Titanium black material for cosmetic and indoor pollution gas treatment and preparation method thereof

Abstract

The application discloses a titanium black material for cosmetic and indoor pollution gas treatment and a preparation method thereof, and belongs to the technical field of green chemistry. First, sulfur powder is dissolved in oleylamine, tetrabutyl titanate is added into the oleylamine, a precursor solution is obtained through a hydrothermal reaction, anhydrous ethanol is added for precipitation of powder, and the titanium black precursor powder is sealed and subjected to heat treatment, and the titanium black material for cosmetic and indoor pollution gas treatment is obtained after natural cooling at room temperature. In the application, oxygen defects are introduced on the surface of TiO2 by using sulfur, a precursor powder is obtained by using a sealed hydrothermal technology, and the precursor powder is subjected to sealed heat treatment, so that the titanium black powder with an anatase crystal form is prepared. The method has the characteristics of simple process, green and safe preparation process, environmental friendliness and low cost, and the titanium black material prepared in the application can effectively degrade organic solvents such as acetone remaining and existing in chemical production environment and air pollutants.

Description

Technical Field

[0001] This invention belongs to the field of green chemistry technology, specifically relating to a titanium black material for cosmetics and indoor air pollution treatment, and its preparation method. Background Technology

[0002] In cosmetic manufacturing, avoiding the use of alkalis is crucial to simplify processes and reduce costs associated with preparation and post-processing. The use and residues of volatile organic solvents (such as acetone, methanol, and butyl acetate) can pollute production sites and affect the usability of cosmetics. Therefore, in addition to meeting quality standards, cosmetics must also be produced in a green and pollution-free manner, making them environmentally friendly.

[0003] The P25 material used for the catalytic treatment of indoor pollutants (such as acetone and formaldehyde) is composed of TiO2. It exhibits excellent catalytic treatment performance under sunlight; however, due to its wide band gap, it cannot fully utilize its treatment capabilities in the visible spectrum region, and indoor natural light significantly reduces its effectiveness. One solution is to dope it with silver nanoparticles to enhance its ability to treat pollutant molecules under indoor natural light. While the use of precious metals broadens the material's spectral range, it significantly increases production costs. To broaden the spectral response range of the material, another form of TiO2, titanium black, has attracted considerable attention in recent years. Titanium black, or black TiO2, is generally produced by the thermal reduction of TiO2. Its black color is its most prominent appearance characteristic, and the introduction of oxygen vacancies on the TiO2 surface is the main reason for its black color. Surface oxygen vacancies reduce the band gap of TiO2, enhancing its absorption of visible light and photocatalytic performance, thus making it a promising catalyst that has been widely studied. However, traditional methods for preparing titanium black require calcination at 800–1000°C in reducing atmospheres such as hydrogen and ammonia, which is costly, has harsh reaction conditions, and involves hazardous gases, making the safety of the experiment unreliable and limiting the widespread application of titanium black materials to some extent. Summary of the Invention

[0004] The technical problem to be solved by this invention is to provide a titanium black material for cosmetics and indoor air pollution treatment, and its preparation method. This invention utilizes sulfur to introduce oxygen defects on the surface of TiO2, obtains precursor powder using hydrothermal technology, and then subjectes the precursor powder to closed-loop heat treatment to prepare titanium black powder with anatase crystal structure. This method is characterized by its simple process, green and safe preparation process, environmental friendliness, and low cost.

[0005] The present invention discloses a method for preparing titanium black material for cosmetics and indoor air pollution treatment, characterized in that: sulfur powder is dissolved in oleylamine to prepare a thiamine solution with a molar concentration of 0.5-1.0 mol / L, and stirred at room temperature for 10-40 minutes to ensure complete dissolution; tetrabutyl titanate with a molar amount of sulfur powder of 1 / 3 to 1 / 2 is added to the fully dissolved thiamine solution, and stirred at room temperature for 10-20 minutes to ensure thorough mixing to obtain a reaction solution; the reaction solution is then placed in a reaction vessel and subjected to hydrothermal reaction at 100-240°C for 2-24 hours in a sealed environment to obtain a precursor solution; 2-4 times the volume of anhydrous ethanol is added to the obtained precursor solution to precipitate powder, which is then dried at 50-70°C to obtain titanium black precursor powder; finally, the titanium black precursor powder is sealed and heat-treated at 200-600°C for 1-3 hours, and then naturally cooled to room temperature to obtain the titanium black material for cosmetics and indoor air pollution treatment described in the present invention.

[0006] The titanium black material for cosmetics and indoor air pollution treatment described in this invention is prepared by the above method.

[0007] Acetone is a common air pollutant from chemical production. To evaluate the effectiveness of the titanium black prepared in this invention in eliminating acetone molecules in the air, the following degradation tests were conducted:

[0008] Take 100 mg of the prepared titanium black material and spread it evenly in a 25 cm2 circular area. Place it in a sealed environment with a chamber volume of 20 L, filled with air and an acetone gas concentration of 100 ppm. First, allow the sample to undergo acetone gas degradation treatment in a dark environment for 30 minutes. Then, irradiate the sample with a white light with a power of 50 W to continue the acetone gas degradation treatment for 60 minutes. Measure the change in acetone gas concentration in the environment throughout the process.

[0009] The titanium black material prepared by this invention can effectively degrade residual organic solvents such as acetone in chemical production environments. From this perspective, this invention is crucial for exploring green production processes for cosmetics. This invention also develops a safe, energy-saving, easily controllable, and low-cost method for preparing titanium black. The prepared titanium black material can effectively remove indoor air pollutants such as acetone. Attached Figure Description

[0010] Figure 1 The XRD pattern of the titanium black material obtained after heat treatment at 400–600℃ is shown; the results are consistent with the 99-0008 standard card, indicating that the product has an anatase structure.

[0011] Figure 2 Photographs of titanium black materials obtained after heat treatment at 400–600℃ and SEM images of titanium black materials obtained after heat treatment at 500℃ are shown; the results indicate that the products are black and have micro-nano scale.

[0012] Figure 3 The infrared spectrum of the titanium black material obtained after heat treatment at 500℃ is shown. The results indicate that the sample adsorbed only a small amount of water molecules and no other molecules harmful to the skin.

[0013] Figure 4 The UV-Vis diffuse reflectance absorption spectrum of the titanium black material obtained after heat treatment at 500℃ is shown. The results indicate that it has excellent light absorption performance in the visible light region, which is beneficial for protecting the skin from UV damage.

[0014] Figure 5 The image shows (a) of the titanium black material prepared in Example 1 being treated with 100 ppm acetone molecules and (b) of the spectrum of the irradiation source used. The results show that the material has a significant visible area photocatalytic degradation function for organic molecules and air purification, which is beneficial for the use of the material in indoor natural light environments. Detailed Implementation

[0015] The present invention will be further described below with reference to examples, but the present invention is not limited to these embodiments.

[0016] Example 1

[0017] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, 1 / 2 molar amount of tetrabutyl titanate was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 180 °C for 18 hours to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60 °C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 500 °C for 2 hours to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 600 mg.

[0018] 100 mg of the titanium black material prepared in this embodiment was evenly spread on a 25 cm² surface. 2 The circular region was placed in a sealed environment with a chamber volume of 20L, filled with air and containing 100ppm acetone gas. The sample was first subjected to acetone gas degradation treatment in a dark environment for 30 minutes, followed by exposure to 50W white light (spectral density as shown in the image). Figure 5 (As shown in b) Irradiate the sample to allow it to continue degrading acetone gas for 60 minutes. Throughout the entire process before and after irradiation, the degradation rate of acetone gas by titanium black reached over 12% (degradation rate as shown in b). Figure 5 As shown in a), the degradation rate under light conditions was increased by more than 5% compared to the condition without light, thus visible light irradiation further enhanced the degradation of acetone pollutants.

[0019] Example 2

[0020] The preparation method of titanium black is the same as that in Example 1, except that the hydrothermal reaction time is changed. Here, the hydrothermal reaction time is 24 hours.

[0021] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, 1 / 2 molar amount of tetrabutyl titanate was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 180 °C for 24 h to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60 °C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 500 °C for 2 h to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 630 mg.

[0022] Example 3

[0023] The preparation method of titanium black is the same as that in Example 1, except that the temperature of the subsequent heat treatment is changed. Here, we choose a heat treatment temperature of 600°C.

[0024] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, 1 / 2 molar amount of tetrabutyl titanate was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 180°C for 18 hours to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60°C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 600°C for 2 hours to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 500 mg.

[0025] Example 4

[0026] The preparation method of titanium black is the same as that in Example 1, except that the temperature of the hydrothermal reaction is changed. Here, the temperature of the hydrothermal reaction is 200°C.

[0027] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, 1 / 2 molar amount of tetrabutyl titanate was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 200 °C for 18 hours to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60 °C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 500 °C for 2 hours to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 630 mg.

[0028] Example 5

[0029] The preparation method of titanium black is the same as that in Example 1, except that the amount of tetrabutyl titanate is changed. Here, tetrabutyl titanate with a molar amount of elemental sulfur is used, which is 1 / 3 of that used.

[0030] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, tetrabutyl titanate with a molar amount of elemental sulfur was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 180 °C for 18 hours to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60 °C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 500 °C for 2 hours to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 350 mg.

[0031] Example 6

[0032] The preparation method of titanium black is the same as that in Example 1, except that the temperature of the subsequent heat treatment is changed. Here, we choose a heat treatment temperature of 400℃.

[0033] 700 mg of elemental sulfur was dissolved in 30 mL of oleylamine solution at room temperature and stirred for 30 minutes at room temperature to ensure complete dissolution of the sulfur. Then, 1 / 2 molar amount of tetrabutyl titanate was added and stirred for 20 minutes at room temperature to ensure uniform dispersion. The reaction solution was then placed in a sealed reactor and subjected to hydrothermal reaction at 180 °C for 18 hours to obtain a precursor solution. Three times the volume of anhydrous ethanol was added to the precursor solution to precipitate a powder, which was then dried at 60 °C to obtain titanium black precursor powder. The titanium black precursor powder was sealed and subjected to high-temperature heat treatment at 400 °C for 2 hours to obtain titanium black material for cosmetics and indoor air pollution treatment, with a product mass of approximately 650 mg.

[0034] Examples 2-6 illustrate the implementation and effects of titanium black in removing acetone pollutants from the air as follows:

[0035] 100 mg of the titanium black material prepared in Examples 2-6 was evenly spread on a 25 cm² surface. 2 The circular region was placed in a sealed environment with a chamber volume of 20L, filled with air and containing 100ppm acetone gas. The sample was first subjected to acetone gas degradation treatment in a dark environment for 30 minutes, followed by exposure to 50W white light (spectral density as shown in the image). Figure 5 (b) The sample was irradiated to continue degrading acetone gas for 60 minutes. Throughout the process before and after irradiation, the degradation rate of acetone gas by titanium black was over 10%. The degradation rate under irradiation was significantly higher than that under no-light conditions, indicating that visible light irradiation accelerated the removal of acetone pollutants.

Claims

1. A method for preparing titanium black material for cosmetics and indoor air pollution treatment, characterized in that: Sulfur powder is dissolved in oleylamine to prepare a thiamine solution, and stirred at room temperature until fully dissolved. Tetrabutyl titanate (1 / 3 to 1 / 2 the molar amount of sulfur powder) is added to the fully dissolved thiamine solution, and stirred at room temperature to obtain a reaction solution. This reaction solution is then placed in a reaction vessel and subjected to a hydrothermal reaction at 100–240°C for 2–24 hours in a sealed environment to obtain a precursor solution. Anhydrous ethanol is added to the precursor solution to precipitate a powder, which is then dried at 50–70°C to obtain titanium black precursor powder. The precursor powder is then subjected to high-temperature heat treatment at 200–600°C for 1–3 hours, followed by natural cooling to room temperature to obtain titanium black material for cosmetics and indoor air pollution treatment.

2. The method for preparing titanium black material for cosmetics and indoor air pollution treatment as described in claim 1, characterized in that: Sulfur powder is dissolved in oleylamine to prepare a thioamine solution with a molar concentration of 0.5~1.0 mol / L.

3. The method for preparing titanium black material for cosmetics and indoor air pollution treatment as described in claim 1, characterized in that: The powder is precipitated by adding 2 to 4 times the volume of anhydrous ethanol to the precursor solution.

4. A titanium black material for use in cosmetics and indoor air pollution treatment, characterized in that: It is prepared by the method described in any one of claims 1 to 3.

Images