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Method for fast preparing small-particle-diameter anatase type nanometer titanium dioxide

A nano-titanium dioxide and anatase-type technology, which is applied in the field of nano-materials, can solve the problems of cumbersome procedures, difficult product grain size to reach the nanometer level, and insufficient simplicity, so as to achieve good photocatalytic activity, good application prospects, and time-consuming short effect

Inactive Publication Date: 2018-06-22
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the sol-gel method is widely used, the process is cumbersome and not simple enough. Moreover, the crystal grain size of the product is difficult to reach the nanometer level by using the above synthesis method.

Method used

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  • Method for fast preparing small-particle-diameter anatase type nanometer titanium dioxide
  • Method for fast preparing small-particle-diameter anatase type nanometer titanium dioxide
  • Method for fast preparing small-particle-diameter anatase type nanometer titanium dioxide

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A method for rapidly synthesizing anatase nano-titanium dioxide, the specific steps are as follows:

[0032] (1) Add 1.5mL of ammonia water (concentration 10mol / L) to a mixture of 40mL of deionized water and 10mL of ethylene glycol, and add 2mL of tetrabutyl titanate and 1mL of 1- Butyl-3-methylimidazolium tetrafluoroborate;

[0033] (2) Transfer the uniformly mixed above-mentioned solution to a microwave reactor, and heat it at 180° C. for 10 minutes by microwave hydrothermal method;

[0034] (3) After the reaction kettle is cooled to room temperature, take out the reaction solution, centrifuge and wash alternately with deionized water and ethanol. After washing several times, put the sample in an oven at 60°C for at least 12 hours, and then transfer it to a muffle furnace. The temperature was raised to 600°C at a rate of 1°C / min, kept for 4 hours for calcination, and finally cooled with the furnace to obtain a titanium dioxide sample.

[0035] Figure 4 c is a larg...

Embodiment 2

[0063] A method for rapidly synthesizing anatase nano-titanium dioxide, comprising the following steps:

[0064] (1) Add 1.5 mL of ammonia water (concentration 10 mol / L) to a mixed solution of 40 mL of deionized water and 10 mL of ethylene glycol, and add 2 mL of tetrabutyl titanate and 1 mL of 1- Butyl-3-methylimidazolium tetrafluoroborate;

[0065] (2) Transfer the uniformly mixed above-mentioned solution to a microwave reactor, and heat it at 150° C. for 15 minutes by microwave hydrothermal method;

[0066] (3) After the reaction kettle is cooled to room temperature, take out the reaction solution, centrifuge and wash alternately with deionized water and ethanol. After washing several times, put the sample in an oven at 60°C for at least 12 hours, and then transfer it to a muffle furnace. Raise the temperature to 650°C at a rate of 3°C / min, keep the temperature for 4h for calcination, and finally cool down with the furnace to obtain a titanium dioxide sample.

[0067] The...

Embodiment 3

[0069] A method for rapidly synthesizing anatase nano-titanium dioxide, comprising the following steps:

[0070] (1) Add 1.5 mL of ammonia water (concentration 15 mol / L) into a mixed solution of 40 mL of deionized water and 10 mL of ethylene glycol, and add 2 mL of tetrabutyl titanate and 1 mL of 1- Butyl-3-methylimidazolium tetrafluoroborate;

[0071] (2) Transfer the uniformly mixed above-mentioned solution to a microwave reactor, and heat it at 180° C. for 10 minutes by microwave hydrothermal method;

[0072] (3) After the reaction kettle is cooled to room temperature, take out the reaction solution, centrifuge and wash alternately with deionized water and ethanol. After washing several times, put the sample in an oven at 60°C for at least 12 hours, and then transfer it to a muffle furnace. Raise the temperature to 550°C at a rate of 1°C / min, keep the temperature for 6h for calcination, and finally cool down with the furnace to obtain a titanium dioxide sample.

[0073] T...

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Abstract

The invention relates to a method for fast preparing small-particle-diameter anatase type nanometer titanium dioxide. The method comprises the following steps of (1) mixing deionized water and ethanediol to obtain a mixed solution of deionized water and ethanediol; using ammonium hydroxide for regulating the pH of the mixed solution into a basic state; then, gradually adding tetrabutyl titanate and 1-butyl-3-methylimidazolium tetrafluoroborate into the mixed solution drip by drip during the stirring so as to obtain the uniformly mixed reaction solution; (2) transferring the reaction solution obtained in the step (1) into a microwave reaction kettle for hydrothermal reaction; after the reaction is completed, performing centrifugation separation, washing and drying on the solid products; then, performing roasting to obtain the small-particle-diameter anatase type nanometer titanium dioxide. Under the condition of existence of a proper amount of ammonium hydroxide, the deionized water andthe ethanediol are used as the solvents; fluorine-containing ionic liquid is used for preparation so as to obtain the small-particle-diameter anatase nanometer titanium dioxide. In the synthesis process, only 10 to 30 min is needed; the time consumption is short; simplicity and convenience are realized; the production efficiency is high; the industrialization is facilitated.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a method for rapidly preparing small-diameter anatase-type nano-titanium dioxide. Background technique [0002] As a semiconductor material with excellent performance, titanium dioxide is widely used in the fields of environment and energy because of its good photocatalytic activity, high chemical and thermal stability, and non-toxicity. [0003] The methods for preparing nano-titanium dioxide mainly include gas-phase synthesis and liquid-phase synthesis. The gas-phase synthesis method has high requirements on the reaction equipment, and the yield is not very ideal, so it is rarely used, while the liquid-phase synthesis method has the advantages of low reaction temperature, simple equipment, and low energy consumption, and has become the current laboratory and industrial method. Widely used methods, wherein the sol-gel method is the most commonly used method for preparing ...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82Y30/00
CPCB82Y30/00C01G23/053C01P2002/72C01P2004/03C01P2004/04C01P2004/64C01P2006/12Y02P20/54
Inventor 阳晓宇肖曼杰肖洒王永黎新肖冰玉钱心怡王雪琴郭定城王赫匡玥
Owner WUHAN UNIV OF TECH
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