CN113336265A - Preparation method of black titanium dioxide B nanosheet with high-content oxygen vacancy defects - Google Patents
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Abstract
The invention discloses a preparation method of a black titanium dioxide B nanosheet with high-content oxygen vacancy defects, which comprises the steps of mixing and stirring a certain amount of ethylene glycol as a solvent and a titanium tetrachloride hydrochloric acid solution as a titanium source until the solution turns brown; putting the brown solution into a reaction kettle, standing for 4-6 hours in a constant temperature box at the temperature of 150-; annealing the obtained white powder at the temperature of 250-350 ℃ in an inert gas for 2-3 hours to obtain a black titanium dioxide B nano sheet, and degrading the organic dye by using the black titanium dioxide B nano sheet. The black titanium dioxide nanosheet aggregate prepared by the method disclosed by the invention is uniform in particle size of 150-200nm, the thickness of the epitaxial wafer is 1-2nm, the high-content oxygen vacancy defect is obtained only through thermal decomposition of the ethylene glycol molecule chemically adsorbed on the surface of the material, the method is mild and simple, and high temperature and high pressure and additional reducing agents are not needed.
Description
Technical Field
The invention relates to a preparation method of a black titanium dioxide B nanosheet with a high content of oxygen vacancy defects, and belongs to the technical field of material synthesis.
Background
The introduction of oxygen vacancies in reduced form, changing the color of titanium dioxide, narrowing the band gap and enhancing its light absorption, is considered to be an effective means of improving the properties of titanium dioxide, and the appearance of black titanium dioxide in particular has given titanium dioxide more research and practical value (Science,2011,331,746). The black titanium dioxide has the characteristics of uniform surface amorphization, wide light absorption range, more chemical defects and enhanced electron conductivity, and is beneficial to enhancing the application of the black titanium dioxide in photocatalysis, energy storage, conversion and the like. However, some existing methods for introducing oxygen vacancies require a high temperature or high pressure environment, and some methods require additional addition of a high-risk reducing agent, so a mild and simple method is needed.
Unlike other crystal forms of titanium dioxide (anatase, rutile, brookite), titanium dioxide B is a new crystal form discovered only in 1980s, which is metastable and can be converted to anatase under milder conditions. And thus frequently appear in the form of a complex with anatase in terms of photocatalysis (adv. energy mater.2015,5,1401756; Scientific reports2017,7: 14594). The titanium dioxide B nanosheet has the advantages of higher specific surface area due to the fact that the titanium dioxide B nanosheet has an open cavity and parallel channels, more active sites can be exposed, charge fluidity is improved, reusability is high, and the like, so that attention is paid to the titanium dioxide B nanosheet, but the application of the titanium dioxide B nanosheet is limited due to the fact that the titanium dioxide B nanosheet is wider in band gap and low in light utilization rate.
Patent CN106076302A discloses a preparation method of a nanometer black titanium dioxide photocatalyst, which comprises the specific operation steps of adding 2-10g of trivalent titanium source which is titanium trichloride or TiOCl and 0-1g of reducing agent which is sodium borohydride, ascorbic acid or hydrazine hydrate into 20-100ml of deionized water, continuously stirring for 1-3 hours to obtain purple transparent solution, adding 0.2-1.5mol of sodium hydroxide solution into the solution until the pH value is 2-10, continuously stirring for 2-3 hours to obtain black titanium dioxide solution, transferring the black titanium dioxide solution into a 100ml hydrothermal reaction kettle, and reacting for 4-20 hours at 80-260 ℃ to obtain nanometer black titanium dioxide. And respectively washing with deionized water and ethanol until the pH value is 7, and drying to obtain the nano black titanium dioxide powder photocatalyst. The patent not only adopts high-risk strong reducing agents such as sodium borohydride and hydrazine hydrate, but also utilizes strong alkali sodium hydroxide solution, and the pH value needs to be adjusted repeatedly.
Patent CN103214032A discloses a method for preparing black titanium dioxide by hydrogen plasma assistance, which comprises the specific steps of placing titanium dioxide in a closed system, vacuumizing to make the pressure of the closed system less than 30Pa, introducing a mixed atmosphere of hydrogen and hydrogen into the closed system, heating the titanium dioxide, adjusting the flow rate of the mixed atmosphere to make the pressure in the closed system 500Pa, turning on a radio frequency power supply to generate active hydrogen plasma, and treating the titanium dioxide for a specified time, wherein the radio frequency power supply is utilized to ionize hydrogen molecules to generate the active hydrogen plasma for reducing the titanium dioxide to obtain black titanium dioxide. The patent adopts vacuum and high-pressure environment and dangerous gas hydrogen to obtain black titanium dioxide nano particles.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of black titanium dioxide B nanosheets with high oxygen vacancy content, compared with the prior high-temperature or high-pressure hydrogenation reduction and addition of strong reducing reagents, the preparation method of black titanium dioxide has mild conditions, no additional reducing reagent is added, the specific surface area of nanosheets is large, the oxygen vacancy content is high, and the application range of the black titanium dioxide B nanosheets is expanded.
The technical scheme of the invention is as follows:
a process for the preparation and use of black titanium dioxide B having a high content of oxygen vacancy defects, comprising the steps of:
(1) taking a certain amount of ethylene glycol in a beaker, taking a certain amount of TiCl4Dissolving into hydrochloric acid solution with certain concentration to form TiCl with certain percentage4A hydrochloric acid solution. Then, 2ml of TiCl were added4The hydrochloric acid solution was dropped into 20mL of ethylene glycol, and the mixture was stirred at room temperature until the mixture became pale yellow, and the stirring was continued until the solution became pale brown.
(2) And transferring the obtained light brown solution into a 50ml reaction kettle, heating in a constant temperature box, and standing for a certain time under the condition of heat preservation to obtain white titanium dioxide B nanosheet precipitate.
(3) And centrifuging the white precipitate, washing, drying, grinding, placing in a porcelain ark, putting in a tube furnace, and annealing in an inert gas atmosphere to obtain a black titanium dioxide B nanosheet, which is marked as B-TiO 2-B.
(4) And respectively carrying out degradation experiments on the rhodamine B (RhB) aqueous solution by using black titanium dioxide B in the absence of light and under simulated solar light.
The content of the ethylene glycol is 20-30ml, the content of the hydrochloric acid in the hydrochloric acid solution is 28-32%, and TiCl is added4TiCl in hydrochloric acid solution4The content of (A) is 14-16%.
The temperature of the constant temperature box is 150-180 ℃, and the standing time is 4-6 hours.
The washing solution is ethanol, and the drying temperature and time are 30-50 ℃ and 10-12 hours.
The inert gas is nitrogen or argon, and the annealing temperature is 250-350 ℃.
The obtained white titanium dioxide B powder is a nanosheet aggregate, the particle size is 150-200nm, and the thickness of the epitaxial wafer is 2-3 nm.
The black titanium dioxide B is a nano-sheet aggregate with the particle size of 150-200nm and the thickness of the epitaxial wafer of 1-2 nm.
The simulated solar energy is 1.5G, the concentration of the rhodamine B aqueous solution is 30-40mg/L, and the concentration of the black titanium dioxide B nanosheet is 1-1.5mg per 1-1.5ml of the rhodamine B aqueous solution.
The invention has the following advantages:
1. the solvent glycol in the synthesis reaction can be used as a nanosheet structure directing agent, can play a role in reduction in the annealing process, and is a main reason for generating oxygen vacancy defects. No additional reducing agent is required.
2. The temperature for obtaining black titanium dioxide is up to 350 deg.c, which is much lower than the temperature required by other synthesis methods.
3. The prepared black titanium dioxide has uniform granularity, the thickness of the epitaxial slice is only 1-2nm, more oxygen vacancy defects are exposed, the specific surface area is improved, more active sites are provided, and the photocatalysis effect is enhanced.
Drawings
Fig. 1 is SEM image and color photograph of brown titanium dioxide nanosheet prepared in example 1 of the present invention.
Fig. 2 is TEM and XRD patterns of black titanium dioxide nanosheets prepared in example 2 of the present invention.
Fig. 3 is a graph of the effect of applying the black titanium dioxide nanosheet prepared in embodiment 2 of the present invention to photodegradation RhB.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but do not limit it in any way:
example 1
2ml of titanium tetrachloride hydrochloric acid solution was added to 20ml of ethylene glycol and stirred uniformly until the solution was light brown in color. Transferring the obtained light brown solution to a 50ml reaction kettle, placing the reaction kettle in a constant temperature box at 150 ℃, preserving heat, standing for 4 hours, and cooling to obtain white precipitate. Centrifuging, washing with ethanol, drying at 30 ℃ for 10 hours, grinding, putting into a porcelain ark, moving to a tube furnace, and annealing at 250 ℃ for 2 hours under the protection of nitrogen to obtain a brown titanium dioxide B nanosheet sample.
Example 2
2ml of titanium tetrachloride hydrochloric acid solution was added to 20ml of ethylene glycol and stirred uniformly until the solution was light brown in color. Transferring the obtained light brown solution to a 50ml reaction kettle, placing the reaction kettle in a constant temperature box at 150 ℃, preserving heat, standing for 4 hours, and cooling to obtain white precipitate. Centrifuging, washing with ethanol, drying at 30 ℃ for 10 hours, grinding, putting into a porcelain ark, moving to a tube furnace, and annealing at 350 ℃ for 2 hours under the protection of nitrogen to obtain a black titanium dioxide B nanosheet sample. And (3) placing 20mg of black sample in 20ml of 40mg/L RhB solution, carrying out dark reaction for 30min, then leaving supernatant to be tested, and then leaving supernatant to be tested under simulated sunlight for 5min, 15min, 25min and 35 min.
Claims (8)
1. A preparation method of a black titanium dioxide B nanosheet with high-content oxygen vacancy defects is characterized by comprising the following steps:
(1) taking a certain amount of ethylene glycol in a beaker, taking a certain amount of TiCl4Dissolving into hydrochloric acid solution with certain concentration to form TiCl with certain percentage4A hydrochloric acid solution. Then, 2ml of TiCl were added4The hydrochloric acid solution was dropped into 20mL of ethylene glycol, and the mixture was stirred at room temperature until the mixture became pale yellow, and the stirring was continued until the solution became pale brown.
(2) And transferring the obtained light brown solution into a 50ml reaction kettle, placing the reaction kettle in a constant temperature box, preserving heat and standing for a certain time to obtain white titanium dioxide B nanosheet precipitate.
(3) Centrifuging the white precipitate, washing, drying, grinding, placing in a porcelain ark, placing in a tube furnace, annealing in an inert gas atmosphere to obtain black titanium dioxide B nanosheet, marked as B-TiO2-B。
(4) And respectively carrying out degradation experiments on the rhodamine B (RhB) aqueous solution by using black titanium dioxide B in the absence of light and under simulated solar light.
2. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the content of ethylene glycol is 20-30ml, the content of hydrochloric acid solution is 28-32%, and TiCl is added4TiCl in hydrochloric acid solution4The content of (A) is 14-16%.
3. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the temperature of the incubator is 150-.
4. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the washing solution is ethanol, and the drying temperature and time are 30-50 ℃ and 10-12 hours.
5. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the inert gas is nitrogen or argon, and the annealing temperature is 250-350 ℃.
6. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the obtained white titanium dioxide B powder is a nanosheet aggregate, the particle size is 150-200nm, and the thickness of the epitaxial wafer is 2-3 nm.
7. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the black titanium dioxide B is in the shape of a nanosheet aggregate, the particle size is 150-200nm, and the thickness of the epitaxial wafer is 1-2 nm.
8. The black titanium dioxide B nanosheet with the high content of oxygen vacancy defects as well as the preparation method and the application thereof as claimed in claim 1, wherein the simulated solar light energy is 1.5G, the concentration of the rhodamine B aqueous solution is 30-40mg/L, and the concentration of the black titanium dioxide B nanosheet is 1-1.5mg per 1-1.5ml of the rhodamine B aqueous solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349037A (en) * | 2022-01-02 | 2022-04-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
| CN114570346A (en) * | 2022-02-22 | 2022-06-03 | 华东理工大学 | Modification method for enhancing visible light response of titanium dioxide photocatalyst |
| CN114714457A (en) * | 2022-03-04 | 2022-07-08 | 哈尔滨工业大学（深圳） | Preparation method of modified natural wood material and application of modified natural wood material in sewage purification |
| CN114873631A (en) * | 2022-05-05 | 2022-08-09 | 长春工程学院 | Preparation method of black ZnO |
| CN115739068A (en) * | 2022-11-18 | 2023-03-07 | 南京大学盐城环保技术与工程研究院 | Supported catalyst, preparation method thereof and photocatalytic treatment device using supported catalyst |
| CN117899864A (en) * | 2024-03-15 | 2024-04-19 | 四川大学 | Method for preparing copper-loaded black titanium dioxide at room temperature and copper-loaded black titanium dioxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349037A (en) * | 2022-01-02 | 2022-04-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
| CN114349037B (en) * | 2022-01-02 | 2023-09-15 | 广西师范大学 | Preparation method and application of black calcium carbonate |
| CN114570346A (en) * | 2022-02-22 | 2022-06-03 | 华东理工大学 | Modification method for enhancing visible light response of titanium dioxide photocatalyst |
| CN114570346B (en) * | 2022-02-22 | 2023-11-10 | 华东理工大学 | Modification method for enhancing visible light response of titanium dioxide photocatalyst |
| CN114714457A (en) * | 2022-03-04 | 2022-07-08 | 哈尔滨工业大学（深圳） | Preparation method of modified natural wood material and application of modified natural wood material in sewage purification |
| CN114873631A (en) * | 2022-05-05 | 2022-08-09 | 长春工程学院 | Preparation method of black ZnO |
| CN115739068A (en) * | 2022-11-18 | 2023-03-07 | 南京大学盐城环保技术与工程研究院 | Supported catalyst, preparation method thereof and photocatalytic treatment device using supported catalyst |
| CN117899864A (en) * | 2024-03-15 | 2024-04-19 | 四川大学 | Method for preparing copper-loaded black titanium dioxide at room temperature and copper-loaded black titanium dioxide |
| CN117899864B (en) * | 2024-03-15 | 2024-06-07 | 四川大学 | Method for preparing copper-loaded black titanium dioxide at room temperature and copper-loaded black titanium dioxide |
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