CN116081684A - Main exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies, preparation method and application thereof - Google Patents
Main exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies, preparation method and application thereof Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 75
- 239000000463 material Substances 0.000 title claims abstract description 69
- 239000013078 crystal Substances 0.000 title claims abstract description 66
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 56
- 239000001301 oxygen Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 20
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 20
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 229940124530 sulfonamide Drugs 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 13
- 229940043267 rhodamine b Drugs 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 9
- 230000015556 catabolic process Effects 0.000 claims description 8
- 238000006731 degradation reaction Methods 0.000 claims description 8
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 150000003456 sulfonamides Chemical class 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
The invention relates to the technical field of photocatalytic materials, in particular to a titanium dioxide material with a main exposure {101} crystal face of oxygen-enriched vacancy, a preparation method and application thereof. Finally, placing the titanium dioxide in an aqueous solution of polyvinylpyrrolidone (PVP) for water bath heating for a plurality of hours, and obtaining the oxygen-enriched vacancy-main exposure {101} crystal face titanium dioxide. The invention has low raw material cost, simple process and easy popularization. The prepared oxygen-enriched vacancy-main exposure {101} crystal face titanium dioxide has more excellent photocatalysis performance than pure titanium dioxide material.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a main exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies, a preparation method and application thereof.
Background
Along with the acceleration of industrialization and urban processes, the world faces the challenges of water resource shortage and serious pollution, and water pollution treatment has become an important problem of current environmental protection treatment. The traditional sewage treatment has low efficiency and high cost, so that the sewage treatment is limited to a certain extent.
The photocatalytic oxidation technology can directly utilize solar energy to remove various environmental pollutants in water under mild conditions, and has the advantages of low consumption, environmental protection, convenience and the like. As a key element of the technology, the property of the catalyst material directly affects the separation efficiency of the photo-generated carriers, and determines the removal capability of pollutants. Titanium dioxide is still one of the photocatalytic materials with the largest industrial application prospect at present due to the consideration of various factors such as comprehensive catalytic activity, production cost, environmental safety influence, environmental stability and the like. However, the difficulty in utilizing visible light and the low efficiency of photogenerated charge separation have always prevented their development.
The exposed crystal face and defect state of the photocatalyst are critical to the photocatalytic performance, and the vacancies of different crystal faces have different coordination unsaturated bonds, so that the microstructure of the material can be effectively adjusted, and the photocatalytic performance of the material is further influenced.
In view of the above drawbacks, the present inventors have finally achieved the present invention through long-time studies and practices.
Disclosure of Invention
The invention aims to solve the problems that the existing titanium dioxide material is difficult to utilize visible light and has low photo-generated charge separation efficiency, and provides a main exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies, a preparation method and application thereof.
In order to achieve the above purpose, the invention discloses a preparation method of a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancy, which comprises the following steps:
s1, uniformly stirring tetrabutyl titanate, deionized water and absolute ethyl alcohol for reaction;
s2, after the reaction in the step S1 is finished, cooling to room temperature, collecting a white product, washing with deionized water and absolute ethyl alcohol, drying and grinding to obtain a titanium dioxide material with a main exposed {101} crystal face;
and S3, dispersing the titanium dioxide material with the main exposure {101} crystal face obtained in the step S3 in a polyvinylpyrrolidone solution, stirring for reaction, centrifuging after the reaction is finished, washing the obtained solid by using deionized water and absolute ethyl alcohol, removing redundant polyvinylpyrrolidone molecules, drying and grinding to obtain the titanium dioxide material with the main exposure {101} crystal face with oxygen-enriched vacancies.
In the step S1, the volume ratio of tetrabutyl titanate, deionized water and absolute ethyl alcohol is 1:1:3, and the stirring time is 1h.
The reaction temperature in the step S1 is 180 ℃ and the reaction time is 6 hours.
The drying temperature in the step S2 is 60 ℃.
The amount of the titanium dioxide material with the {101} crystal face mainly exposed in the step S3 is 0.25g, the concentration of the polyvinylpyrrolidone solution is 10g/L, and the amount is 100mL.
The preparation process of the polyvinylpyrrolidone solution is as follows: 1g of polyvinylpyrrolidone was weighed out and dissolved in 100mL of deionized water.
The reaction temperature of the stirring reaction in the step S3 is 90 ℃ and the time is 4 hours.
The drying temperature in the step S3 is 60 ℃.
Titanium dioxide has the problems of narrow light absorption range, lower quantum efficiency and short service life of photo-generated carriers when used as a photocatalyst. According to the invention, oxygen vacancies are introduced into the titanium dioxide with the {101} crystal face mainly exposed, the energy band structure is regulated by using the oxygen vacancies, the charge separation is promoted, the oxygen molecules are activated, the effect of the crystal face effect reduces the thermodynamic energy barrier of active oxygen generation and conversion, and the photocatalytic performance is improved.
The invention also discloses a main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancies prepared by the preparation method and application of the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancies in rhodamine B or sulfanilamide degradation.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method comprises the steps of preparing a titanium dioxide material with a main exposure {101} crystal face by adopting a hydrothermal growth method, and then introducing oxygen vacancies on the titanium dioxide with the main exposure {101} crystal face by adopting a PVP hydrothermal reduction method, so that the whole process is simple in process, easy to operate, high in repeatability, good in stability of the prepared material, stable in physical and chemical states, and has reference significance for preparation of other photocatalysts, crystal face engineering and defect engineering modification;
2. according to the invention, the preparation material is used for degrading rhodamine B and sulfanilamide, so that the obtained main-exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies has excellent photocatalysis performance.
Drawings
FIG. 1 is a flow chart of a simplified apparatus for preparing a material according to an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies prepared in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of a main exposed {101} crystal face titanium dioxide material of oxygen-enriched vacancies prepared in example 1 of the present invention;
FIG. 4 is a photo-catalytic degradation graph of rhodamine B by the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancies prepared in the example 1 and the comparative examples 1, 2, 3, 4 and 5;
FIG. 5 is a photo-catalytic degradation graph of the main exposed {101} crystal face titanium dioxide material of oxygen-enriched vacancies and commercial titanium dioxide P25 versus rhodamine B prepared in example 1 of the present invention;
FIG. 6 is a photo-catalytic degradation pattern of the main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies and commercial titanium dioxide P25 vs. sulfonamide prepared in example 1 of the present invention.
Detailed Description
The above and further technical features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Example 1
A preparation method of a main exposure {101} crystal face titanium dioxide material capable of improving the photocatalytic activity of titanium dioxide and rich in oxygen vacancies comprises the following steps:
(A) To a clean and dry beaker (50 ml) was added 5ml tetrabutyl titanate, 5ml deionized water, 15ml absolute ethanol and magnetically stirred for 1h.
(B) Transferring the white slurry uniformly stirred in the step (A) into a clean and dry 50ml Teflon high-temperature high-pressure reaction kettle, and reacting for 6 hours at 180 ℃ in a blast oven; after the reaction is finished and cooled to room temperature, the white product is collected, washed by deionized water and absolute ethyl alcohol for several times, dried for 12 hours at 60 ℃, and ground to obtain the titanium dioxide material with the main exposed {101} crystal face.
(C) 1g of polyvinylpyrrolidone (PVP) was dissolved in 100ml of water and poured into a 150ml beaker and heated to 90℃in a thermostatic water bath.
(D) Dispersing 0.25g of titanium dioxide with a main exposed {101} crystal face in the PVP solution prepared in the step (C), and magnetically stirring for 4 hours under the condition of a constant-temperature water bath at 90 ℃; and (3) immediately centrifuging after the reaction is finished, washing the obtained solid with deionized water and absolute ethyl alcohol once, removing redundant PVP molecules, drying at 60 ℃ for 12 hours, and grinding to obtain the main exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies.
In the invention, the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancy comprises two parts of main exposure {101} crystal face titanium dioxide prepared by a hydrothermal method and PVP hydrothermal reduction treatment for introducing the oxygen vacancy.
Comparative example 1
Preparing a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies: the preparation method is the same as that of the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy in example 1, except that the constant-temperature water bath time at 90 ℃ in the step (D) is 1h.
Comparative example 2
Preparing a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies: the preparation method is the same as that of the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy in example 1, except that the constant-temperature water bath time at 90 ℃ in the step (D) is 2h.
Comparative example 3
Preparing a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies: the preparation method is the same as that of the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy in example 1, except that the constant-temperature water bath time at 90 ℃ in the step (D) is 3h.
Comparative example 4
Preparing a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies: the preparation method is the same as that of the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy in example 1, except that the constant-temperature water bath time at 90 ℃ in the step (D) is 5h.
Comparative example 5
Preparing a main exposure {101} crystal face titanium dioxide material of oxygen-enriched vacancies: the preparation method is the same as that of the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy in example 1, except that the constant-temperature water bath time at 90 ℃ in the step (D) is 6h. FIGS. 2 and 3 are scanning electron micrographs and transmission electron micrographs of a titanium dioxide material with a main exposed {101} crystal face of oxygen-enriched vacancies prepared in example 1, and it can be seen that the titanium dioxide has an octahedral structure with a size of about 7 nm.
1. Degradation of rhodamine B solution
The photocatalytic reaction was carried out under a 300w xenon lamp light source at a reaction temperature of 25 ℃. In the photocatalytic experiments, a quartz reactor containing 100ml of rhodamine B solution (10 mg/L) was charged with 0.05g of the prepared main exposed {101} crystal face titanium dioxide material having oxygen-enriched vacancies. Before irradiation, the suspension was magnetically stirred in the dark for 30min to allow the catalyst and rhodamine B to reach adsorption-desorption equilibrium, and then exposed to a light source, and the magnetic stirring was used to initiate the reaction. About 3mL of the suspension was extracted every 5min with a syringe, and the catalyst powder was completely removed by passing through a 0.22 μm polytetrafluoroethylene syringe filter. The concentration of rhodamine B solution was analyzed by ultraviolet-visible spectrum (characteristic absorption peak of rhodamine B at λ=554 nm) to obtain a photocatalytic degradation curve of rhodamine B solution reacting for 0.5h, and the test materials include commercial titanium dioxide P25, and materials prepared in example 1 and comparative examples 1, 2, 3, 4, and 5. As can be seen from fig. 4, the photocatalytic activity of the rhodamine B degraded by the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy increases with the increase of the hydrothermal treatment time of the PVP, and the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy treated by the PVP for 4 hours has the best photocatalytic performance in the examples. As can be seen from fig. 5: the degradation rate of the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancy to rhodamine B reaches 95.2% in 30min, and the pure {101} titanium dioxide and commercial titanium dioxide P25 only reach 56.3% and 30.1% respectively.
2. Degradation of sulfonamides
The photocatalytic reaction was carried out under a 300w xenon lamp light source at a reaction temperature of 25 ℃. In the photocatalytic experiments, 0.05g of the prepared oxygen-enriched vacancy-rich mainly exposed {101} crystal face titanium dioxide material was charged into a quartz reactor containing 100mL of a sulfanilamide solution (10 mg/L). Before irradiation, the suspension is magnetically stirred for 30min in the dark to make the catalyst and the sulfanilamide reach adsorption-desorption equilibrium, and then the catalyst and the sulfanilamide are exposed to a light source, and the reaction is started by magnetic stirring. About 3ml of the suspension was extracted every 5min with a syringe, and the catalyst powder was completely removed by passing through a 0.22 μm polytetrafluoroethylene syringe filter. The concentration of the sulfonamide solution was analyzed by uv-vis spectrum (characteristic absorption peak of sulfonamide at λ=260 nm) to obtain a photocatalytic degradation curve of the sulfonamide solution reaction for 2h, see fig. 6. As can be seen from fig. 6: the degradation rate of the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancy to the sulfanilamide reaches 80.4% in 60min, the degradation rate of the main exposure {101} crystal face titanium dioxide material of the oxygen-enriched vacancy to the sulfanilamide reaches 95.4% in 120min, the degradation rate of the {101} crystal face titanium dioxide material of the oxygen-enriched vacancy to the sulfanilamide reaches about 80.0% in 100min, and the commercial titanium dioxide P25 is only degraded by 41.0% in 120 min.
The foregoing description of the preferred embodiment of the invention is merely illustrative of the invention and is not intended to be limiting. It will be appreciated by persons skilled in the art that many variations, modifications, and even equivalents may be made thereto without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The preparation method of the titanium dioxide material with the main exposure {101} crystal face of oxygen-enriched vacancies is characterized by comprising the following steps:
s1, uniformly stirring tetrabutyl titanate, deionized water and absolute ethyl alcohol for reaction;
s2, after the reaction in the step S1 is finished, cooling to room temperature, collecting a white product, washing with deionized water and absolute ethyl alcohol, drying and grinding to obtain a titanium dioxide material with a main exposed {101} crystal face;
and S3, dispersing the titanium dioxide material with the main exposure {101} crystal face obtained in the step S3 in a polyvinylpyrrolidone solution, stirring for reaction, centrifuging after the reaction is finished, washing the obtained solid by using deionized water and absolute ethyl alcohol, removing redundant polyvinylpyrrolidone molecules, drying and grinding to obtain the titanium dioxide material with the main exposure {101} crystal face with oxygen-enriched vacancies.
2. The method for preparing the titanium dioxide material with the main exposed {101} crystal face of the oxygen-enriched vacancy as claimed in claim 1, wherein the volume ratio of tetrabutyl titanate, deionized water and absolute ethyl alcohol in the step S1 is 1:1:3, and the stirring time is 1h.
3. The method for preparing a main-exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies according to claim 1, wherein the reaction temperature in the step S1 is 180 ℃ and the reaction time is 6h.
4. The method for preparing a main exposed {101} crystal face titanium dioxide material having oxygen-enriched vacancies as claimed in claim 1, wherein the drying temperature in the step S2 is 60 ℃.
5. The method for preparing a titanium dioxide material with a main exposed {101} crystal face of oxygen-enriched vacancy as claimed in claim 1, wherein the amount of the titanium dioxide material with a main exposed {101} crystal face in the step S3 is 0.25g, the concentration of the polyvinylpyrrolidone solution is 10g/L, and the amount is 100mL.
6. The method for preparing the titanium dioxide material with the main exposed {101} crystal face of oxygen-enriched vacancy as claimed in claim 5, wherein the preparation process of the polyvinylpyrrolidone solution is as follows: 1g of polyvinylpyrrolidone was weighed out and dissolved in 100mL of deionized water.
7. The method for preparing a main-exposure {101} crystal face titanium dioxide material with oxygen-enriched vacancies according to claim 1, wherein the reaction temperature of the stirring reaction in the step S3 is 90 ℃ and the time is 4 hours.
8. The method for preparing a main exposed {101} crystal face titanium dioxide material having oxygen-enriched vacancies as claimed in claim 1, wherein the drying temperature in the step S3 is 60 ℃.
9. A predominantly exposed {101} crystal face titanium dioxide material having oxygen-enriched vacancies produced by the production method according to any one of claims 1 to 8.
10. Use of the oxygen-enriched vacancy-main-exposure {101} crystal face titanium dioxide material as claimed in claim 9 in rhodamine B or sulfanilamide degradation.
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