CN111036191A - Preparation method of metal molybdenum-doped modified titanium dioxide visible-light-driven photocatalyst - Google Patents
Preparation method of metal molybdenum-doped modified titanium dioxide visible-light-driven photocatalyst Download PDFInfo
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- CN111036191A CN111036191A CN201911283946.2A CN201911283946A CN111036191A CN 111036191 A CN111036191 A CN 111036191A CN 201911283946 A CN201911283946 A CN 201911283946A CN 111036191 A CN111036191 A CN 111036191A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 239000002184 metal Substances 0.000 title claims description 20
- 229910052751 metal Inorganic materials 0.000 title claims description 19
- 239000011941 photocatalyst Substances 0.000 title claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 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
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 13
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 2
- 239000001301 oxygen Substances 0.000 abstract 2
- 229910052760 oxygen Inorganic materials 0.000 abstract 2
- 238000011156 evaluation Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B01J35/39—
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- B01J35/40—
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention relates to a molybdenum-doped modified titanium dioxide visible light catalyst (Mo-TiO)2) Belonging to the technical field of nano material preparation and application. Doping of metallic Mo into TiO2In semiconductors, artificial introduction of surface oxygen defects can be achieved. TiO caused by Mo doping and introduction of surface oxygen defect2Narrowing the band gap of the semiconductor to make Mo-TiO2The range of light absorption is expanded to the visible light area, and then the TiO content is improved2Utilization of visible light by semiconductors. Further, NH per unit time is used3Evaluation of Mo-TiO2Photocatalytic nitrogen fixation performance. The method has simple preparation process, is environment-friendly, and is Mo-TiO2The efficiency of nitrogen fixation is high by visible light catalysis, so that the Mo-TiO2Has potential application value in the field of visible light catalytic nitrogen fixation.
Description
Technical Field
The invention belongs to the field of preparation and application of nano materials, and particularly relates to metal Mo-doped modified TiO2Visible light catalyst (Mo-TiO)2) The preparation method of (1).
Background
In recent years, the photocatalytic nitrogen fixation technology has the advantages of cleanness, high efficiency, selectivity and the like, and thus, the photocatalytic nitrogen fixation technology becomes a hot point of research of people. Researchers are actively developing some catalysts for the photocatalytic nitrogen fixation field, among which titanium dioxide (TiO)2) Semiconductors are one of the semiconductor materials widely studied at present due to their advantages such as chemical stability and low toxicity. But due to TiO2The semiconductor is a wide-band gap semiconductor, has a band gap of 3.2eV, can only be excited by Ultraviolet (UV) light, and has almost no absorption to visible light. In addition, TiO is prepared2The general process of semiconductor materials is complicated and it is difficult to control the particle uniformity, which makes TiO difficult2The application of semiconductors in the field of photocatalysis is greatly restricted. At present, in TiO2Doping a transition metal or a non-metal element in a semiconductor can improve the band gap energy, and is receiving wide attention from researchers. Therefore, the TiO is scaled down by doping with metal2Increasing TiO by making semiconductor band gap and its light absorption band edge red shift2Absorption of visible light is possible.
The invention develops a simple and convenient route for preparing the metal Mo-doped modified TiO2Visible light catalyst, and the nitrogen fixation performance of the visible light catalyst is researched.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a modified TiO doped with metal Mo2Visible light catalyst (Mo-TiO)2) The method is simple and easy to implement, and has higher yieldHigh.
The purpose of the invention is realized as follows: metal Mo-doped modified TiO2The preparation method of the visible light photocatalyst comprises the following steps:
(1) 1.6g of (polyethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (F127, molecular weight: 13000) and 0.273g of molybdenum pentachloride (MoCl) were added to 30mL of an anhydrous ethanol solvent5) Stirring at 60 ℃ for 1h at the rotation speed of 500rpm to fully dissolve the components to form a solution.
(2) Adding 2.3mL of glacial acetic acid, 0.7mL of concentrated hydrochloric acid and 3.5mL of tetrabutyl titanate (TBT) into the solution obtained in the step (1), and continuously stirring for 30min at the rotating speed of 500rpm to obtain a mixed solution; then the mixed solution is moved into an electrothermal blowing dry box and dried for 24 hours at the temperature of 60 ℃ to obtain the TiO doped with the metal Mo2And (4) gelling.
(3) TiO doped with metal Mo obtained in the step (2)2Transferring the gel into a muffle furnace for high-temperature calcination treatment, heating to 450 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling at room temperature to obtain the metal Mo-doped modified TiO2Visible light catalyst (Mo-TiO)2)。
The invention has the following advantages and positive effects:
1. the catalyst synthesized by the method has the advantages of high sample purity, high chemical stability, good dispersibility, uniform particle size and higher photocatalytic nitrogen fixation activity under the irradiation of visible light.
2. The process method is environment-friendly, low in cost, wide in raw material source, simple and easy to operate, and good in repeatability; has very wide application prospect for fixing nitrogen under the condition of visible light.
Drawings
FIG. 1 shows the Mo-doped modified TiO of the invention2Visible light catalyst (Mo-TiO)2) X-ray diffraction (XRD) pattern of (a);
FIG. 2 shows Mo-TiO of the present invention2Graph of solid ultraviolet diffuse reflectance spectrum (UV-vis DRS);
FIG. 3 shows Mo-TiO of the present invention2A Scanning Electron Microscope (SEM) image of (a);
FIG. 4 shows Mo-TiO of the present invention2The photocatalytic nitrogen fixation performance of (a).
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Metal Mo-doped modified TiO2The preparation method of the visible light photocatalyst comprises the following steps:
(1) 1.6g of (polyethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (F127, molecular weight: 13000) and 0.273g of molybdenum pentachloride (MoCl) were added to 30mL of an anhydrous ethanol solvent5) Stirring at 60 ℃ for 1h at the rotation speed of 500rpm to fully dissolve the components to form a solution.
(2) Adding 2.3mL of glacial acetic acid, 0.7mL of concentrated hydrochloric acid and 3.5mL of tetrabutyl titanate (TBT) into the solution obtained in the step (1), and continuously stirring for 30min at the rotating speed of 500rpm to obtain a mixed solution; then the mixed solution is moved into an electrothermal blowing dry box and dried for 24 hours at the temperature of 60 ℃ to obtain the TiO doped with the metal Mo2And (4) gelling.
(3) TiO doped with metal Mo obtained in the step (2)2Transferring the gel into a muffle furnace for high-temperature calcination treatment, heating to 450 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling at room temperature to obtain the metal Mo-doped modified TiO2Visible light catalyst (Mo-TiO)2)。
The metal Mo-doped modified TiO prepared by the method is characterized by X-ray diffraction (XRD), a solid ultraviolet-visible diffuse reflectance spectrum (UV-vis DRS) diagram and a Scanning Electron Microscope (SEM)2Visible light catalyst (Mo-TiO)2)；
Mo-TiO can be seen from the XRD diffraction pattern of FIG. 12All diffraction peaks of (A) are in contact with anatase phase TiO2The obtained XRD standard card (JCPDS card No.21-1272) has no other diffraction peaks, which indicates that the metal Mo is successfully doped into TiO2In semiconductors, and Mo-TiO2The purity of (A) is very high;
FIG. 2 is a graph of the UV-vis DRS spectrum showing the Mo-TiO sample2The absorption peak in a visible light region is obviously enhanced, and further shows that Mo-TiO2Visible by absorptionPhoto, catalytic nitrogen fixation is possible;
Mo-TiO can be seen from the SEM image of FIG. 32The particles are distributed in an aggregated spherical state, the particle size is uniform, and the diameter is about 30 nm;
FIG. 4 is Mo-TiO2The photocatalytic nitrogen fixation performance of (1) is shown in a figure, and Mo-TiO can be seen under the irradiation of visible light2Catalysis of N per unit time as a catalyst2Generation of NH3In an amount of pure TiO2More than 3 times of the catalyst indicates Mo-TiO2Has potential application value in the aspect of visible light catalysis nitrogen fixation.
1. The reagent dosage in the above steps can not be scaled up.
2. The reagents in the above steps are all analytically pure and are not further processed.
Claims (2)
1. A preparation method of a metal molybdenum-doped modified titanium dioxide visible-light-driven photocatalyst comprises the following steps:
(1) adding 1.6g of (polyethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) and 0.273g of molybdenum pentachloride into 30mL of absolute ethanol solvent, and stirring at 60 ℃ for 1h at the rotating speed of 500rpm to fully dissolve the mixture to form a solution;
(2) adding 2.3mL of glacial acetic acid, 0.7mL of concentrated hydrochloric acid and 3.5mL of tetrabutyl titanate into the solution obtained in the step (1), and continuously stirring for 30min at the rotating speed of 500rpm to obtain a mixed solution; then the mixed solution is moved into an electrothermal blowing dry box and dried for 24 hours at the temperature of 60 ℃ to obtain the TiO doped with the metal Mo2Gelling;
(3) TiO doped with metal Mo obtained in the step (2)2Transferring the gel into a muffle furnace for high-temperature calcination treatment, heating to 450 ℃ at the speed of 5 ℃/min, preserving the temperature for 4 hours, and naturally cooling at room temperature to obtain the metal Mo-doped modified TiO2A visible light photocatalyst.
2. The molybdenum metal doped modified titanium dioxide visible-light-driven photocatalyst as claimed in claim 1 is used for visible-light-driven photocatalytic nitrogen fixation.
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