CN104591273A - A kind of preparation method of Ti3+doped titanium dioxide synthesized by alcohol thermal method - Google Patents

Abstract

The invention discloses a preparation method of synthesizing Ti<3+>-doped titanium dioxide by using an alcohol thermal method. The method comprises the following steps: firstly, configuring precursor solutions prepared by mixing precursor of titanium and alcohol solvents under a constant temperature; then, transferring the precursor solutions to a hydrothermal kettle to control the solvothermal temperature to be between 433K and 623K for 12 to 240 hours to obtain Ti<3+>-doped titanium dioxide. Titanium dioxide moderated with Ti<3+> has potential application possibly in the other fields such as solar batteries and photoelectric materials.

Description

A kind of preparation method of Ti3+doped titanium dioxide synthesized by alcohol thermal method

technical field

The invention relates to a preparation method for synthesizing Ti ³⁺ doped titanium dioxide by an alcohol thermal method.

technical background

With the increasingly severe environmental problems and increasing air and water pollution, the use of photocatalytic technology to treat various pollutants in the environment has become the focus of people's attention. Titanium dioxide (TiO ₂ ) is known for its non-toxicity and catalytic activity. The advantages of high photocatalyst, good chemical stability, cheap and easy to obtain, and direct use of sunlight have attracted people's attention and become a typical photocatalyst. Titanium dioxide, because of its own band gap of 3.2eV, determines that it can only be excited by ultraviolet light that only accounts for 5% of sunlight to generate photogenerated electrons and holes, which are used to redox organic pollutants. Therefore, how to expand the light absorption of titanium dioxide has become the focus of attention. As one of the most commonly used methods, modification of titanium dioxide can effectively reduce the energy band of titanium dioxide and improve its absorption of visible light. Ti ³⁺ modification has the advantages of simple experimental operation and significant enhancement of light absorption, and is one of the ideal ways to design new visible light catalysts of titanium dioxide.

The alcohol solvothermal method is applied to the heat treatment of the titanium precursor sol, and the alcohol is reduced to Ti ³⁺ by the high temperature and high pressure environment, and Ti ³⁺ in situ modified titanium dioxide can be synthesized in situ in one step ^. By adjusting the synthesis temperature and reaction time, not only the light absorption of titanium dioxide is expanded, but also compared with other metals, non-metal doped titanium dioxide and Ti ³⁺ modified titanium dioxide prepared by means of high-energy ion bombardment, its advantage is that it does not Other impurities are introduced, and the synthesis process has low requirements, low cost and good stability. Because it is formed by reaction under high temperature and high pressure environment, this Ti ³⁺ in situ modified titanium dioxide has good thermal stability, and at the same time increases the light absorption of TiO ₂ and improves the utilization rate of light, thereby improving its photocatalytic activity.

Contents of the invention

The purpose of the present invention is to propose a new method for the convenient and rapid synthesis of Ti ³⁺ doped titanium dioxide.

A kind of preparation method of synthesizing Ti ³⁺ doped titanium dioxide by alcohol thermal method, it is characterized in that, carry out according to the following steps:

First, configure a precursor solution composed of a titanium precursor and an alcohol solvent at room temperature;

Then, the precursor solution was transferred to a hydrothermal tank, and the solvothermal temperature was controlled at 433K to 623K, and the time was 12h to 240h to obtain Ti ³⁺ doped titanium dioxide.

The alcohol solvent is a monohydric or polyhydric alcohol with one to four carbon atoms, such as methanol, ethanol, isopropanol, ethylene glycol, butanol, benzyl alcohol.

The titanium precursor is one or two of titanium tetrafluoride, titanium tetrachloride, tetrabutyl titanate, titanium trichloride and titanyl sulfate.

The molar ratio of titanium precursor to alcohol solvent is 1:1 to 1:3000.

In the present invention, Ti ³⁺ doped titanium dioxide can be obtained by adjusting the ratio of the precursor solution, alcohol heating time and temperature. This Ti ³⁺ in-situ modified titanium dioxide may have potential applications in other fields, such as solar cells and optoelectronic materials.

Description of drawings

FIG. 1 is a typical powder crystal diffraction XRD pattern of a Ti ³⁺ doped titanium dioxide sample in Example 1.

FIG. 2 is a typical solid ultraviolet diffuse reflectance diagram of a Ti ³⁺ doped titanium dioxide sample in Example 1.

FIG. 3 is a typical optical photo of the Ti ³⁺ doped titanium dioxide sample in Example 1.

Detailed ways

Example 1

At room temperature, add 1mL of titanium trichloride (70wt%) and 1mL of tetrabutyl titanate into 30mL of ethanol, stir well, and transfer the solution without solid precipitation to a 50mL hydrothermal kettle, and put it in an oven for 200 ℃, 14h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 2

At room temperature, add 0.05g of titanium tetrafluoride into 20mL of absolute ethanol, stir well to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it in an oven to keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 3

At room temperature, add 0.05g of titanium tetrafluoride into 20mL of tert-butanol, stir well to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it into an oven to keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 4

At room temperature, add 0.05g of titanium tetrafluoride into 20mL of methanol, stir well to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it into an oven to keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 5

At room temperature, add 0.05g of titanium tetrafluoride into 20mL of ethylene glycol, stir well to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it into an oven to keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 6

At room temperature, add 1 mL of titanium tetrachloride (AR, 99%) into 20 mL of tert-butanol, stir well to obtain a colorless and transparent solution, transfer it to a 50 mL hydrothermal kettle, and put it in an oven at 200°C for 24 hours. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 7

At room temperature, add 0.05g of titanium tetrafluoride and 0.2mL of tetrabutyl titanate into 30mL of ethanol at a molar ratio of 1:1, stir thoroughly to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it in an oven Keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Example 8

At room temperature, add 1.0mL of titanium tetrachloride and 3.0mL of tetrabutyl titanate to 30mL of ethanol at a molar ratio of 1:1, stir thoroughly to obtain a colorless and transparent solution, transfer it to a 50mL hydrothermal kettle, and put it in an oven Keep at 250°C for 24h. Take it out and cool it down to room temperature naturally, wash and dry to obtain Ti ³⁺ doped titanium dioxide.

Claims (4)

1. a kind of alcohol thermal method is synthesized Ti The preparation method of doped titanium ^dioxide is characterized in that, carries out according to the following steps: First, configure a precursor solution composed of a titanium precursor and an alcohol solvent at room temperature; Then, the precursor solution was transferred to a hydrothermal tank, and the solvothermal temperature was controlled at 433K to 623K, and the time was 12h to 240h to obtain Ti ³⁺ doped titanium dioxide. 2. preparation method according to claim 1, is characterized in that, described alcohol solvent is the monohydric or polyhydric alcohol of one to four carbon atoms, as methyl alcohol, ethanol, Virahol, ethylene glycol, butanol, benzene Methanol. 3. The preparation method according to claim 1, wherein the titanium precursor is one of titanium tetrafluoride, titanium tetrachloride, tetrabutyl titanate, titanium trichloride and titanyl sulfate one or two. 4. The preparation method according to claim 1, characterized in that the molar ratio of the titanium precursor to the alcohol solvent is 1:1 to 1:3000.