° C. / h, and the reactor was taken out of the muffle furnace.

[0064] 4. Washing:

[0065] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.45 nm in...

Embodiment 3

[0072] 1. Ingredients:

[0073] Mix 60ml of methanol and 40ml of ultrapure water evenly, and then disperse 0.8392g of lithium hydroxide monohydrate and 7.45ml of titanium isopropoxide into the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0074] 2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0075] Put the sealed reaction kettle into a muffle furnace, heat it to 380°C (the pressure inside the vessel reaches 29.5MPa), and keep the temperature constant for 2 hours.

[0076] 3. Cooling:

[0077] The reactor was cooled to room temperature (20-25° C.) with ice water, and the reactor was taken out from the muffle furnace.

[0078] 4. Washing:

[0079] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.22 nanometers in aper...

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Abstract

The invention discloses a method for synthesizing a lithium titanate / titanium dioxide compound nano polycrystalline powder material by utilizing a high-temperature and high-pressure mixed solvent thermal system. The lithium titanate / titanium dioxide compound nano polycrystalline powder material is prepared by taking solid lithium hydroxide monohydrate powder and liquid titanium isopropylate as rawmaterials, taking a high-temperature and high-pressure mixed solvent as a reaction medium, reacting in a high-temperature and high-pressure container under the conditions that the pressure is 4 to 34MPa and the temperature is 260 to 400 DEG C and then calcining at 700 to 740 DEG C. The method disclosed by the invention has simple synthesis steps and a rapid and safe reaction process. A phase component of an obtained product is controllable and particle shapes are relatively regular; the particle size range is 20 to 100nm and the dispersity is relatively good. The method disclosed by the invention has unique advantages, a reaction process is easy to adjust and control, and energy saving and environment protection are realized, so that the method is especially suitable for industrial batchproduction.

Description

technical field [0001] The present invention relates to a kind of preparation method of composite polycrystalline powder that can be used as lithium-ion battery negative electrode material, relate in particular to a kind of synthesis lithium titanate / titanium dioxide (Li 4 Ti 5 o 12 / TiO 2 ) method for composite nano polycrystalline powder material. Background technique [0002] Titanium-based oxides (such as titanate compounds and titanium dioxide) are a typical class of safe lithium-ion battery anode materials. Its structural stability and safety properties make this type of compound have very important application value in the field of lithium-ion batteries. Lithium titanate (Li 4 Ti 5 o 12 ) has a theoretical capacitance of 175mAh / g, and is a zero-strain material that hardly changes its structure during the process of intercalation and extraction of lithium ions. It has the characteristics of good cycle performance and high Coulombic efficiency. Titanium dioxide ...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/48H01M4/485H01M10/0525C30B28/04C30B29/32B82Y30/00
CPCB82Y30/00C30B28/04C30B29/32H01M4/362H01M4/48H01M4/485H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 李博陶绪堂刘阳阳张梦起张玉鹏
Owner SHANDONG UNIV
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