CN113134349B - Blue layered Nb 2 O 5 Preparation method and application of photocatalyst - Google Patents
Blue layered Nb 2 O 5 Preparation method and application of photocatalyst Download PDFInfo
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01J23/20—Vanadium, niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
Abstract
The invention provides a blue layered Nb 2 O 5 A preparation method and application of a photocatalyst, belonging to the field of environmental functional materials. The blue layered Nb 2 O 5 The photocatalyst is prepared by the following method: (1) Mixing Nb with 2 C MXene is placed in a tube furnace, heat treatment is carried out in the air atmosphere, and white layered Nb is obtained after cooling to room temperature 2 O 5 (ii) a (2) In a reducing atmosphere, white layered Nb 2 O 5 Continuously carrying out heat treatment for 1-5 h, cooling to room temperature to obtain blue Nb 2 O 5 A photocatalyst. The blue layered Nb prepared by the method of the invention 2 O 5 The photocatalyst has an obvious layered structure, and can increase the contact area of the catalyst and gas pollutants; the surface has abundant oxygen vacancies, which can expand the light absorption area of the surface, promote charge separation and localize electrons, and has higher NO removal efficiency by photocatalysis.
Description
Technical Field
The invention belongs to the field of environment functional materials, and particularly relates to blue layered Nb 2 O 5 A preparation method of the photocatalyst and application thereof in removing NO by photocatalysis.
Background
With the acceleration of industrialization and urbanization, air pollution has become an important challenge for sustainable development of human society. Nitrogen oxides (NOx) are one of the main pollutants in the atmosphere, cause body diseases such as hypoxia, pulmonary edema and neurasthenia, and are closely related to photochemical smog, acid rain, haze, ozone layer destruction, and the like. NO is the main form of NOx, and among the existing methods for removing NO, the photocatalysis method has the advantages of simple equipment, mild reaction conditions, low energy consumption, less secondary pollution and the like, and becomes a hotspot of research.
Photocatalysts are the heart of the technology for photocatalytic treatment of NO, mainly semiconductors or materials with semiconducting properties. Conventional metal oxide semiconductors such as Nb 2 O 5 The material is white particles, has large forbidden band width, weak visible light response and high recombination rate of photo-generated electrons and holes, and causes low utilization rate of solar energy. In addition, when used as a photocatalyst, particles are easily accumulated, and contact of the catalytically active sites with the reaction gas is affected. In patent CN201911354599.8, blue Nb is prepared by a wet chemical treatment method 2 O 5 The energy band structure of the photocatalyst is changed, so that the absorption of visible light and near infrared light is enhanced, and the utilization rate of solar energy is improved. The invention patent CN201310692528.5 prepares a nitrogen-doped rod-like niobium pentoxide photocatalyst, which has a large specific surface area and a better length-diameter ratio, effectively inhibits the recombination of photo-generated electrons and holes, and improves the light energy conversion efficiency of the catalyst. Therefore, by pairing Nb 2 O 5 The photocatalyst is reasonably designed, the macroscopic configuration and the energy band structure of the photocatalyst are changed, the contact of catalytic activity sites and reactants can be enhanced, the separation of photoproduction electrons and holes is promoted, and the NO removal performance of the photocatalyst is improved.
Disclosure of Invention
In view of the above, the present invention aims to provideProvides a blue layered Nb 2 O 5 Preparation method and application of photocatalyst, nb of the invention 2 O 5 Photocatalyst by oxidation of Nb 2 The C MXene is prepared, the method and the process are simple, the operation is convenient, and the large-scale production is easy; nb 2 O 5 The photocatalyst keeps the layered structure of MXene, and the specific surface area is far higher than that of the traditional powder Nb 2 O 5 The full contact between the reaction gas and the active site is facilitated; nb of the invention 2 O 5 The photocatalyst is blue, has obvious absorbance in a visible light region, and obviously inhibits the recombination of photo-generated electrons and holes; the photocatalyst has higher NO conversion rate of photocatalytic removal, and has good application prospect in the field of gas pollutant treatment.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
blue layered Nb 2 O 5 The preparation method of the photocatalyst comprises the following steps: mixing Nb with 2 C MXene is put in a tubular furnace, heated to 400-700 ℃, heat-treated in the air for 1-10 h, cooled to room temperature to obtain white layered Nb 2 O 5 (ii) a Subjecting white layered Nb to reduction atmosphere 2 O 5 Heating to 400-700 ℃, continuing to carry out heat treatment for 1-5 h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
Heat treatment in air at high temperatures is critical. The temperature is too low, and the oxidation effect is poor; over-high temperature, nb 2 O 5 The crystal form is transformed, and the catalytic activity is reduced.
Furthermore, the heating rate of heating to 400-700 ℃ is 1-20 ℃/min, and the cooling to room temperature is natural cooling.
Furthermore, the reducing atmosphere is a mixed gas of hydrogen and inert gas, the inert gas is one of nitrogen, argon and helium, and the volume fraction of the hydrogen in the reducing atmosphere is 2-20%.
The second purpose of the invention is to provide a blue layered Nb prepared by the method 2 O 5 A photocatalyst.
Further, it is possible to provideSaid Nb 2 O 5 The photocatalyst is blue, has an obvious layered structure, has rich oxygen vacancies on the surface, and has obvious absorbance in a visible light region.
Commercial powdered Nb 2 O 5 Specific surface area 3m 2 (g) layered Nb prepared by the process of the present application 2 O 5 Can reach 60m 2 /g。
The third purpose of the invention is to provide the blue layered Nb 2 O 5 Application of a photocatalyst in photocatalytic removal of NO.
Compared with the prior art, the blue layered Nb provided by the invention 2 O 5 The preparation method of the photocatalyst has the following beneficial effects:
the invention is from Nb 2 C MXene, and heat treatment in air to obtain white layered Nb 2 O 5 Then heat-treated in a reducing atmosphere to form white layered Nb 2 O 5 Introducing oxygen vacancy on the surface to prepare blue layered Nb 2 O 5 A photocatalyst; the preparation method has simple process, convenient operation and easy large-scale production; blue layered Nb prepared by the invention 2 O 5 The photocatalyst has abundant oxygen vacancies on the surface, can provide an intermediate level in a forbidden band to expand a light absorption region, promotes charge separation and localizes electrons, and effectively enhances the photocatalytic activity. Meanwhile, the layered structure is beneficial to improving the specific surface area, increasing the contact of reaction gas and catalytic active sites and further improving the NO removal efficiency of photocatalysis.
Prepared Nb 2 O 5 The photocatalyst has an obvious layered structure and can enhance the contact of catalytic active sites and gas pollutants; prepared Nb 2 O 5 The photocatalyst is blue, has abundant oxygen vacancies on the surface, can expand the light absorption area of the photocatalyst, promotes charge separation and localizes electrons, and has higher NO removal efficiency by photocatalysis; the preparation method has the advantages of simple process, convenient operation and easy large-scale production.
The application of the photocatalyst is the same as the advantages of the preparation method compared with the prior art, and the description is omitted.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows the preparation of blue layered Nb in inventive example 1 2 O 5 Scanning electron micrographs of the photocatalyst;
FIG. 2 is a schematic representation of the preparation of blue layered Nb in inventive example 1 2 O 5 An X-ray diffraction pattern of the photocatalyst;
FIG. 3 is a schematic representation of the preparation of blue layered Nb in inventive example 1 2 O 5 The NO removal performance of the photocatalyst by photocatalysis.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Blue layered Nb 2 O 5 The preparation method of the photocatalyst comprises the following process steps:
(1) Preparation of white layered Nb 2 O 5 : mixing Nb with 2 C MXene is put in a tubular furnace, heated to 400-700 ℃ at the speed of 1-20 ℃/min, heat-treated in the air for 1-10 h, and cooled to room temperature to obtain white layered Nb 2 O 5 。
(2) Preparation of blue layered Nb 2 O 5 Photocatalyst: in the atmosphere of nitrogen, argon, helium and the like containing 2 to 20 percent of hydrogen, white layered Nb is added 2 O 5 Heating to 400-700 ℃ at the speed of 1-20 ℃/min, continuing heat treatment for 1-5 h, and cooling to room temperature to obtain blue Nb 2 O 5 A photocatalyst.
In the following examples, the Nb 2 The C MXene is prepared by the following method:
adding 75mL of concentrated hydrochloric acid into 25mL of deionized water to prepare 100mL of 9M hydrochloric acid; adding 8g of LiF into the prepared hydrochloric acid, and stirring at 600rpm until the LiF is completely dissolved to form a mixed solution; 5g of Nb was added to the mixed solution 2 AlC reacts for 96 hours at 40 ℃ under the stirring of 600 rpm; centrifuging the reacted suspension at 200rpm for 1min, centrifuging the upper layer liquid at 4000rpm for 10min, and washing the precipitate with deionized water to neutrality to obtain Nb 2 C MXene。
Example 1
(1) Mixing Nb with 2 Placing C MXene in a tube furnace, heating to 500 ℃ at the speed of 10 ℃/min, carrying out heat treatment in air for 2h, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) White layered Nb in argon atmosphere containing 10% hydrogen 2 O 5 Heating to 700 deg.C at a rate of 5 deg.C/min, continuing heat treatment for 1h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed in a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate is as high as 62.2%.
Example 2
(1) Mixing Nb with 2 Placing C MXene in a tube furnace, heating to 600 deg.C at the rate of 5 deg.C/min, heat treating in air for 8 hr, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) White layered Nb in argon atmosphere containing 8% hydrogen 2 O 5 Heating to 600 deg.C at a rate of 10 deg.C/min, continuously heat treating for 2h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed into a continuous flow type photocatalytic reactor, and a 300W xenon lamp is used as a simulated sunThe light source is used for treating 500ppb NO under the relative humidity of 50%, and the NO removal rate is as high as 58.9%.
Example 3
(1) Mixing Nb with 2 Placing C MXene in a tube furnace, heating to 400 ℃ at the speed of 10 ℃/min, carrying out heat treatment in air for 9h, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) White layered Nb is added in argon atmosphere containing 5% hydrogen 2 O 5 Heating to 600 deg.C at a rate of 10 deg.C/min, continuously heat treating for 3h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly drop-coated onto a 5cm by 10cm test piece. After drying at room temperature, the test piece is placed into a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate is as high as 57.4%.
Example 4
(1) Mixing Nb with 2 Placing C MXene in a tube furnace, heating to 700 deg.C at 3 deg.C/min, heat treating in air for 4 hr, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) White layered Nb in argon atmosphere containing 10% hydrogen 2 O 5 Heating to 700 ℃ at the speed of 5 ℃/min, continuing heat treatment for 2h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed into a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate is as high as 59.3%.
Example 5
(1) Nb to 2 Placing C MXene in a tube furnace, heating to 600 deg.C at 5 deg.C/min, heat treating in air for 5 hr, and cooling to room temperature to obtain white pigmentColor laminated Nb 2 O 5 。
(2) White layered Nb in argon atmosphere containing 10% hydrogen 2 O 5 Heating to 600 deg.C at a rate of 10 deg.C/min, continuously heat treating for 2h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed into a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate is as high as 60.7%.
Example 6
(1) Mixing Nb with 2 Placing C MXene in a tube furnace, heating to 500 deg.C at a rate of 10 deg.C/min, heat treating in air for 6h, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) White layered Nb in argon atmosphere containing 15% hydrogen 2 O 5 Heating to 600 deg.C at a rate of 5 deg.C/min, continuously heat treating for 4h, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of blue Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed in a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate reaches 61.5%.
Comparative example 1
(1) Commercial Nb in an argon atmosphere containing 15% hydrogen 2 O 5 Heating the powder to 600 deg.C at a rate of 5 deg.C/min, continuously heat treating for 2 hr, and cooling to room temperature to obtain powdered Nb 2 O 5 A photocatalyst.
(3) Taking 0.1g of powdered Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly drop-coated onto a 5cm by 10cm test piece. Drying at room temperature, and placing the test pieceAnd (3) putting the mixture into a continuous flow type photocatalytic reactor, treating 500ppb NO at 50% relative humidity by using a 300W xenon lamp as a simulated sunlight source, wherein the NO removal rate is 32.6%.
Comparative example 2
(1) Nb to 2 Placing C MXene in a tube furnace, heating to 500 ℃ at the speed of 5 ℃/min, carrying out heat treatment in air for 4h, and cooling to room temperature to obtain white layered Nb 2 O 5 。
(2) Taking 0.1g of white layered Nb 2 O 5 The photocatalyst was dispersed in 5mL of water to form a suspension, and the suspension was uniformly applied dropwise to a 5cm X10 cm test piece. After drying at room temperature, the test piece is placed into a continuous flow type photocatalytic reactor, a 300W xenon lamp is used as a simulated sunlight source, 500ppb NO is treated under 50% relative humidity, and the NO removal rate is 39.3%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. Blue layered Nb 2 O 5 The application of the photocatalyst in the photocatalytic removal of NO is characterized in that: the blue layered Nb 2 O 5 The preparation method of the photocatalyst comprises the following steps: mixing Nb with 2 C MXene is put in a tube furnace, heated to 400 to 700 ℃, heat-treated in the air for 1 to 10 hours, and cooled to room temperature to obtain white layered Nb 2 O 5 (ii) a Subjecting white layered Nb to reduction atmosphere 2 O 5 Heating to 400 to 700 ℃, continuously performing heat treatment for 1 to 5 hours, and cooling to room temperature to obtain blue layered Nb 2 O 5 A photocatalyst;
the reducing atmosphere is a mixed gas of hydrogen and an inert gas, the inert gas is one of nitrogen, argon and helium, and the volume fraction of the hydrogen in the reducing atmosphere is 2-20%.
2. Use according to claim 1, characterized in that: the heating rate of the two parts is 1 to 20 ℃/min when the temperature is increased to 400 to 700 ℃, and the two parts are naturally cooled when the temperature is reduced to room temperature.
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