CN117380218A - Preparation method of carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material - Google Patents
Preparation method of carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material Download PDFInfo
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- CN117380218A CN117380218A CN202210758971.7A CN202210758971A CN117380218A CN 117380218 A CN117380218 A CN 117380218A CN 202210758971 A CN202210758971 A CN 202210758971A CN 117380218 A CN117380218 A CN 117380218A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 40
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002135 nanosheet Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 32
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 13
- -1 functional group organic compound Chemical class 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 13
- 150000003608 titanium Chemical class 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 239000007853 buffer solution Substances 0.000 claims abstract description 9
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000012467 final product Substances 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000004098 Tetracycline Substances 0.000 claims abstract description 8
- 229960002180 tetracycline Drugs 0.000 claims abstract description 8
- 229930101283 tetracycline Natural products 0.000 claims abstract description 8
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 8
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 8
- 230000015556 catabolic process Effects 0.000 claims abstract description 6
- 238000006731 degradation reaction Methods 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 4
- 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 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material. Adding organic titanium salt and sulfur-containing functional group organic compound into a mixed solution of ethylene glycol and deionized water, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, and performing ultrasonic dispersion to obtain a solution A; transferring the solution A into a reaction kettle, naturally cooling the heated solution to room temperature, and filtering, washing and drying to obtain a solution B; dispersing the B into a buffer solution for ultrasonic dispersion, adding dopamine hydrochloride into a suspension for magnetically stirring precipitate centrifugation, and drying the obtained product in a vacuum oven to obtain C; and C is placed in an argon mixed atmosphere containing hydrogen for heating and calcining, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained. In the dark, firstly, the carbon skeleton supports the ultrathin titanium disulfide nanosheet photocatalytic material to balance the adsorption of the tetracycline, and then under the ultraviolet light catalytic condition, the degradation of the tetracycline reaches 99.3% after 60 min.
Description
Technical Field
The invention relates to a photocatalytic material, in particular to a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material.
Background
With the development of the chemical industry, environmental pollution is increasingly serious. The discharge of printing and dyeing wastewater is one of the important causes of water pollution. There is a large amount of commercial dye emissions each year, and the dyes are stable in chemical property and cause great harm to the ecological environment. The characteristic that the semiconductor oxide material can be stimulated and activated under the irradiation of sunlight is utilized, so that organic matters can be effectively oxidized and degraded into small molecules such as carbon dioxide, water and the like. Compared with the traditional purification method, the semiconductor photocatalysis technology has the advantages of mild reaction condition, no secondary pollution, simple operation, obvious degradation effect and the like. Titanium dioxide is one of the photocatalysts of great interest, which is low-toxic, low-cost, durable, super-hydrophilic and has excellent photochemical stability.
Transition metal dichalcogenides are an important class of materials that have received attention due to their abundant physical and chemical properties. In particular MoS 2 、WS 2 And WSe 2 As a typical transition metal dichalcogenide, a phenomenon which is abundant in the fields of optoelectronics, energy valley electronics, and spintronics has been stimulated to widely study the hot spot. Recent studies have shown that titanium disulfide in transition metal dichalcogenides is nanoelectronicApplications in optics, photonics, sensors, energy storage system electrodes, etc. have attracted considerable attention. Can be used in the field of photocatalysis.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material.
Still another object of the present invention is a product obtained by the above process.
A further object of the invention is the use of the above-mentioned product.
The invention discloses a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material, which comprises the following specific steps:
the first step: adding 0.02-0.04 mmol of organic titanium salt and 0.04-0.08 mmol of sulfur-containing functional group organic compound into a mixed solution of 80 mL glycol and deionized water (wherein the volume ratio of the organic titanium salt to the sulfur-containing functional group organic compound is 1-2:1), magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 20-30 min to uniformly disperse the mixture, and fully mixing the solution, and marking the mixture as a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 200-240 ℃ to react for 20-30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3-5 times, and drying in a vacuum drying oven at 100-120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion, adding 40-60 mg dopamine hydrochloride into the suspension, magnetically stirring for 20-30 h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 60-80 ℃ to obtain C;
fourth step: and C is placed in an argon gas mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 500-600 ℃ at a heating and cooling rate of 1-2 ℃/min, and kept at a temperature of 2-4 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
The invention provides a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material, which has a larger specific surface area and plays an important role in improving the photocatalytic performance of the material. Is beneficial to improving the photocatalysis performance of the material. The preparation process is relatively simple and easy to operate.
The organic titanium salt is one or a combination of tetrabutyl titanate, isopropyl titanate or ethyl titanate.
The sulfur-containing functional group is one or a combination of thiourea, mercaptan and sulfur-containing amino acid.
The invention provides a product obtained by the method.
The invention also provides application of the product in tetracycline catalytic degradation.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material, which has a larger specific surface area and plays an important role in improving the photocatalytic performance of the material. Is beneficial to improving the photocatalysis performance of the material. The preparation process is relatively simple and easy to operate. In the dark, firstly, the carbon skeleton supports the ultrathin titanium disulfide nanosheet photocatalytic material to balance the adsorption of the tetracycline, and then under the ultraviolet light catalytic condition, the degradation of the tetracycline reaches 99.3% after 60 min.
Drawings
FIG. 1 is a graph showing the photocatalytic performance of the ultrathin titanium disulfide nanosheet photocatalytic material supported by a carbon skeleton in example 1.
Detailed Description
The present invention will be described in detail by way of the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
The carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is prepared by the following steps:
the first step: adding 0.02 mmol of organic titanium salt tetrabutyl titanate and 0.04mmol of sulfur-containing functional group organic compound l thiourea into a mixed solution of 80 mL glycol and deionized water, wherein the volume ratio of the tetrabutyl titanate to the thiourea is 1:1, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 20 min to uniformly disperse the hollow tube carbon skeleton, and fully mixing the solution, and marking the mixture as a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 200 ℃ to react for 30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3-5 times, and drying in a vacuum drying oven at 100 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 40 mg dopamine hydrochloride into the suspension, magnetically stirring for 20 hours, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon gas mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 500 ℃ at a heating rate of 2 ℃/min, and kept at a temperature of 4 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
FIG. 1 is a graph showing the photocatalytic performance of a carbon skeleton-supported ultrathin titanium disulfide nanosheet photocatalytic material, wherein in the dark, the carbon skeleton-supported ultrathin titanium disulfide nanosheet photocatalytic material is balanced in adsorption of tetracycline, and then the degradation of the tetracycline reaches 99.3% after 60 min under the ultraviolet light catalytic condition.
Example 2
The carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is prepared by the following steps:
the first step: adding 0.02 mmol of organic titanium salt ethyl propyl titanate and 0.04mmol of mercaptan into a mixed solution of ethylene glycol and deionized water with the volume ratio of 2:1 of 80 mL, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 30 min to uniformly disperse the mixed solution, and fully mixing the mixed solution to obtain a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 220 ℃ to react for 30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3 times, and drying in a vacuum drying oven at 120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 40 mg dopamine hydrochloride into the suspension, magnetically stirring for 20h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 550 ℃ at a heating rate of 2 ℃/min, and kept at a temperature of 3 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
Example 3
The carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is prepared by the following steps:
the first step: adding 0.02 mmol of organic titanium salt ethyl propyl titanate and 0.04mmol of sulfur-containing amino acid into a mixed solution of ethylene glycol and deionized water with the volume ratio of 80 mL being 2:1, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 30 min to uniformly disperse the mixed solution, and fully mixing the mixed solution to obtain a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 240 ℃ to react 20 and h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing 3 times with deionized water and an organic solvent, and drying in a vacuum drying oven at 120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 60 mg dopamine hydrochloride into the suspension, magnetically stirring for 25 h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 600 ℃ at a heating and cooling rate of 2 ℃/min, and kept at a temperature of 2 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
Claims (8)
1. A preparation method of a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is characterized by comprising the following steps of,
the first step: adding 0.02-0.04 mmol of organic titanium salt and 0.04-0.08 mmol of sulfur-containing functional group organic compound into a mixed solution of 80 mL glycol and deionized water (wherein the volume ratio of the organic titanium salt to the sulfur-containing functional group organic compound is 1-2:1), magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 20-30 min to uniformly disperse the mixture, and fully mixing the solution, and marking the mixture as a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 200-240 ℃ to react for 20-30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3-5 times, and drying in a vacuum drying oven at 100-120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion, adding 40-60 mg dopamine hydrochloride into the suspension, magnetically stirring for 20-30 h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 60-80 ℃ to obtain C;
fourth step: and C is placed in an argon gas mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 500-600 ℃ at a heating and cooling rate of 1-2 ℃/min, and kept at a temperature of 2-4 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
2. The method for preparing the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material as claimed in claim 1, wherein the organic titanium salt is one or a combination of tetrabutyl titanate, isopropyl titanate and ethyl titanate.
3. The method for preparing the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material as claimed in claim 1, wherein the sulfur-containing functional group is one or a combination of thiourea, mercaptan and sulfur-containing amino acid.
4. A method for preparing a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material as claimed in any one of claims 1 to 3, wherein the method comprises the following steps:
the first step: adding 0.02 mmol of organic titanium salt tetrabutyl titanate and 0.04mmol of sulfur-containing functional group organic compound l thiourea into a mixed solution of 80 mL glycol and deionized water, wherein the volume ratio of the tetrabutyl titanate to the thiourea is 1:1, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 20 min to uniformly disperse the hollow tube carbon skeleton, and fully mixing the solution, and marking the mixture as a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 200 ℃ to react for 30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3-5 times, and drying in a vacuum drying oven at 100 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 40 mg dopamine hydrochloride into the suspension, magnetically stirring for 20 hours, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon gas mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 500 ℃ at a heating rate of 2 ℃/min, and kept at a temperature of 4 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
5. A method for preparing a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material as claimed in any one of claims 1 to 3, wherein the method comprises the following steps:
the first step: adding 0.02 mmol of organic titanium salt ethyl propyl titanate and 0.04mmol of mercaptan into a mixed solution of ethylene glycol and deionized water with the volume ratio of 2:1 of 80 mL, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 30 min to uniformly disperse the mixed solution, and fully mixing the mixed solution to obtain a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 220 ℃ to react for 30 h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing with deionized water and an organic solvent for 3 times, and drying in a vacuum drying oven at 120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 40 mg dopamine hydrochloride into the suspension, magnetically stirring for 20h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 550 ℃ at a heating rate of 2 ℃/min, and kept at a temperature of 3 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
6. A method for preparing a carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material as claimed in any one of claims 1 to 3, wherein the method comprises the following steps:
the first step: adding 0.02 mmol of organic titanium salt ethyl propyl titanate and 0.04mmol of sulfur-containing amino acid into a mixed solution of ethylene glycol and deionized water with the volume ratio of 80 mL being 2:1, magnetically stirring, adding a hollow tube carbon skeleton into the mixed solution, performing ultrasonic dispersion for 30 min to uniformly disperse the mixed solution, and fully mixing the mixed solution to obtain a solution A;
and a second step of: transferring the solution A into a reaction kettle, heating to 240 ℃ to react 20 and h, naturally cooling the solution to room temperature, filtering the obtained precipitate, washing 3 times with deionized water and an organic solvent, and drying in a vacuum drying oven at 120 ℃ to obtain B;
and a third step of: dispersing the B obtained in the second step into a 100 mL buffer solution for ultrasonic dispersion to obtain a suspension; adding 60 mg dopamine hydrochloride into the suspension, magnetically stirring for 25 h, centrifugally separating precipitate, and drying the obtained product in a vacuum oven at 80 ℃ to obtain C;
fourth step: and C is placed in an argon mixed atmosphere containing 5% of hydrogen by volume fraction, heated to 600 ℃ at a heating and cooling rate of 2 ℃/min, and kept at a temperature of 2 h, so that the final product of the carbon skeleton supported ultrathin titanium disulfide nanosheet photocatalytic material is obtained.
7. A carbon skeleton-supported ultrathin titanium disulfide nanosheet photocatalytic material obtained by the preparation method according to any one of claims 1 to 6.
8. The use of the carbon skeleton-supported ultrathin titanium disulfide nanosheet photocatalytic material in tetracycline catalytic degradation as claimed in claim 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117511348A (en) * | 2024-01-02 | 2024-02-06 | 成都虹润制漆有限公司 | Self-repairing heavy-duty anticorrosive paint and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117511348A (en) * | 2024-01-02 | 2024-02-06 | 成都虹润制漆有限公司 | Self-repairing heavy-duty anticorrosive paint and preparation method thereof |
| CN117511348B (en) * | 2024-01-02 | 2024-03-22 | 成都虹润制漆有限公司 | Self-repairing heavy-duty anticorrosive paint and preparation method thereof |
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