CN116272985B - Preparation method, product and application of silver molybdate@titanium@network titanium dioxide - Google Patents
Preparation method, product and application of silver molybdate@titanium@network titanium dioxide 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 85
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 39
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 34
- MHLYOTJKDAAHGI-UHFFFAOYSA-N silver molybdate Chemical compound [Ag+].[Ag+].[O-][Mo]([O-])(=O)=O MHLYOTJKDAAHGI-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 32
- 239000011259 mixed solution Substances 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 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
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 9
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 239000011541 reaction mixture Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 150000003608 titanium Chemical class 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 230000001699 photocatalysis Effects 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 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 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000004964 aerogel Substances 0.000 claims description 5
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 5
- 229940071536 silver acetate Drugs 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 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 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 239000004098 Tetracycline Substances 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 229960002180 tetracycline Drugs 0.000 abstract description 6
- 229930101283 tetracycline Natural products 0.000 abstract description 6
- 235000019364 tetracycline Nutrition 0.000 abstract description 6
- 150000003522 tetracyclines Chemical class 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 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
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/686—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with molybdenum
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
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- 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
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a preparation method of silver molybdate@titanium@network titanium dioxide, which comprises the following specific steps: adding titanium salt and strong alkali into deionized water, stirring uniformly, transferring into a flask, stirring, and introducing inert gas; adding ethanol into the mixed solution, dissolving a reducing agent in deionized water, rapidly adding the reducing agent solution into the solution, centrifuging and washing to obtain network Ti@TiO; adding silver salt into oleylamine, stirring to obtain a mixed solution, introducing inert gas into the mixed solution, and heating the mixed solution to dissolve the silver salt; injecting alcohol into the solution, stirring, heating, maintaining the reaction mixture at the temperature for 20-30 min, and cooling to room temperature to obtain A; adding Ti@TiO and A into an ammonium molybdate solution, stirring uniformly, heating and evaporating the solvent, and calcining to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide. In the dark, the adsorption of the tetracycline reaches the equilibrium, and then the degradation of the tetracycline reaches 99.8% after 60min under the ultraviolet light catalysis condition.
Description
Technical Field
The invention relates to a nano photocatalytic material and preparation and application thereof, in particular to a preparation method, a product and application of silver molybdate@titanium@network titanium dioxide.
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 these dyes are chemically stable 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.
Titanium dioxide (TiO 2) is paid attention to as a photocatalytic material, and under the illumination condition, the TiO2 can oxidize organic pollutants in water, so that the photocatalytic technology has great breakthrough in the field of treating organic pollutants in water phase and gas phase. Since then, photocatalytic degradation of organic pollutants has become one of the hot areas.
In order to improve the catalytic efficiency of TiO2 as a photocatalyst, various means have been employed to modify the material. The TiO2 is coated, so that the spectral absorption range of the material is remarkably improved, and the effective separation and transmission of photo-generated charges are promoted, so that the photocatalytic performance of the material is improved. Silver molybdate is also an important photocatalyst, and silver molybdate materials have a narrow spectral response range and low photogenerated carrier separation efficiency. Coating the titanium dioxide with the catalyst further improves the electrochemical performance of the material.
The invention provides a preparation method of silver molybdate@titanium@network titanium dioxide. Firstly preparing Ti@TiO by a one-step synthesis method, and then further carrying out secondary coating of silver molybdate, wherein the photocatalytic performance of titanium dioxide can be improved by the secondary coating. The preparation process is relatively simple and easy to operate.
Disclosure of Invention
In order to overcome the defect that the existing titanium dioxide has insufficient photocatalytic performance, the invention aims to: a preparation method of silver molybdate@titanium@network titanium dioxide is provided.
Still another object of the present invention is: there is provided a silver molybdate @ titanium @ network titanium dioxide product obtained by the above method.
Yet another object of the present invention is: there is provided the use of the above product.
The invention aims at realizing the following scheme: the preparation method of the silver molybdate@titanium@network titanium dioxide is characterized by preparing the silver molybdate@titanium@network titanium dioxide by a two-step chemical solution method, and comprises the following specific steps of:
(1) Adding 4-6 g of soluble titanium salt and 1.6-2.4 g of strong alkali into deionized water, stirring for 1-2 h until uniform, transferring the mixed solution into a three-neck flask, continuously stirring for 20-30 min, and then introducing inert gas for 20-30 min;
(2) Adding 100-150 mu L of ethanol into the mixed solution, dissolving 12-16 g of reducing agent into deionized water, rapidly adding the reducing agent solution into the solution in the stirring process, centrifuging after 15-20 min, and washing 3-5 times by using deionized water and absolute ethanol to obtain three-dimensional aerogel network Ti@TiO;
(3) Adding 0.02-0.04 mmol of silver salt into 10-15 mL of oleylamine, magnetically stirring to form a mixed solution, then introducing inert gas Ar gas into the mixed solution for 20-30 min, and gradually heating the mixed solution to 120-150 ℃ to completely dissolve the silver salt to form a solution;
(4) Injecting alcohol into the solution, wherein the molar ratio of silver salt to alcohol is 1:4, magnetically stirring for 30-60 min at the temperature, then heating to 160-180 ℃, keeping the reaction mixture at the temperature for 20-30 min, and naturally cooling to room temperature to obtain A;
(5) Adding Ti@TiO obtained in the step (2) and the A obtained in the step (4) into an ammonium molybdate solution, uniformly stirring, heating and evaporating the solvent, and calcining in a muffle furnace at 500-700 ℃ for 3-5 h to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide.
Preferably, in the step (1), the titanium salt is one of tetrabutyl titanate or tetraisopropyl titanate or a combination thereof.
Preferably, in the step (1), the strong base is one or a combination of sodium hydroxide and potassium hydroxide.
Preferably, in the step (1), the inert gas is one of argon or nitrogen or a combination thereof.
Preferably, in the step (2), the reducing agent is one or a combination of hydrazine hydrate and sodium borohydride.
Preferably, in the step (3), the silver salt is one or a combination of silver acetate, silver nitrate and silver chlorate.
Preferably, in the step (4), the alcohol is one or a combination of ethylene glycol and glycerol.
The invention provides silver molybdate@titanium@network titanium dioxide which is prepared by any one of the above methods.
The invention provides an application of a silver molybdate@titanium@network titanium dioxide photocatalytic material in wastewater treatment.
The beneficial effects are that:
the invention provides a preparation method of silver molybdate@titanium@network titanium dioxide. Firstly preparing Ti@TiO by a one-step synthesis method, and then further carrying out secondary coating of silver molybdate, wherein the photocatalytic performance of titanium dioxide can be improved by the secondary coating. The preparation process is relatively simple and easy to operate. The silver molybdate@titanium@network titanium dioxide firstly reaches equilibrium on the adsorption of the tetracycline in darkness, and then reaches 99.8% on the degradation of the tetracycline after 60min under the ultraviolet light catalysis condition.
Drawings
FIG. 1 is a graph of ultraviolet light catalyzed degradation of example 1 silver molybdate @ titanium @ network titanium dioxide.
Fig. 2 is an SEM image of example 2 silver molybdate @ titanium @ network titanium dioxide.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
(1) Adding 4g of soluble tetrabutyl titanate and 1.6g of strong alkali sodium hydroxide into deionized water, stirring for 1h to uniformity, transferring the mixed solution into a three-neck flask, continuously stirring for 20min, and then introducing inert gas argon for 20min;
(2) Adding 100 mu L of ethanol into the mixed solution, dissolving 12g of reducing agent sodium borohydride into deionized water, rapidly adding sodium borohydride solution into the solution in the stirring process, centrifuging after 15min, and washing 3 times with deionized water and absolute ethanol to obtain three-dimensional aerogel network Ti@TiO;
(3) Adding 0.02mmol of silver nitrate into 10mL of oleylamine, magnetically stirring to form a mixed solution, then introducing inert gas Ar gas into the mixed solution for 20min, and gradually heating the mixed solution to 120 ℃ to completely dissolve the silver nitrate to form a solution;
(4) Ethylene glycol was injected into the above solution, wherein the molar ratio of silver nitrate to ethylene glycol was 1:4, magnetically stirring for 30min at the temperature, then heating to 160 ℃, keeping the reaction mixture at the temperature for 20min, and naturally cooling to room temperature to obtain A;
(5) Adding Ti@TiO obtained in the step (2) and the A obtained in the step (4) into an ammonium molybdate solution, uniformly stirring, heating and evaporating the solvent, and calcining in a muffle furnace at 500 ℃ for 5 hours to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide.
FIG. 1 is a graph of ultraviolet light catalyzed degradation of silver molybdate @ titanium @ network titanium dioxide. The silver molybdate@titanium@network titanium dioxide firstly reaches equilibrium on the adsorption of the tetracycline in darkness, and then reaches 99.8% on the degradation of the tetracycline after 60min under the ultraviolet light catalysis condition.
Example 2
(1) Adding 5g of soluble tetraisopropyl titanate and 2g of strong alkali potassium hydroxide into deionized water, stirring for 1.5h to uniformity, transferring the mixed solution into a three-neck flask, continuously stirring for 25min, and then introducing inert gas nitrogen for 25min;
(2) Adding 120 mu L of ethanol into the mixed solution, dissolving 14g of reducing agent hydrazine hydrate in deionized water, rapidly adding a hydrazine hydrate solution into the solution in the stirring process, centrifuging after 20min, and washing with deionized water and absolute ethanol for 5 times to obtain three-dimensional aerogel network Ti@TiO;
(3) Adding 0.04mmol of silver acetate into 15mL of oleylamine, magnetically stirring to form a mixed solution, then introducing inert gas Ar gas into the mixed solution for 25min, and gradually heating the mixed solution to 150 ℃ to completely dissolve the silver acetate to form a solution;
(4) Injecting glycerol into the solution, wherein the molar ratio of the silver acetate to the glycerol is 1:4, magnetically stirring for 60min at the temperature, then heating to 180 ℃, keeping the reaction mixture at the temperature for 25min, and naturally cooling to room temperature to obtain A;
(5) Adding Ti@TiO obtained in the step (2) and the A obtained in the step (4) into an ammonium molybdate solution, uniformly stirring, heating and evaporating the solvent, and calcining in a muffle furnace at 600 ℃ for 4 hours to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide.
FIG. 2 is an SEM image of silver molybdate@titanium@network titanium dioxide, which shows that the image is a three-dimensional network structure with the particle size of 200-300 nm.
Example 3
(1) Adding 6g of soluble tetraisopropyl titanate and 2.4g of strong alkali sodium hydroxide into deionized water, stirring for 2 hours until the mixture is uniform, transferring the mixed solution into a three-neck flask, continuously stirring for 30 minutes, and then introducing inert gas argon for 30 minutes;
(2) Adding 150 mu L of ethanol into the mixed solution, dissolving 116g of reducing agent sodium borohydride into deionized water, rapidly adding sodium borohydride solution into the solution in the stirring process, centrifuging after 20min, and washing 3 times with deionized water and absolute ethanol to obtain three-dimensional aerogel network Ti@TiO;
(3) Adding 0.04mmol of silver chlorate into 15mL of oleylamine, magnetically stirring to form a mixed solution, then introducing inert gas Ar gas into the mixed solution for 30min, and gradually heating the mixed solution to 150 ℃ to completely dissolve silver salt to form a solution;
(4) Ethylene glycol was injected into the above solution, wherein the molar ratio of silver chlorate to ethylene glycol was 1:4, magnetically stirring for 60min at the temperature, then heating to 180 ℃, keeping the reaction mixture at the temperature for 30min, and naturally cooling to room temperature to obtain A;
(5) Adding Ti@TiO obtained in the step (2) and the A obtained in the step (4) into an ammonium molybdate solution, uniformly stirring, heating and evaporating the solvent, and calcining in a muffle furnace at 700 ℃ for 3 hours to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide.
Claims (9)
1. The preparation method of the silver molybdate@titanium@network titanium dioxide is characterized by preparing the silver molybdate@titanium@network titanium dioxide by a two-step chemical solution method and comprises the following steps of:
(1) Adding 4-6 g of soluble titanium salt and 1.6-2.4 g of strong alkali into deionized water, stirring for 1-2 h until uniform, transferring the mixed solution into a three-neck flask, continuously stirring for 20-30 min, and then introducing inert gas for 20-30 min;
(2) Adding 100-150 mu L of ethanol into the mixed solution, dissolving 12-16 g of reducing agent into deionized water, rapidly adding the reducing agent solution into the solution in the stirring process, centrifuging after 15-20 min, and washing 3-5 times by using deionized water and absolute ethanol to obtain three-dimensional aerogel network Ti@TiO;
(3) Adding 0.02-0.04 mmol of silver salt into 10-15 mL of oleylamine, magnetically stirring to form a mixed solution, then introducing inert gas Ar gas into the mixed solution for 20-30 min, and gradually heating the mixed solution to 120-150 ℃ to completely dissolve the silver salt to form a solution;
(4) Injecting alcohol into the solution, wherein the molar ratio of silver salt to alcohol is 1:4, magnetically stirring for 30-60 min at the temperature, then heating to 160-180 ℃, keeping the reaction mixture at the temperature for 20-30 min, and naturally cooling to room temperature to obtain A;
(5) Adding Ti@TiO obtained in the step (2) and the A obtained in the step (4) into an ammonium molybdate solution, uniformly stirring, heating and evaporating the solvent, and calcining in a muffle furnace at 500-700 ℃ for 3-5 h to obtain B, namely: silver molybdate @ titanium @ network titanium dioxide.
2. The method for preparing the silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the titanium salt is one or a combination of tetrabutyl titanate and tetraisopropyl titanate.
3. The method for preparing the silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the strong base is one or a combination of sodium hydroxide and potassium hydroxide.
4. The method for preparing the silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the inert gas is one or a combination of argon and nitrogen.
5. The method for preparing the silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the reducing agent is one or a combination of hydrazine hydrate and sodium borohydride.
6. The method for preparing the silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the silver salt is one or a combination of silver acetate, silver nitrate and silver chlorate.
7. The method for preparing silver molybdate@titanium@network titanium dioxide according to claim 1, wherein the alcohol is one or a combination of ethylene glycol and glycerol.
8. A silver molybdate@titanium@network titanium dioxide prepared according to the method of any one of the preceding claims 1-7.
9. Use of a silver molybdate @ titanium @ network-like titanium dioxide photocatalytic material according to claim 8 in wastewater treatment.
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