CN115709085A - In-situ corrosion preparation method of titanium dioxide/molybdenum disulfide heterojunction - Google Patents
In-situ corrosion preparation method of titanium dioxide/molybdenum disulfide heterojunction 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 210
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 105
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 15
- 238000005260 corrosion Methods 0.000 title claims abstract description 13
- 230000007797 corrosion Effects 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000008367 deionised water Substances 0.000 claims abstract description 38
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 38
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 23
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004073 vulcanization Methods 0.000 claims abstract description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 12
- 239000011733 molybdenum Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 17
- -1 titanium ions Chemical class 0.000 claims description 14
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical group CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 12
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 9
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 9
- 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
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005987 sulfurization reaction Methods 0.000 claims 2
- 239000002019 doping agent Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052979 sodium sulfide Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 description 22
- 239000007789 gas Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 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 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- 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 belongs to the field of preparation of nano functional materials, and particularly relates to an in-situ corrosion preparation method of a titanium dioxide/molybdenum disulfide heterojunction material. The in-situ corrosion preparation method comprises the following steps: 1) Mixing a titanium source with water to prepare a titanium ion solution; then mixing the sodium ion solution with a molybdenum doping source and urea to obtain a precursor solution; 2) Carrying out hydrothermal treatment on the precursor solution in the step 1) at the temperature of 100-180 ℃ to obtain molybdenum-doped titanium dioxide; 3) Mixing the molybdenum-doped titanium dioxide, the sulfur source and the deionized water in the step 2), stirring, and carrying out hydrothermal vulcanization at 180-250 ℃ to obtain the titanium dioxide/molybdenum disulfide heterojunction. The invention can realize more uniform and firm combination of the molybdenum disulfide and the titanium dioxide, further enhance the carrier density of the titanium dioxide and improve the photocatalysis and gas sensitivity performance of the titanium dioxide.
Description
Technical Field
The invention belongs to the field of preparation of nano functional materials, and particularly relates to an in-situ corrosion preparation method of a titanium dioxide/molybdenum disulfide heterojunction material.
Background
Titanium dioxide is a traditional semiconductor material, can be used for decomposing organic pollutants, photolyzing water to produce hydrogen, sensing gas and the like, and has important application prospects in the fields of environment and energy. Researches show that the performance of the titanium dioxide is related to the forbidden bandwidth and the carrier density thereof, and the photocatalytic and gas-sensitive performances can be effectively improved by reducing the forbidden bandwidth or increasing the carrier density.
The molybdenum disulfide is a two-dimensional semiconductor, has the characteristics of narrow forbidden band width and high carrier density, and can effectively improve the photocatalysis and gas-sensitive performance of the titanium dioxide after forming a heterojunction with the titanium dioxide. The existing preparation method of the titanium dioxide/molybdenum disulfide heterojunction mainly comprises a step method and a one-step method. The step method is that titanium dioxide material is firstly synthesized, then titanium dioxide is added into the precursor for preparing molybdenum disulfide, and molybdenum disulfide is deposited on the surface of titanium dioxide by hydrothermal method or other treatment means, so as to obtain titanium dioxide/molybdenum disulfide heterojunction. The one-step preparation method is to mix precursors of titanium dioxide and molybdenum disulfide and then obtain the titanium dioxide/molybdenum disulfide heterojunction by preparation means such as a hydrothermal method.
In the step-by-step preparation process, due to the fact that the lattices of the titanium dioxide and the sulfur dioxide are not matched, the subsequently grown sulfur dioxide is difficult to be firmly combined on the surface of the titanium dioxide, and is easy to separate in the using process, and the using performance is reduced. In the one-step preparation process, the titanium dioxide and the molybdenum disulfide are not uniformly dispersed in the heterojunction due to inconsistent crystal growth conditions of the titanium dioxide and the molybdenum disulfide, so that the performance is influenced. At present, a new preparation method of a titanium dioxide/molybdenum disulfide heterojunction is urgently needed to be provided to solve the problems of weak combination, uneven dispersion and the like of titanium dioxide and molybdenum disulfide in the existing preparation method.
Disclosure of Invention
In order to solve the technical problems, the invention provides an in-situ corrosion preparation method of a titanium dioxide/molybdenum disulfide heterojunction.
Specifically, the in-situ corrosion preparation method of the titanium dioxide/molybdenum disulfide heterojunction provided by the invention comprises the following steps:
1) Mixing a titanium source with water to prepare a titanium ion solution; then mixing the sodium ion solution with a molybdenum doping source and urea to obtain a precursor solution;
2) Carrying out hydrothermal treatment on the precursor solution in the step 1) at the temperature of 100-180 ℃ to obtain molybdenum-doped titanium dioxide;
3) Mixing the molybdenum-doped titanium dioxide, the sulfur source and the deionized water in the step 2), stirring, and carrying out hydrothermal vulcanization at 180-250 ℃ to obtain the titanium dioxide/molybdenum disulfide heterojunction.
According to the invention, under the conditions of specific raw materials, hydrothermal and hydrothermal vulcanization, molybdenum doped titanium dioxide is corroded by sulfur, molybdenum is stripped out of titanium dioxide crystal lattices and is combined with sulfur in situ on the surface of titanium dioxide to form molybdenum disulfide, so that uniform and firm combination of molybdenum disulfide and titanium dioxide is realized, the carrier density of titanium dioxide is further enhanced, and the photocatalysis and gas sensitivity performance of the titanium dioxide are improved.
Preferably, the titanium source is selected from titanyl sulfate, titanium tetrachloride or tetrabutyl titanate, preferably titanyl sulfate.
Preferably, the molybdenum doping source is selected from sodium molybdate, sodium molybdate dihydrate or ammonium molybdate, preferably sodium molybdate dihydrate.
Preferably, the sulphur source is selected from thioacetamide, sodium sulphide or thiourea, preferably thioacetamide.
In the invention, by adopting the preferable titanium source, molybdenum doping source and sulfur source, the molybdenum disulfide can be dispersed more uniformly on the surface of the titanium dioxide, so that the photocatalysis effect is better.
More preferably, in the step 1), the concentration of the titanium source in the titanium ion solution is 0.1 to 1.5mol/L, and preferably 0.5mol/L. In the invention, the titanium ion solution with specific concentration is adopted, so that the hydrolysis speed of titanium ions can be controlled more easily, and the particle size of the synthesized molybdenum-doped titanium dioxide is more uniform.
Further preferably, in step 1), the molar ratio of the titanium ions in the titanium ion solution, the molybdenum doping source and the urea is 100: (0.1-20): (50 to 300), preferably 100:5:200. in the invention, the molar ratio of the titanium ions, the molybdenum doping source and the urea is optimized, so that the molybdenum element can be more uniformly distributed in the crystal lattice of the titanium dioxide.
More preferably, in the step 3), the mass volume ratio of the molybdenum-doped titanium dioxide to the sulfur source to the deionized water is 10g (0.2-2 g) to 200mL, preferably 10 g. The invention unexpectedly discovers that the proportion of molybdenum element in the molybdenum-doped titanium dioxide converted into molybdenum disulfide is higher by carrying out hydrothermal vulcanization on the molybdenum-doped titanium dioxide, the sulfur source and the deionized water in a specific preferred proportion, and the photocatalytic performance and the gas-sensitive performance of the molybdenum-doped titanium dioxide are further improved.
Further preferably, in the step 2), the hydrothermal temperature is 100-180 ℃, and the hydrothermal time is 10-15 h; preferably, the hydrothermal temperature is 150 ℃ and the hydrothermal time is 12h.
Further preferably, in the step 3), the hydrothermal vulcanization temperature is 180-250 ℃, and the hydrothermal vulcanization time is 18-48 h; preferably, the hydrothermal vulcanization temperature is 200 ℃ and the hydrothermal vulcanization time is 24h. According to the invention, by optimizing hydrothermal and hydrothermal vulcanization conditions, molybdenum disulfide can be dispersed on the surface of titanium dioxide more uniformly and combined more firmly, and the photocatalytic performance and gas-sensitive performance of the molybdenum disulfide are further improved.
Further preferably, step 2) further comprises: and filtering and washing the product after the hydrothermal reaction by using deionized water.
Further preferably, step 3) further comprises: and washing the hydrothermal vulcanization product by using deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
More preferably, in step 3), the stirring time is 30min.
The invention provides an in-situ corrosion preparation method of a titanium dioxide/molybdenum disulfide heterojunction, which comprises the following steps:
step 1: adding a certain amount of titanyl sulfate, titanium tetrachloride or tetrabutyl titanate serving as a titanium source into 1L of water to prepare a titanium ion solution of 0.1-1.5 mol/L, then adding 0.1-20% of a molybdenum doping source and 50-300% of urea into the solution by taking the molar weight of the titanium ions as a reference, and stirring to obtain a reaction precursor solution;
step 2: heating the precursor solution in the step 1 at 100-180 ℃ for 10-15 h, and filtering and washing a product after reaction by using deionized water to obtain molybdenum-doped titanium dioxide;
and step 3: and (3) adding 10g of the molybdenum-doped titanium dioxide obtained in the step (2) and 0.2g to 2g of sulfur source into 200mL of deionized water, stirring for 30min, carrying out hydrothermal vulcanization reaction, wherein the hydrothermal vulcanization temperature is 180 ℃ to 250 ℃, the hydrothermal vulcanization time is 18h to 48h, and washing the hydrothermal vulcanization product with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
In a second aspect, the invention also provides the titanium dioxide/molybdenum disulfide heterojunction prepared by the in-situ corrosion preparation method of the titanium dioxide/molybdenum disulfide heterojunction.
The invention has the beneficial effects that: according to the invention, under specific raw materials and conditions, the molybdenum-doped titanium dioxide is corroded by using the sulfur element, the molybdenum element is stripped out of titanium dioxide crystal lattices and is combined with the sulfur element in situ on the surface of the titanium dioxide to form molybdenum disulfide, so that the uniform and firm combination of the molybdenum disulfide and the titanium dioxide is realized, the carrier density of the titanium dioxide is enhanced, and the photocatalysis and gas sensitivity performance of the titanium dioxide is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a transmission electron micrograph of a titanium dioxide/molybdenum disulfide heterojunction prepared according to example 1 of the present invention.
FIG. 2 is a chart of the UV-VIS absorption spectrum of the titanium dioxide/molybdenum disulfide heterojunction prepared in example 1 of the present invention.
FIG. 3 shows the photocatalytic degradation rate of phenol in the examples and comparative examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The instruments and the like are conventional products which are purchased by normal distributors and are not indicated by manufacturers. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Adding titanyl sulfate into water to prepare a solution of 0.5mol/L, then adding 5% of sodium molybdate dihydrate and 200% of urea based on the molar weight of titanium ions, carrying out hydrothermal treatment for 12h at 150 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 1g of thioacetamide, stirring for 30min, reacting at 200 ℃ for 24h, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Fig. 1 is a TEM image of example 1, and it can be seen from fig. 1 that the lattices of the molybdenum disulfide and titanium dioxide synthesized in this example are tightly combined together to form a stronger heterostructure.
Fig. 2 shows the uv-vis absorption spectrum of example 1, and it can be seen from fig. 2 that the titanium dioxide/molybdenum disulfide heterojunction synthesized in this example has excellent absorption capacity in the visible light region of 200nm to 800 nm.
Example 2
Adding titanium tetrachloride into water to prepare a 0.1mol/L solution, then adding 0.1% of sodium molybdate and 50% of urea by taking the molar weight of titanium ions as a reference, heating for 10 hours at 100 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 0.2g of thioacetamide, stirring for 30min, reacting at 180 ℃ for 18h, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Example 3
Adding tetrabutyl titanate into water to prepare a solution of 1.5mol/L, then adding 20% of ammonium molybdate and 300% of urea by taking the molar weight of titanium ions as a reference, heating for 15h at 180 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 2g of thioacetamide, stirring for 30min, reacting for 48h at 250 ℃, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Example 4
Adding titanyl sulfate into water to prepare a solution of 1.0mol/L, then adding 15% of sodium molybdate dihydrate and 150% of urea by taking the molar weight of titanium ions as a reference, heating for 12h at 120 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 0.5g of thioacetamide, stirring for 30min, reacting for 36h at 220 ℃, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Example 5
Adding titanyl sulfate into water to prepare a solution of 1.2mol/L, then adding 18 percent of sodium molybdate dihydrate and 80 percent of urea by taking the molar weight of titanium ions as a reference, heating for 14 hours at 130 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 0.6g of thioacetamide, stirring for 30min, reacting for 30h at 240 ℃, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Example 6
Adding tetrabutyl titanate into water to prepare a 0.8mol/L solution, then adding 12% of ammonium molybdate and 240% of urea by taking the molar weight of titanium ions as a reference, heating for 10 hours at 130 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 1.5g of thioacetamide, stirring for 30min, reacting for 20h at 240 ℃, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Comparative example 1
Adding titanium isopropoxide into water to prepare a solution of 0.5mol/L, then adding 5% of sodium molybdate dihydrate and 100% of urea by taking the molar weight of titanium ions as a reference, heating for 12h at 150 ℃ after stirring, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 1g of thioacetamide, stirring for 30min, reacting at 200 ℃ for 24h, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Comparative example 2
Adding titanyl sulfate into water to prepare a 0.5mol/L solution, then adding 25% of sodium molybdate dihydrate and 300% of urea by taking the molar weight of titanium ions as a reference, stirring, carrying out hydrothermal treatment at 150 ℃ for 12h, and washing with deionized water to obtain molybdenum-doped titanium dioxide;
adding 10g of molybdenum-doped titanium dioxide into 200mL of deionized water, adding 1g of thioacetamide, stirring for 30min, reacting at 200 ℃ for 24h, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Comparative example 3
Adding titanyl sulfate into water to prepare a solution of 0.5mol/L, then adding 200% of urea by taking the molar weight of titanium ions as a reference, stirring, performing hydrothermal treatment at 150 ℃ for 12 hours, and washing with deionized water to obtain titanium dioxide;
adding 10g of titanium dioxide into 200mL of deionized water, adding 1g of sodium molybdate dihydrate and 1g of thioacetamide, stirring for 30min, reacting for 24h at 200 ℃, and washing with deionized water to obtain the titanium dioxide/molybdenum disulfide heterojunction.
Experimental example 1
0.1g of the synthesized titanium dioxide/molybdenum disulfide heterojunction was added to 100mL of a phenol solution (10 mg/L), and the concentration of phenol in the solution was measured after standing in the dark for 30min (c) 0 ) Then, a 25W fluorescent lamp is turned on for illumination, and the concentration of phenol in the solution is detected after 8 hours (c) 8 ) Degradation rate of phenol = (c) 0 -c 8 )/c 0 X 100%, the results are shown in FIG. 3. The titanium dioxide/molybdenum disulfide heterojunction prepared by the in-situ corrosion method of the invention has the best phenol degradation effect especially with the raw materials and conditions of example 1.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. An in-situ corrosion preparation method of a titanium dioxide/molybdenum disulfide heterojunction is characterized by comprising the following steps:
1) Mixing a titanium source with water to prepare a titanium ion solution; then mixing the sodium ion solution with a molybdenum doping source and urea to obtain a precursor solution;
2) Carrying out hydrothermal treatment on the precursor solution in the step 1) at the temperature of 100-180 ℃ to obtain molybdenum-doped titanium dioxide;
3) Mixing the molybdenum-doped titanium dioxide, the sulfur source and the deionized water in the step 2), stirring, and carrying out hydrothermal vulcanization at 180-250 ℃ to obtain the titanium dioxide/molybdenum disulfide heterojunction.
2. The method of claim 1, wherein the titanium source is selected from the group consisting of titanyl sulfate, titanium tetrachloride, and tetrabutyl titanate.
3. The method of claim 2, wherein the molybdenum dopant source is selected from sodium molybdate, sodium molybdate dihydrate or ammonium molybdate.
4. The method for the in situ corrosion production of a titanium dioxide/molybdenum disulfide heterojunction as claimed in claim 3 wherein said sulfur source is selected from thioacetamide, sodium sulfide or thiourea.
5. The method for preparing a titanium dioxide/molybdenum disulfide heterojunction as claimed in any one of claims 2 to 4, wherein in step 1), the concentration of the titanium source in the titanium ion solution is 0.1 to 1.5mol/L.
6. The method for preparing a titanium dioxide/molybdenum disulfide heterojunction as claimed in any one of claims 2 to 5, wherein in step 1), the molar ratio of the titanium ions in the titanium ion solution, the molybdenum doping source and the urea is 100: (0.1-20): (50-300).
7. The method for preparing the titanium dioxide/molybdenum disulfide heterojunction as in any one of claims 2 to 6, wherein in the step 3), the mass-to-volume ratio of the molybdenum-doped titanium dioxide, the sulfur source and the deionized water is 10g (0.2-2 g) to 200mL.
8. The method for preparing the titanium dioxide/molybdenum disulfide heterojunction as in any one of claims 1 to 7, wherein in the step 2), the hydrothermal temperature is 100-180 ℃ and the hydrothermal time is 10-15 h.
9. The method for preparing the titanium dioxide/molybdenum disulfide heterojunction as in any one of claims 1 to 8, wherein in the step 3), the hydrothermal sulfurization temperature is 180-250 ℃ and the hydrothermal sulfurization time is 18-48 h.
10. A titanium dioxide/molybdenum disulfide heterojunction prepared by the in situ corrosion method of preparing a titanium dioxide/molybdenum disulfide heterojunction as defined in any one of claims 1 to 9.
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