CN113926443A - Multi-element composite material for visible light catalytic aldehyde removal, preparation method and air purifier - Google Patents
Multi-element composite material for visible light catalytic aldehyde removal, preparation method and air purifier Download PDFInfo
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- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 10
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- 238000013329 compounding Methods 0.000 claims description 3
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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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
Abstract
The invention discloses a multi-component composite material for visible light catalytic aldehyde removal, a preparation method and an air purifier3N4/CuOXTernary complex, ZnO/g-C3N4/CuOXThe photocatalytic nano material can efficiently degrade formaldehyde pollutants in the air, and has the characteristics of good stability and reusability.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a multielement composite material for visible light catalytic aldehyde removal, a preparation method and an air purifier.
Background
Formaldehyde (HCHO) is considered as a main toxic indoor pollutant, directly affects indoor air quality, has a good living environment related to the health of all residents, and needs to be explored and solved more urgently for the indoor formaldehyde pollution problem.
The existing formaldehyde removal method is to combine ZnO and graphite carbon nitride to form a heterojunction structure so as to obtain higher visible light absorption range and electron transfer efficiency. g-C as a non-metallic organic photocatalyst3N4It has been extensively studied for its unique properties, such as narrow energy gap (2.7eV), rapid charge transfer, and many redox active sites. However, in the use of carbon nitride (g-C)3N4) After modification of ZnO, g-C3N4the/ZnO can remove pollutants by using a small amount of visible light, and the degradation efficiency is still low.
Disclosure of Invention
The invention mainly aims to provide a multi-element composite material for visible light catalytic aldehyde removal, a preparation method and an air purifier, and aims to solve the problem that carbon nitride (g-C) is utilized in the prior art3N4) After modification of ZnO, g-C3N4The ZnO can remove pollutants by using a small amount of visible light, and the degradation efficiency is still low.
In order to achieve the aim, the invention provides a multi-element composite material for visible light catalytic aldehyde removal, which comprises ZnO/g-C3N4/CuOXAnd (4) ternary compounding.
In order to achieve the purpose, the invention provides a preparation method of a multi-element composite material for visible light catalytic aldehyde removal, which comprises the following steps:
s20, mixing zinc oxide precursor with g-C3N4Dispersed in CuSO4Heating in water bath to obtain solid product;
s30, washing the solid product, and then drying to obtain ZnO/g-C3N4/CuOXA precursor of (a);
s40, calcining the precursor under vacuum condition to obtain the product ZnO/g-C3N4/CuOX。
Optionally, step S20 is preceded by:
s101a, mixing a urea aqueous solution and a zinc acetate aqueous solution with a solute mass ratio of 1: 2-5 to obtain a solution A;
s102a, placing the solution A in an environment of 120-200 ℃ for hydrothermal reaction for 6-18h, cooling, washing and drying to obtain a zinc oxide precursor.
Alternatively, in step S102a,
the drying temperature is 40-80 ℃, and the drying time is 10-20 h.
Optionally, step S10 further includes:
s101b, calcining a carbon-nitrogen source with the carbon-nitrogen ratio of 1: 2, cooling to room temperature, and grinding to obtain g-C3N4。
Alternatively, in step S101b,
the carbon-nitrogen source comprises one or more of cyanamide, dicyandiamide, melamine and urea; and/or the presence of a gas in the gas,
in the step S102b, in step S102,
during the calcination treatment, the temperature is raised to 500-600 ℃ at the temperature rise rate of 2-10 ℃/min, and then the calcination is carried out for 3-5h at the temperature of 500-600 ℃.
Alternatively, in step S20,
g-C3N4the mass ratio of the ZnO to the ZnO is 1 to (0.1-1) g-C3N4Mass of (2) and Cu2+The mass ratio of (1) to (0.001-0.01); and/or the presence of a gas in the gas,
heating in water bath at 80-100 deg.C under stirring for 0.5-3 hr.
Alternatively, in step S30,
when washing is carried out, the washing times of water washing are 6-10 times; and/or the presence of a gas in the gas,
when the drying treatment is carried out, the drying temperature is 60-100 ℃, and the drying time is 12-24 h.
Alternatively, in step S40,
when the calcination treatment is carried out, the calcination temperature is 300-500 ℃, the calcination time is 2-5h, and the temperature rise rate is 5-15 ℃/min.
The invention further provides an air purifier, which comprises the above-mentioned multi-component composite material for visible light catalytic aldehyde removal, and the preparation method comprises the following steps:
s20, mixing zinc oxide precursor with g-C3N4Dispersed in CuSO4Heating in water bath to obtain solid product;
s30, washing the solid product, and then drying to obtain ZnO/g-C3N4/CuOXA precursor of (a);
s40, calcining the precursor under vacuum condition to obtain the product ZnO/g-C3N4/CuOX。
In the technical scheme of the invention, ZnO/g-C is included3N4/CuOXThe ternary composite multielement composite material for visible light catalytic aldehyde removal has the advantages of higher visible light utilization rate, higher formaldehyde degradation rate in air medium, better stability and reusability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of an embodiment of a method for preparing a multi-component composite material for visible light catalytic aldehyde removal according to the present invention;
FIG. 2 shows ZnO/g-C prepared by the preparation method in FIG. 13N4/CuOXComposite visible light catalytic nano material SEMAn image;
FIG. 3 shows ZnO/g-C prepared by the preparation method in FIG. 13N4/CuOXUltraviolet diffuse reflection spectrogram of the composite visible light catalytic nano material and ZnO;
FIG. 4 shows ZnO/g-C prepared by the preparation method in FIG. 13N4/CuOXComposite visible light catalytic nano material N2Adsorption-desorption isotherm diagram;
FIG. 5 shows ZnO/g-C prepared by the preparation method in FIG. 13N4/CuOXComposite visible light catalytic nano material, ZnO and g-C3N4(ii) a Fourier infrared spectrum;
FIG. 6 shows ZnO/g-C prepared by the preparation method in FIG. 13N4/CuOXA performance contrast diagram of visible light catalysis degradation of formaldehyde by the photocatalytic nanomaterial and the ZnO and g-C3N4 photocatalyst;
FIG. 7 shows ZnO/g-C3N4/CuOXAnd (3) a test result chart of stable photocatalytic performance of the photocatalytic nano material.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that those whose specific conditions are not specified in the examples were performed according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope 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.
Formaldehyde (HCHO) is considered as a main toxic indoor pollutant, directly affects indoor air quality, has a good living environment related to the health of all residents, and needs to be explored and solved more urgently for the indoor formaldehyde pollution problem.
The existing formaldehyde removal method is to combine ZnO and graphite carbon nitride to form a heterojunction structure so as to obtain higher visible light absorption range and electron transfer efficiency. g-C as a non-metallic organic photocatalyst3N4It has been extensively studied for its unique properties, such as narrow energy gap (2.7eV), rapid charge transfer, and many redox active sites. However, in the use of carbon nitride (g-C)3N4) After modification of ZnO, g-C3N4the/ZnO can remove pollutants by using a small amount of visible light, and the degradation efficiency is still low.
In view of the above, the invention provides a preparation method of a multi-component composite material for visible light catalytic aldehyde removal, and aims to prepare the multi-component composite material for visible light catalytic aldehyde removal.
The multielement composite material for visible light catalytic aldehyde removal provided by the invention comprises ZnO/g-C3N4/CuOXAnd (4) ternary compounding.
In the technical scheme of the invention, ZnO/g-C is included3N4/CuOXThe ternary composite multielement composite material for visible light catalytic aldehyde removal has the advantages of higher visible light utilization rate, higher formaldehyde degradation rate in air medium, better stability and reusability.
Referring to fig. 1, the present invention further provides a method for preparing the above-mentioned multicomponent composite material for visible light catalyzed aldehyde removal, comprising the following steps:
s20, mixing zinc oxide precursor with g-C3N4Dispersed in CuSO4Heating in water bath to obtain solid product;
specifically, in step S20, g-C3N4The mass ratio of the ZnO to the ZnO is 1 to (0.1-1) g-C3N4Mass of (2) and Cu2+The mass ratio of the zinc oxide precursor to the zinc oxide precursor is 1 to (0.001-0.01), and the zinc oxide precursor are heated and stirred for 0.5-3h at the temperature of 80-100 ℃ during water bath heating, so that the zinc oxide precursor and the zinc oxide precursor g-C3N4And CuSO4Can fully react.
Specifically, step S20 is preceded by:
s101a, mixing a urea aqueous solution and a zinc acetate aqueous solution with a solute mass ratio of 1: 2-5 to obtain a solution A;
s102a, placing the solution A in an environment of 120-200 ℃ for hydrothermal reaction for 6-18h, cooling, washing and drying to obtain a zinc oxide precursor.
It is noted that the drying temperature is 40-80 ℃, and the drying time is 10-20 h, so that the drying efficiency of the zinc oxide precursor is improved, and the dryness of the zinc oxide precursor is ensured.
Specifically, during washing, the zinc oxide precursor is centrifugally washed for 6-10 times at 8000-10000 rpm, so that the washing is more sufficient, and impurities in the prepared zinc oxide precursor are avoided.
Specifically, step S20 is preceded by:
s101b, calcining a carbon-nitrogen source with the carbon-nitrogen ratio of 1: 2, cooling to room temperature, and grinding to obtain g-C3N4。
Specifically, the carbon-nitrogen source comprises one or more of cyanamide, dicyandiamide, melamine and urea.
Preferably, in step S101b, during the calcination treatment, the temperature is raised to 500-600 ℃ at a rate of 2-10 ℃/min, and then the calcination is carried out for 3-5h at a temperature of 500-600 ℃, so that the improvement is achievedg-C3N4The preparation efficiency of (1).
It should be noted that, preferably, the carbon nitrogen source is selected from dicyandiamide, and when the dicyandiamide is calcined, the dicyandiamide is placed in an alumina crucible with a cover and calcined by a muffle furnace, so that the g-C is improved3N4The preparation efficiency of (1).
S30, washing the solid product, and then drying to obtain ZnO/g-C3N4/CuOXA precursor of (a);
specifically, in step S30, the washing time is 6-10 times during washing, so as to sufficiently wash off impurities in the solid product, and the drying temperature is 60-100 ℃ during drying treatment, and the drying time is 12-24h, so as to sufficiently remove moisture in the solid product, thereby ensuring the dryness of the solid product.
It should be noted that, when performing the drying treatment, the adopted device is an oven, and in other embodiments, the drying device may also be a hot air blower, a dryer, and the like, which is not limited in this application.
S40, calcining the precursor under vacuum condition to obtain the product ZnO/g-C3N4/CuOX。
Specifically, in step S40, during the calcination process, the calcination temperature is 300-.
The preparation method of the multi-component composite material for visible light catalytic aldehyde removal provided by the invention has the advantages that the preparation success rate of the multi-component composite material for visible light catalytic aldehyde removal is obviously improved by controlling the preparation conditions, and the prepared multi-component composite material for visible light catalytic aldehyde removal can efficiently degrade formaldehyde pollutants in the air and has the characteristics of good stability and reusability.
In addition, the air purifier provided by the invention comprises the multi-component composite material for visible light catalytic aldehyde removal, which is prepared by the preparation method of the multi-component composite material for visible light catalytic aldehyde removal, so that the air purifier has all the beneficial effects of the multi-component composite material for visible light catalytic aldehyde removal, and the details are not repeated herein.
An example of the preparation process of the multicomponent composite according to the invention for visible light catalyzed aldehyde removal is given below:
(1) mixing a urea aqueous solution and a zinc acetate aqueous solution with a solute mass ratio of 1: 2-5 to obtain a solution A, placing the solution A in a 120-10000 ℃ environment for hydrothermal reaction for 6-18h, cooling, washing and drying to obtain a zinc oxide precursor, wherein the solution A is centrifugally washed for 6-10 times at 8000-10000 rpm, the drying temperature is 40-80 ℃, and the drying time is 10-20 h; calcining carbon-nitrogen source with carbon-nitrogen ratio of 1: 2, cooling to room temperature, and grinding to obtain g-C3N4The carbon-nitrogen source comprises one or more of cyanamide, dicyandiamide, melamine and urea, and is heated to 500-600 ℃ at a heating rate of 2-10 ℃/min during calcination treatment, and then calcined for 3-5h at 500-600 ℃;
(2) mixing zinc oxide precursor with g-C3N4Dispersed in CuSO4Heating in water bath to obtain solid product, wherein g-C3N4The mass ratio of the zinc oxide precursor to the zinc oxide precursor is 1 to (0.1-1) g-C3N4Mass of (2) and Cu2+The mass ratio of the components is 1 to (0.001-0.01), and the components are heated and stirred for 0.5-3h at the temperature of 80-100 ℃ when heated in a water bath;
(3) washing the solid product, and then drying to obtain ZnO/g-C3N4/CuOXThe precursor is washed by water for 6-10 times, and dried at 60-100 deg.C for 12-24 h;
(4) calcining the precursor under vacuum condition to obtain a product ZnO/g-C3N4/CuOXWhen the calcination treatment is carried out, the calcination temperature is 300-500 ℃, the calcination time is 2-5h, and the temperature rise rate is 5-15 ℃/min.
The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.
Example 1
(1) Mixing a zinc acetate aqueous solution with a solute of 3.596g and a urea aqueous solution with a solute of 0.984g to obtain a solution A, placing the solution A in a 160 ℃ environment for a hydrothermal reaction for 10h, cooling, centrifugally washing for 6 times at 8000rpm, drying at a drying temperature of 40 ℃ for 10h to obtain a zinc oxide precursor, placing 5g of dicyandiamide in an alumina crucible with a cover, heating to 550 ℃ at a heating rate of 5 ℃/min in a muffle furnace, calcining at 550 ℃ for 3h, cooling to room temperature, and grinding to obtain g-C3N4；
(2) 0.4g of zinc oxide precursor and 1g of g-C3N4Dispersed in 50ml of CuSO4In aqueous solution, Cu2+Relative to the mass of g-C3N4The mass of the product is 0.5 wt%, heating in water bath to obtain a solid product, and heating and stirring at 90 ℃ for 1h during heating in water bath;
(3) the solid product was washed 6 times with deionized water and dried in an oven at 70 ℃ for 24 hours to obtain ZnO/g-C3N4/CuOXThe precursor of (1).
(4) Putting the precursor into a muffle furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, and calcining for 5h at 300 ℃ to obtain a product ZnO/g-C3N4/CuOX。
Example 2
(1) Mixing 1g of urea aqueous solution and 2g of zinc acetate aqueous solution to obtain solution A, placing the solution A in an environment of 120 ℃ for hydrothermal reaction for 6h, cooling, centrifugally washing for 10 times at 10000rpm, drying for 20h at a drying temperature of 80 ℃ to obtain a zinc oxide precursor, placing 7g of melamine into an aluminum oxide crucible with a cover, heating to 500 ℃ at a heating rate of 2 ℃/min in a muffle furnace, calcining for 5h at 500 ℃, and grinding after cooling to room temperature to obtain g-C3N4；
(2) 0.1g of zinc oxide precursor and 1g of g-C3N4Dispersed in 60ml of CuSO4In aqueous solution, Cu2+Relative to the mass of g-C3N4The mass of the product is 0.1 wt%, heating in water bath to obtain a solid product, and heating and stirring at 80 ℃ for 0.5h during heating in water bath;
(3) washing the solid product with deionized water for 10 times, and drying in an oven at 60 ℃ for 12 hours to obtain ZnO/g-C3N4/CuOXThe precursor of (1).
(4) Putting the precursor into a muffle furnace, heating to 500 ℃ at a heating rate of 15 ℃/min, and calcining for 2h at 500 ℃ to obtain a product ZnO/g-C3N4/CuOX。
Example 3
(1) Mixing a urea aqueous solution with a solute of 2g and a zinc acetate aqueous solution with a solute of 10g to obtain a solution A, placing the solution A in a 200 ℃ environment for hydrothermal reaction for 18h, cooling, centrifugally washing for 8 times at 9000rpm, drying for 15h at a drying temperature of 60 ℃ to obtain a zinc oxide precursor, placing 6.5g of urea in an alumina crucible with a cover, heating to 600 ℃ in a muffle furnace at a heating rate of 10 ℃/min, calcining for 4h at 600 ℃, and grinding after cooling to room temperature to obtain g-C3N4；
(2) 2g of zinc oxide precursor and 2g of g-C3N4Dispersed in 70ml of CuSO4In aqueous solution, Cu2+Relative to the mass of g-C3N4The mass of the product is 1 wt%, heating in water bath to obtain a solid product, and heating and stirring for 3 hours at 100 ℃ during heating in water bath;
(3) the solid product was washed 8 times with deionized water and dried in an oven at 100 ℃ for 18 hours to give ZnO/g-C3N4/CuOXThe precursor of (1).
(4) Putting the precursor into a muffle furnace, heating to 400 ℃ at a heating rate of 10 ℃/min, and calcining for 3.5h at 400 ℃ to obtain a product ZnO/g-C3N4/CuOX。
Example 4
(1) Mixing 1g of urea aqueous solution and 3g of zinc acetate aqueous solution to obtain solution A, placing the solution A in an environment with the temperature of 170 ℃ for hydrothermal reaction for 12h, cooling, centrifugally washing for 7 times at 8500rpm, drying for 14h at the drying temperature of 50 ℃ to obtain a zinc oxide precursor, mixing 8.5g of cyanamide and dicyandiamide, placing the mixture in an alumina crucible with a cover, heating to 580 ℃ at the heating rate of 6 ℃/min in a muffle furnace, calcining for 3.5h at the temperature of 580 ℃, cooling to room temperature, and grinding to obtain g-C3N4；
(2) 0.5g of zinc oxide precursor and 1g of g-C3N4Dispersed in 35ml of CuSO4In aqueous solution, Cu2+Relative to the mass of g-C3N4The mass of the product is 0.55 wt%, heating in water bath to obtain a solid product, and heating and stirring at 85 ℃ for 2h during heating in water bath;
(3) the solid product was washed 9 times with deionized water and dried in an oven at 75 ℃ for 20 hours to give ZnO/g-C3N4/CuOXThe precursor of (1).
(4) Putting the precursor into a muffle furnace, heating to 450 ℃ at a heating rate of 8 ℃/min, and calcining for 4.5h at 450 ℃ to obtain a product ZnO/g-C3N4/CuOX。
ZnO/g-C prepared for the inventive example3N4/CuOXSEM test of the composite visible light catalytic nano material, and FIG. 2 shows ZnO/g-C prepared in example 13N4/CuOXSEM image of composite visible light catalytic nano material, and ZnO/g-C is shown in figure 23N4/CuOXThe materials are in the form of sheets stacked on top of each other.
FIG. 3 shows ZnO and ZnO/g-C prepared in example 13N4/CuOXUltraviolet diffuse reflection spectrogram of the composite visible light catalytic nano material. As shown in the figure, the light absorption edge of the ZnO photocatalyst is about 380nm, namely, the zinc oxide only responds to ultraviolet light, and the composite material ZnO/g-C3N4/CuOXIn (1),due to CuOXThe doping has stronger light absorption edge, the light absorption edge is stronger, and the obvious light absorption extends to the full visible spectrum, ZnO/g-C3N4/CuOXThe absorption peak of visible light demonstrates the successful synthesis of the composite.
FIG. 4 shows ZnO/g-C in example of the present invention3N4/CuOXN of (A)2Adsorption-desorption isotherm diagram, the specific surface area of the composite material is 48.2m2The/g shows that the formaldehyde adsorption performance is weak, and the degradation is mainly caused by the reaction of persistent free radicals generated by photocatalysis on formaldehyde.
FIG. 5 shows ZnO and g-C3N4And ZnO/g-C prepared in example 13N4/CuOXA fourier infrared spectrum of (a). To study the composition and structure of the post-synthesis samples, FTIR analysis was used, as shown in FIG. 5, at 3500cm for ZnO-1Has a strong broadband absorption peak at 442cm-1Is a Zn-O bond stretching vibration absorption peak; for g-C3N4At 810cm-1，1150-1700cm-1，3100-3300cm-1A strong absorption band appears. It is worth mentioning that pure ZnO and g-C3N4The main typical absorption peaks of (A) are all present in ZnO/g-C3N4/CuOXIn the sample, this further indicates ZnO/g-C3N4/CuOXSuccessful synthesis of the composite catalyst. Due to CuOXIs less doped, CuO is not observed in Fourier infrared spectrumXA distinct functional group.
Application example 1
(1) In a 1.5L quartz photocatalytic reactor, formaldehyde was removed photocatalytically with a 5W fan under visible light irradiation at room temperature. A350W xenon lamp was placed vertically outside the photoreactor. The ultraviolet rays were removed using an ultraviolet cut filter (420 nm). The average light intensity of the surface of the reaction solution in the reaction solution measured by a photon densitometer was 200mW/cm2I.e., 2 standard solar intensities (AM3G), 0.1g ZnO/g-C3N4/CuOXThe photocatalytic nanomaterial and 15ml of deionized water were sonicated in a petri dish (7.0 cm diameter) for 25min to form a suspension. The culture dishDried under vacuum at 60 ℃ for 1h and formed a uniform photocatalyst film on the bottom of the dish.
(2) The petri dish was placed in a photocatalytic reactor. A certain amount of 38% aqueous formaldehyde was injected into the reactor, and the initial concentration of HCHO evaporated after reaching adsorption-desorption equilibrium in the dark was 100 ppm. Formaldehyde, CO in the reactor during irradiation2And H2The O concentration was monitored on-line by a photoacoustic infrared multi-gas monitor (inova Air Tech 95 Instruments model 1412). The formaldehyde removal rate (Y) was calculated as Y (%) ═ 1-C/C0) X 100% where C and C0The concentrations of formaldehyde at 0min and t min, respectively.
(3) After the first degradation reaction is finished, drying the culture dish containing the photocatalyst at 60 ℃ for 0.5 hour, then putting the culture dish into the reactor again for the next formaldehyde removal reaction, wherein the reaction conditions except materials are consistent with those of the first time; and after the second reaction is finished, repeating the steps and carrying out a third degradation experiment.
The detection result shows that under the irradiation of 2 standard sunlight intensity visible lights (lambda is more than 400nm), the adding amount of the catalyst is 0.1g, the initial concentration of formaldehyde is 100ppm, and the initial temperature is room temperature, ZnO/g-C3N4/CuOXThe degradation efficiency of the photocatalytic nano material to formaldehyde after 180min is up to 96.5%.
It is noted that the air pollutants include, but are not limited to, formaldehyde, SO2Ammonia gas, NO-XAnd the like. Preferably, the ZnO/C of the invention3N4/CuOXUnder the photocatalysis condition, the catalyst has an especially excellent degradation effect on formaldehyde. Formaldehyde is firstly adsorbed on ZnO/C3N4/CuOXSurface of (2) when the visible light excites ZnO/C3N4/CuOXThen, electrons are driven from C3N4The conduction band of (A) is transferred to the conduction band of ZnO, and the hole is left in C3N4In the valence band, at the same time CuOx on ZnO has high redox reversibility between Cu (II) and Cu (I), the separation of holes and electrons is greatly promoted, formaldehyde is easily oxidized by surface active oxygen or hydroxyl, and finally water and di-water are generatedAnd (3) oxidizing the carbon.
FIG. 6 shows ZnO/g-C prepared in example 13N4/CuOXPhotocatalytic nano material and ZnO and g-C3N4A performance contrast diagram of the photocatalyst for degrading formaldehyde by visible light catalysis. It can be seen that since ZnO does not absorb visible light, formaldehyde hardly degrades after 180min of illumination, while g-C3N4The nano particles can only be removed by about 20 percent at 180min, and ZnO/g-C3N4/CuOXThe degradation efficiency of the photocatalytic nano material to formaldehyde is up to 96.5 percent within 180 min.
FIG. 7 shows ZnO/g-C3N4/CuOXThe photocatalytic nanomaterial has stable photocatalytic performance. After the first degradation reaction is finished, drying the culture dish containing the photocatalyst at 60 ℃ for 0.5 hour, then putting the culture dish into the reactor again for the next formaldehyde removal reaction, wherein the reaction conditions except materials are consistent with those of the first time; and after the second reaction is finished, repeating the steps and carrying out a third degradation experiment. The formaldehyde degradation efficiency in three successive degradation experiments is over 90 percent, which shows that ZnO/g-C3N4/CuOXThe photocatalytic activity of the photocatalytic nanomaterial remains good after three cycles.
Application example 2
The procedure was as in application example 1, except that ZnO/g-C was added3N4/CuOXThe adding amount of the photocatalytic nano material is replaced by 0.5 g/L.
The detection result shows that after the illumination is carried out for 180min, the formaldehyde degradation efficiency is over 90 percent in three continuous degradation experiments.
Application example 3
The procedure was as in application example 1, except that ZnO/g-C was added3N4/CuOXThe adding amount of the photocatalytic nano material is replaced by 2 g/L.
The detection result shows that after the illumination is carried out for 180min, the formaldehyde degradation efficiency is over 90 percent in three continuous degradation experiments.
Comparative example 1
Step (a) andthe same applies to example 1, except that ZnO/g-C is added3N4/CuOXThe photocatalytic nanomaterial is replaced by ZnO.
The detection result shows that after the illumination is carried out for 180min, the formaldehyde is hardly degraded in three continuous degradation experiments.
Comparative example 2
The procedure was as in application example 1, except that ZnO/g-C was added3N4/CuOXReplacement of photocatalytic nanomaterial to g-C3N4And (3) nanoparticles.
The detection result shows that after the illumination is carried out for 180min, about 20 percent of formaldehyde is removed in three continuous degradation experiments.
As can be seen from the comparison of the above application examples 1 to 3 with the comparative examples 1 to 2, the ZnO photocatalyst hardly degraded formaldehyde after 180min of light irradiation, g-C3N4The nano particles remove about 20 percent of formaldehyde after being illuminated for 180min, and the ZnO/g-C prepared by the embodiment of the invention3N4/CuOXThe degradation efficiency of the photocatalytic nano material to formaldehyde after 180min is up to 96.5%.
As can be seen from the comparison of application example 1 with application example 3, the ZnO/g-C prepared by the examples of the present invention3N4/CuOXThe photocatalytic nano material has good stability, higher visible light utilization rate, higher formaldehyde degradation rate in air medium, better stability and reusability.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (10)
1. The multielement composite material for visible light catalytic aldehyde removal is characterized by comprising ZnO/g-C3N4/CuOXAnd (4) ternary compounding.
2. The preparation method of the multielement composite material for visible light catalytic aldehyde removal is characterized by comprising the following steps:
s20, mixing zinc oxide precursor with g-C3N4Dispersed in CuSO4Heating in water bath to obtain solid product;
s30, washing the solid product, and then drying to obtain ZnO/g-C3N4/CuOXA precursor of (a);
s40, calcining the precursor under vacuum condition to obtain the product ZnO/g-C3N4/CuOX。
3. The method for preparing the multi-component composite material for visible light catalytic aldehyde removal according to claim 2, wherein step S20 is preceded by the steps of:
s101a, mixing the solute with the mass ratio of 1: (2-5) mixing the urea aqueous solution and the zinc acetate aqueous solution to obtain a solution A,
s102a, placing the solution A in an environment of 120-200 ℃ for hydrothermal reaction for 6-18h, cooling, washing and drying to obtain a zinc oxide precursor.
4. The method of claim 3, wherein in step S102a,
the drying temperature is 40 ℃ and 480 ℃, and the drying time is 10420 h.
5. The method for preparing the multi-component composite material for visible light catalytic aldehyde removal according to claim 2, wherein step S20 is preceded by the steps of:
s101b, adjusting the carbon-nitrogen ratio to be 1: 2, calcining the carbon-nitrogen source, cooling to room temperature, and grinding to obtain g-C3N4。
6. The method of claim 5, wherein in step S101b,
the carbon-nitrogen source comprises one or more of cyanamide, dicyandiamide, melamine and urea; and/or the presence of a gas in the gas,
during the calcination treatment, the temperature is raised to 5004600 ℃ at the temperature raising rate of 2-10 ℃/m/n, and then the calcination is carried out for 3-5h under the temperature condition of 5004600 ℃.
7. The method for preparing the multi-component composite material for visible light catalyzed aldehyde removal according to claim 2, wherein, in step S20,
g-C3N4the mass ratio of the ZnO to the ZnO is 1: (0.1-1), g-C3N4Mass of (2) and Cu2+The mass ratio of (1) to (0.001-0.01); and/or the presence of a gas in the gas,
heating in water bath at 80-100 deg.C under stirring for 0.5-3 hr.
8. The method for preparing the multi-component composite material for visible light catalyzed aldehyde removal according to claim 2, wherein, in step S30,
when washing is carried out, the washing times of water washing are 6-10 times; and/or the presence of a gas in the gas,
when the drying treatment is carried out, the drying temperature is 60-100 ℃, and the drying time is 12-24 h.
9. The method for preparing the multi-component composite material for visible light catalyzed aldehyde removal according to claim 2, wherein, in step S40,
when the calcination treatment is carried out, the calcination temperature is 300-500 ℃, the calcination time is 2-5h, and the temperature rise rate is 5-15 ℃/m/n.
10. An air cleaner, characterized by comprising the multi-component composite material for visible light catalytic aldehyde removal prepared by the method for preparing the multi-component composite material for visible light catalytic aldehyde removal according to any one of claims 2 to 9.
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