CN112007683A - Carbon nitride-based ternary composite photocatalyst with full visible spectrum response and preparation method thereof - Google Patents
Carbon nitride-based ternary composite photocatalyst with full visible spectrum response and preparation method thereof Download PDFInfo
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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Abstract
The invention discloses a carbon nitride-based three-way composite photocatalyst with full visible spectrum response and a preparation method thereof. The preparation method comprises the steps of firstly dispersing polytriazine imine (PTI) nanosheets in an organic alcohol solvent containing aromatic organic matters (Ph) through ultrasonic until the polytriazine imine (PTI) nanosheets are uniformly dispersed, adding cyanamide, heating and stirring in a water bath at 60 ℃ until white precipitates are generated, drying in vacuum to obtain white solid powder, and then carrying out thermal polymerization in an air atmosphere to obtain the carbon nitride based ternary composite photocatalyst PTI/Ph/GCN. The preparation method disclosed by the invention is simple, and the obtained carbon nitride-based ternary composite photocatalyst has a full-spectrum response characteristic in a visible light range (200-800 nm), and has a wide application prospect in the aspects of energy conversion and environmental management.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a carbon nitride-based three-way composite photocatalyst with full visible spectrum response and a preparation method thereof.
Background
In recent years, semiconductor photocatalysts are widely applied to solving the problems of environmental organic pollution and energy crisis due to the 'green' characteristic. Among the existing photocatalysts, the polymeric semiconductor carbon nitride, which is used as a light nonmetal semiconductor, is one of the most promising semiconductor materials due to the advantages of appropriate energy band structure, good stability, easy preparation and the like. However, the carbon nitride material in the prior art generally has only a relatively narrow absorption range of visible spectrum (< 560 nm), which limits the application of the carbon nitride material in the visible light catalysis field.
The carbon nitride has stronger in-plane pi conjugated bonds, and the residual amino groups at the edge of the triazine ring can provide ideal sites for the expansion of a pi conjugated system, so that the absorption range of the carbon nitride on visible light can be expanded by expanding the conjugated system.
At present, there is no report on formation of a ternary composite carbon nitride-based photocatalyst by covalent bonding of polytriazine imine (PTI), graphite-phase carbon nitride (GCN) and an aromatic organic compound (Ph). Therefore, the PTI/Ph/GCN carbon nitride-based ternary composite photocatalyst is formed by using carbon nitride with different crystal phases and performing polycondensation reaction with a p-pi conjugated aromatic compound (Ph) containing lone-pair electrons, so that the spectral response range of the compound can be expanded, the photoelectric response performance of the photocatalyst is improved, and the development and practical application of the photocatalytic technology are further promoted.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a carbon nitride-based three-way composite photocatalyst with full visible spectrum response performance, wherein the response of the catalyst to visible light is expanded to a full visible light region (200-800 nm), and the catalyst has high photoelectric response performance; and the preparation process is simple, the operation is convenient, the industrial production is easy to realize, and the method has wide application prospect in the aspects of energy conversion and environmental management.
The technical scheme of the invention is as follows:
a preparation method of a carbon nitride-based three-way composite photocatalyst with full visible spectrum response comprises the following specific preparation steps:
(1) dispersing polytriazine imine nanosheets in an organic alcohol solution of p-pi conjugated aromatic organic matters containing lone pair electrons, and performing ultrasonic treatment until the dispersion is uniform;
(2) dispersing cyanamide in a certain proportion in the solution obtained in the step (1) and carrying out ultrasonic treatment;
(3) stirring the mixed solution obtained in the step (2) at 60 ℃ until white precipitate is generated in the solution, and then drying in vacuum to obtain white solid powder;
(4) and transferring the white solid powder into a container with a cover, and calcining in a muffle furnace to obtain the carbon nitride based three-way composite photocatalyst PTI/Ph/GCN.
Preferably, the aromatic organic compound in step (1) includes p-phenylenediamine, pyromellitic dianhydride, and p-aminobenzaldehyde.
Preferably, the concentration of the organic alcohol solution of the aromatic organic substance in the step (1) is 0.001 to 0.05 mol.L-1。
Preferably, the mass ratio of the polytriazine imine to the aromatic organic compound in step (1) is 2:1 to 100: 1.
Preferably, in step (1), the organic alcohol includes ethanol, isopropanol and butanol.
Preferably, the mass ratio of the cyanamide to the polytriazine imine in the step (2) is 1: 1-50: 1.
Preferably, the ultrasonic time in the step (1) is 2-8 h; and (3) the ultrasonic time in the step (2) is 1-4 h.
Preferably, in the step (3), the vacuum drying temperature is 60-80 ℃ and the time is 12-24 h.
Preferably, the heating rate is 2-20 ℃/min, the thermal polymerization temperature is 500-650 ℃, and the thermal polymerization constant temperature time is 4-12 h when the calcination is carried out in a muffle furnace.
The carbon nitride based ternary composite photocatalyst prepared by the preparation method of the carbon nitride based ternary composite photocatalyst has the full visible spectrum response performance of 200-800 nm; has photoelectric effect in the range of 400-700 nm.
The invention has the beneficial effects that:
1. the PTI and the GCN are compounded through conjugated aromatic organic matters by utilizing chemical bonds to form the carbon nitride-based ternary composite photocatalytic material, so that the absorption range of the photocatalyst on visible light is expanded, and the obtained carbon nitride-based ternary composite photocatalyst has full-spectrum response characteristics within the visible light range (200-800 nm);
2. the carbon nitride-based ternary composite photocatalyst prepared by the method disclosed by the invention is of a porous sheet structure, has a large specific surface area and a small photon-generated carrier migration path, is beneficial to providing a plurality of reaction active sites and improving the separation efficiency of photon-generated carriers;
3. the prepared carbon nitride-based ternary composite photocatalyst has excellent photoelectric response performance, the instantaneous photocurrents generated in a visible light region are respectively 2.1, 3.8 and 6.7 times of PTI/GCN, GCN and PTI, and the carbon nitride-based ternary composite photocatalyst still has excellent photoelectric response performance particularly under the condition of 700 nm monochromatic light;
4. the preparation process of the ternary composite photocatalyst is simple, the operation is convenient, and the industrial production is easy to realize.
Drawings
FIG. 1 is an optical photograph and FESEM image of PTI/PPD/GCN prepared in example 1;
FIG. 2 is an XRD pattern of PTI/PPD/GCN prepared in example 1 and PTI/GCN, PTI prepared in comparative examples 1-3, respectively, where #: GCN; *: PTI;
FIG. 3 is a UV-Vis DRS plot of PTI/PPD/GCN prepared in example 1 and PTI/GCN, PTI prepared in comparative examples 1-3, respectively;
FIG. 4 is a graph of transient photocurrent for PTI/PPD/GCN prepared in example 1 and PTI/GCN, PTI prepared in comparative examples 1-3, respectively;
FIG. 5 is a graph of the transient photocurrent of the PTI/PPD/GCN prepared in example 1 under monochromatic light irradiation at 700 nm.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
Example 1: preparation of PTI/PPD/GCN carbon nitride based ternary composite photocatalyst
0.1 g of polytriazine imine (PTI) nanosheets dispersed in 10 mL of 0.03 mol.L-1Performing ultrasonic treatment on p-phenylenediamine (PPD) in isopropanol for 4 h, dispersing 5 g of cyanamide in the mixed solution, performing ultrasonic treatment for 2 h, stirring at the constant-temperature water bath condition of 60 ℃ until white solid is generated, and performing vacuum drying at the temperature of 60 ℃ for 24 h to obtain white solid powder. Transferring the white solid powder into a container with a cover, heating to 550 ℃ in a muffle furnace at a speed of 17 ℃/min, and keeping the temperature for 4 hours to prepare the PTI/PPD/GCN carbon nitride based ternary composite photocatalyst.
The field emission scanning electron microscope image of the obtained PTI/PPD/GCN ternary heterogeneous photocatalyst is shown in a small image (b) in fig. 1, and as can be seen from the image, the PTI/PPD/GCN synthesized by the embodiment is of a porous lamellar structure, has a large specific surface area and a small photon-generated carrier migration path, and is helpful for providing a plurality of reaction active sites and enhancing the absorption efficiency of light. The panel (a) in FIG. 1 is an optical photograph of the synthesized PTI/PPD/GCN of this example, which is a brown powdery solid.
Comparative example 1: preparation of PTI/GCN carbon nitride based binary composite photocatalyst
0.1 g of PTI nano sheet is dispersed in 10 mL of isopropanol solution for ultrasonic treatment for 4 h, 5 g of cyanamide is dispersed in the mixed solution for ultrasonic treatment for 2 h, the obtained mixture is stirred in a constant-temperature water bath condition at 60 ℃ until a white solid is generated, and then the white solid powder is obtained after vacuum drying for 24 h at 60 ℃. And transferring the white solid powder into a container with a cover, heating to 550 ℃ in a muffle furnace at the speed of 17 ℃/min, and keeping the temperature for 4 hours to obtain the PTI/GCN carbon nitride based binary composite photocatalyst.
Comparative example 2: preparation of GCN photocatalyst
Placing 5 g of cyanamide in an agate mortar, adding 5 mL of absolute ethyl alcohol, grinding and uniformly mixing, transferring the mixture to a crucible, drying in an oven at 100 ℃ to obtain a precursor of the carbon nitride photocatalyst, heating the precursor to 550 ℃ at a speed of 17 ℃/min in a muffle furnace, and calcining for 2 h to obtain the GCN photocatalyst.
Comparative example 3: preparation of polytriazine imines (PTI)
Weighing 10.0 g of zinc chloride in an agate mortar, adding a small amount of distilled water, grinding uniformly, adding 9.23 g of potassium chloride and 2.0 g of cyanamide, continuously grinding until no particle sense exists, transferring to a 50 mL crucible, heating to 100 ℃ at the speed of 8 ℃/min in a muffle furnace, keeping the temperature for 40 min, heating to 520 ℃ at the speed of 2.1 ℃/min, keeping the temperature for 4 h, and cooling to room temperature at the speed of 1 ℃/min. And taking out a sample, adding a proper amount of distilled water, stirring for dissolving, transferring to a 250 mL beaker, adding water to a scale of 250 mL, heating and stirring until steam comes out, stopping heating, continuing stirring for 3 min, repeatedly washing until the salinity is less than 50 ppm, centrifuging, and drying to obtain the polytriazine imine/zinc oxide (PTI/ZnO) heterostructure. And finally, washing the polytriazine imine/zinc oxide (PTI/ZnO) heterojunction with acid, and washing away ZnO quantum dots to obtain the PTI.
Results of the correlation performance test:
XRD spectra of PTI/PPD/GCN prepared in example 1 and PTI/GCN, GCN and PTI prepared in comparative examples 1 to 3 are shown in FIG. 2, main diffraction peaks of PTI/PPD/GCN synthesized in example 1 correspond to main diffraction peaks of PTI and GCN, and diffraction peaks at 12.1 degrees, 20.9 degrees and 32.3 degrees correspond to (100) plane, (110) plane and (210) plane of PTI. Diffraction peaks at 13.1 ° and 27.1 ° correspond to the (100) plane and the (002) plane of the GCN, respectively.
The UV-vis DRS spectra of PTI/GCN, GCN and PTI prepared in example 1 and PTI/PPD/GCN prepared in comparative examples 1 to 3 are shown in FIG. 3, and the results show that the PTI/PPD/GCN synthesized in example 1 has full visible spectrum (200-800 nm) response.
Transient photocurrents of PTI/PPD/GCN prepared in example 1 and PTI/GCN, GCN and PTI prepared in comparative examples 1 to 3 respectively are shown in FIG. 4, and the PTI/PPD/GCN synthesized in example 1 has excellent photoelectric response performance and shows larger photocurrent densities which are 2.1, 3.8 and 6.7 times of those of PTI/GCN, GCN and PTI under the irradiation of visible light with the wavelength of more than 420 nm.
Transient photocurrents of the PTI/PPD/GCN prepared in example 1 and the PTI/GCN, the GCN and the PTI prepared in comparative examples 1 to 3 respectively under the irradiation of monochromatic light with the wavelength of 700 nm are shown in FIG. 5, and the PTI/PPD/GCN synthesized in example 1 still has certain current density under the irradiation of the monochromatic light with the wavelength of 700 nm, which shows that the PTI/PPD/GCN has good photoelectric response performance at 700 nm.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.
Claims (8)
1. A preparation method of a carbon nitride-based three-way composite photocatalyst with full visible spectrum response is characterized by comprising the following specific preparation steps:
(1) dispersing polytriazine imine nanosheets in an organic alcohol solution of p-pi conjugated aromatic organic matters containing lone pair electrons, and performing ultrasonic treatment until the dispersion is uniform;
(2) dispersing cyanamide in a certain proportion in the solution obtained in the step (1) and carrying out ultrasonic treatment;
(3) stirring the mixed solution obtained in the step (2) at 60 ℃ until white precipitate is generated in the solution, and then drying in vacuum to obtain white solid powder;
(4) and transferring the white solid powder into a container with a cover, and calcining in a muffle furnace to obtain the carbon nitride based three-way composite photocatalyst PTI/Ph/GCN.
2. The method for preparing the carbon nitride-based three-element composite photocatalyst with full visible-spectrum response as claimed in claim 1, wherein the aromatic organic substances in the step (1) comprise p-phenylenediamine, pyromellitic dianhydride and p-aminobenzaldehyde.
3. The preparation method of the carbon nitride-based three-way composite photocatalyst with full visible spectrum response as claimed in claim 1, wherein the concentration of the organic alcohol solution of the aromatic organic substance in the step (1) is 0.001-0.05 mol-L-1。
4. The preparation method of the carbon nitride-based three-way composite photocatalyst with full visible spectrum response as claimed in claim 1, wherein the mass ratio of polytriazine imine to aromatic organic matter in step (1) is 2: 1-100: 1.
5. The method for preparing the carbon nitride-based three-way composite photocatalyst with the full visible light spectral response as claimed in claim 1, wherein in the step (1), the organic alcohol comprises ethanol, isopropanol and butanol.
6. The preparation method of the full visible spectrum response carbon nitride-based three-way composite photocatalyst, as claimed in claim 1, wherein the mass ratio of cyanamide to polytriazine imine used in step (2) is 1: 1-50: 1.
7. The preparation method of the carbon nitride-based three-way composite photocatalyst with full visible spectrum response as claimed in claim 1, wherein the ultrasonic time in the step (1) is 2-8 h; and (3) the ultrasonic time in the step (2) is 1-4 h.
8. The preparation method of the carbon nitride-based three-way composite photocatalyst with full visible spectrum response as claimed in claim 1, wherein in the step (3), the vacuum drying temperature is 60-80 ℃ and the time is 12-24 h.
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| CN114453001A (en) * | 2022-03-10 | 2022-05-10 | 江苏理工学院 | Aromatic ring and cyano co-doped carbon nitride nanosheet and preparation method and application thereof |
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