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Preparation method of brookite titanium doxide nano-rod

A technology of titanium dioxide and brookite, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc.

Active Publication Date: 2015-07-08
CAPITAL NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of high-purity brookite-type titania nanorods by one-step hydrothermal method assisted by inorganic salts has not been reported yet.

Method used

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  • Preparation method of brookite titanium doxide nano-rod

Examples

Experimental program
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Embodiment 1

[0023] (1) 10ml of tetra-n-butyl titanate was added to 3.4ml of trifluoroacetic acid solution with a mass concentration of 50% for hydrolysis, wherein the molar ratio of tetra-n-butyl titanate: trifluoroacetic acid was 1:0.5, and it was heated violently at room temperature After stirring for 1 hour, the obtained tan solution was directly dried in the air at room temperature to remove volatile by-products to obtain a soluble xerogel;

[0024] (2) Dissolve 0.5 g of the soluble xerogel obtained in step (1) in 20 mL of water, add 0.84 g of NaF to make the NaF concentration 1 mol / L, and then put the mixed solution into a polytetrafluoroethylene-lined stainless steel autoclave , 180 ℃ hydrothermal reaction for 24 hours. After the reaction, the precipitated product obtained is filtered, washed and dried to obtain brookite titanium dioxide nanorods. The prepared nanorods have a diameter of 14nm and a length of 220nm, such as figure 1 shown.

Embodiment 2

[0026] (1) 10ml of tetra-n-butyl titanate was added to 6.8ml of trifluoroacetic acid solution with a mass concentration of 50% for hydrolysis, wherein the molar ratio of tetra-n-butyl titanate: trifluoroacetic acid was 1: 1. After stirring for 1 hour, the obtained tan solution was directly dried in the air at room temperature to remove volatile by-products to obtain a soluble xerogel;

[0027] (2) Dissolve 0.5 g of the soluble xerogel obtained in step (1) in 20 mL of water, add 1.16 g of KF to make the KF concentration 1 mol / L, and then put the mixed solution into a polytetrafluoroethylene-lined stainless steel autoclave , 230 ℃ hydrothermal reaction for 48 hours. After the reaction, the precipitated product obtained is filtered, washed and dried to obtain brookite titanium dioxide nanorods. The prepared nanorods have a diameter of 20nm, a length of 300nm, and a purity of 98%, such as figure 2 shown.

Embodiment 3

[0029] (1) Add 10ml of tetra-n-butyl titanate to 13.6ml of trichloroacetic acid solution with a mass concentration of 75% for hydrolysis, wherein the molar ratio of tetra-n-butyl titanate: trichloroacetic acid is 1:3, and the After stirring for 1 hour, the obtained tan solution was directly dried in the air at room temperature to remove volatile by-products to obtain a soluble xerogel;

[0030] (2) Dissolve 0.8 g of soluble xerogel obtained in step (1) in 20 mL of water, add 2.12 g of Na 2 CO 3 , so that Na 2 CO 3 The concentration was 1 mol / L, and then the mixed solution was put into a polytetrafluoroethylene-lined stainless steel autoclave for a hydrothermal reaction at 180°C for 48 hours. After the reaction, the precipitated product obtained is filtered, washed and dried to obtain brookite titanium dioxide nanorods. The prepared nanorods have a diameter of 25nm, a length of 200nm, and a purity of 96%.

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Abstract

The invention relates to a preparation method of brookite titanium doxide nano-rods, which comprises following steps: (1) hydrolyzing titanate in an organic acid aqueous solution and drying a hydrolysis product to obtain a soluble dry gel; (2) dissolving the soluble dry gel in water with addition of an inorganic salt aqueous solution; and (3) performing a hydrothermal reaction in a high-pressure reaction kettle to prepare the high-purity brookite titanium doxide nano-rods. The preparation method is simple in operation, is low in cost, is high in purity of the product, brookite titanium doxide nano-rods, and can producing the brookite titanium doxide nano-rods commercially in large scales.

Description

technical field [0001] The invention relates to a preparation method of brookite titanium dioxide nanorods. Background technique [0002] Nano-TiO 2 Due to the advantages of non-toxicity, low price, and high catalytic activity, it has received extensive attention in the fields of photocatalysis, solar cells, and photolysis of water to produce hydrogen. It has always been a hot spot in the field of energy and environment research, and is widely used in air purification and sewage treatment and other environmental fields. [0003] Affect TiO 2 There are many factors affecting the separation efficiency of photogenerated electrons and holes, such as crystal form, grain size, specific surface area, doping, etc., among which the most important factor is the crystal form. TiO 2 There are three common crystal forms: anatase, rutile and brookite, among which anatase has the highest photocatalytic activity. The photocatalytic activity of brookite titanium dioxide is close to that...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82Y30/00B82Y40/00
Inventor 孟祥福吕立贞刘秀云王苗苗
Owner CAPITAL NORMAL UNIVERSITY
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