CN114453001A - Aromatic ring and cyano co-doped carbon nitride nanosheet and preparation method and application thereof - Google Patents
Aromatic ring and cyano co-doped carbon nitride nanosheet and preparation method and application thereof Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
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Abstract
The invention provides an aromatic ring and cyano co-doped carbon nitride nanosheet and a preparation method and application thereof, and the preparation method comprises the following steps: (1) dispersing the nitrogen-rich organic matter in an organic solvent to obtain a dispersion liquid; (2) and (3) uniformly stirring the aromatic compound, and sequentially heating, washing with alcohol and drying to obtain the carbon nitride nanosheet co-doped with the aromatic ring and the cyano group. The present invention obtains conjugated polymers by integrating aromatic compounds into the traditional carbon nitride synthesis route, i.e., by polymerizing nitrogen-rich organics and aromatic compounds by a solvothermal process. The preparation method of the aromatic ring and cyano co-doped carbon nitride nanosheet has the advantages of simplicity, low cost, high photocatalytic efficiency and good stability.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to an aromatic ring and cyano co-doped carbon nitride nanosheet and a preparation method and application thereof.
Background
Under the dual influence of environmental problems and energy crisis, clean energy is widely developed and utilized. The photocatalytic water splitting hydrogen production is one of important means for converting solar energy into clean and available chemical energy, and the search for a high-efficiency, stable and visible light-responsive semiconductor catalyst is always the core problem in the field, namely graphite phase carbon nitride (g-C)3N4) As an excellent semiconductor visible light photocatalyst, the photocatalyst has the characteristics of high efficiency, stability and visible light response, but carbon nitride has the defect of narrow light absorption range, so that the method for improving the visible light absorption range of the carbon nitride is an effective method for improving the photocatalytic performance of the carbon nitride. At present, no report related to a one-step solvothermal preparation method of carbon nitride co-doped with aromatic rings and cyano groups is found.
The patent application number 202010928866.4 discloses a carbon nitride based ternary composite photocatalyst with full visible light spectral response and a preparation method thereof, and the preparation method comprises the steps of firstly dispersing polytriazine imine (PTI) nanosheets in an organic alcohol solvent containing aromatic organic matters (Ph) and carrying out ultrasonic treatment 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, carrying out vacuum drying to obtain white solid powder, and carrying out thermal polymerization in an air atmosphere to prepare the carbon nitride based ternary composite photocatalyst PTI/Ph/GCN. Although this patent also broadens the light absorption range of carbon nitride, the technical solution and the operation principle adopted by the patent are not the same as those of the present application.
Disclosure of Invention
In view of the above, the invention provides an aromatic ring and cyano co-doped carbon nitride nanosheet and a preparation method and application thereof, wherein the absorption of the carbon nitride in a visible light region is increased by enlarging the range of pi-pi conjugation of the carbon nitride, and a large conjugation system is considered firstly, so that a derivative of a benzene ring can be selected, and simultaneously an atom containing lone pair electrons can influence the electronic structure of the carbon nitride, such as amino groups and other groups.
The invention aims to provide a preparation method of an aromatic ring and cyano co-doped carbon nitride nanosheet, which comprises the following preparation steps:
(1) grinding urea uniformly, and dispersing in dimethyl sulfoxide solvent;
(2) adding p-aminobenzaldehyde, stirring uniformly, heating, washing with alcohol, and drying in sequence to obtain the aromatic ring and cyano co-doped carbon nitride nanosheet.
Preferably, the urea in step (1) may be replaced by cyanamide, dicyandiamide or melamine.
Preferably, the dimethyl sulfoxide solvent in step (1) may be replaced with n-octanol, ethylene glycol or dimethylformamide.
Preferably, the para-aminobenzaldehyde in step (2) may be replaced with para-aminobenzaldehyde or para-aminobenzoic acid.
Preferably, the heating temperature in the step (2) is 160-220 ℃.
Preferably, the heating time in step (2) is 12 h.
The second purpose of the invention is to provide an aromatic ring and cyano co-doped carbon nitride nanosheet, which is prepared by the method of any one of claims 1 to 6.
The third purpose of the invention is to provide the application of the carbon nitride nanosheet co-doped with the aromatic ring and the cyano group, and the carbon nitride nanosheet is applied to the field of photocatalysis.
Preferably, the carbon nitride nanosheet is applied to a process for preparing hydrogen by photocatalytic decomposition of water.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method is simple, the raw materials are easy to obtain, the cost is low, and the prepared photocatalyst widens the visible light response range of the carbon nitride, so that the photocatalytic performance is improved;
2. in the photocatalyst prepared by the invention, the visible light response range of the system is widened, and the separation and migration efficiency of photon-generated carriers is further improved, so that the photocatalytic performance is improved;
3. the photocatalyst prepared by the invention has wide selectivity range of aromatic organic matters for widening the visible light response range of a system, and has good controllability and universality.
Drawings
FIG. 1 is a scanning electron micrograph of UCN-PABA-0.002 sample of example 1 of the present invention;
FIG. 2 is an X-ray diffraction (XRD) spectrum of each of the samples in examples 1 to 4 of the present invention and comparative example 1;
FIG. 3 is a graph showing the UV-VIS diffuse reflectance spectrum of each of examples 1 to 4 of the present invention and comparative example 1;
FIG. 4 is a graph of transient photocurrent for each of examples 1 to 4 of the present invention and comparative example 1;
FIG. 5 is a Fourier transform Infrared Spectroscopy (FT-IR) plot of samples of examples 1-4 of the present invention and comparative example 1;
FIG. 6 is a graph showing the hydrogen production performance under irradiation of visible light (. lamda. gtoreq.420 nm) of each of the samples of examples 1 to 4 of the present invention and comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the 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.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the starting materials and auxiliaries are, unless otherwise specified, obtained from customary commercial sources or prepared in customary manner.
Example 1
Weighing 5g of urea, grinding the urea, uniformly dispersing the urea in 30mL of dimethyl sulfoxide, adding 2mg of p-aminobenzaldehyde, fully stirring, placing the mixture in a reaction kettle, heating for reaction at the constant temperature of 200 ℃ for 12 hours, and washing and drying the mixture by alcohol to obtain a product UCN-PABA-0.002.
As shown in fig. 1, the sample UCN-PABA-0.002 is a porous sheet structure, has a slight roll at the edge, has a uniform surface, and has absorption at the visible light position (fig. 3) corresponding to the (100) surface and the (002) surface of the GCN (fig. 2) respectively at 2 θ ═ 12.9 ° and 27.2 °, and a photocatalytic reaction under the irradiation of visible light (a filter with λ ≥ 420nm is mounted on a 300W xenon lamp), with a hydrogen production rate of 18.66 μmol/h.
Example 2
A photocatalyst was prepared according to the method of example 1, except that the amount of PABA doped was 4mg and other conditions were unchanged, and was named UCN-PABA-0.004.
Under the same photocatalytic reaction conditions as in the first example, the hydrogen production rate was 26.26. mu. mol/h.
Example 3
A photocatalyst was prepared according to the procedure of example 1, except that the doping amount of PABA was 6mg and the other conditions were not changed, and was designated UCN-PABA-0.006.
Under the same photocatalytic reaction conditions as in example one, the hydrogen production rate was 30.67. mu. mol/h.
Example 4
A photocatalyst was prepared according to the method of example 1, except that the amount of PABA doped was 8mg and the other conditions were unchanged, and was named UCN-PABA-0.008.
Under the same photocatalytic reaction conditions as in the first example, the hydrogen production rate was 10.30. mu. mol/h.
Comparative example 1
The difference from example 1 is that pure graphite phase carbon nitride is obtained without adding PABA and without changing other conditions.
The results of the effect verification for examples 1 to 4 and comparative example 1 were as follows:
the above examples demonstrate that the addition of PABA improves the photocatalytic hydrogen production efficiency.
From the scanning electron microscope of FIG. 1, it can be seen that UCN-PABA is a lamellar structure.
As can be seen from the XRD pattern of fig. 2, the addition of PABA did not change the structure of the carbon nitride.
From the ultraviolet-visible diffuse reflection spectrogram of FIG. 3, it can be seen that UCN-PABA-0 has almost no absorption to light when the wavelength λ > 500nm, and UCN-PABA-0.006 has strong absorption to light, and still has an absorption intensity of more than 0.2 at 800 nm.
The test result shows that the polymer after PABA is added can completely absorb ultraviolet and visible light, and the absorption intensity is very high, so that the PABA is proved to be added to expand the conjugated system of the carbon nitride and greatly enhance the light absorption range of the pure carbon nitride.
As can be seen from the transient photocurrent diagram of FIG. 4, the photocurrent intensity was maximized when PABA was added in an amount of 6 mg.
From the FT-IR spectrum of FIG. 5, it can be seen that the peak value at 1456cm-1，1562cm-1The two peaks are characteristic peaks of benzene ring, and are at 2160cm-1The peak of (a) is a characteristic peak of a cyano group, indicating that co-doping of an aromatic ring and a cyano group with carbon nitride is achieved.
From the photolysis water performance test chart of fig. 5, it can be seen that the addition of PABA improves the photolysis water hydrogen production performance of carbon nitride.
As can be seen from FIG. 6, there is an optimum amount of PABA added, and the photocatalytic hydrogen production efficiency of UCN-PABA-0.006 is optimum.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The preparation method of the aromatic ring and cyano co-doped carbon nitride nanosheet is characterized by comprising the following preparation steps:
(1) grinding urea uniformly, and dispersing in dimethyl sulfoxide solvent;
(2) adding p-aminobenzaldehyde, stirring uniformly, heating, washing with alcohol, and drying in sequence to obtain the aromatic ring and cyano co-doped carbon nitride nanosheet.
2. The method for preparing carbon nitride nanosheets co-doped with aromatic rings and cyano groups according to claim 1, wherein the urea is replaceable with cyanamide, dicyandiamide or melamine in step (1).
3. The method for preparing an aromatic ring and cyano co-doped carbon nitride nanosheet according to claim 1, wherein the dimethyl sulfoxide solvent in step (1) is replaceable with n-octanol, ethylene glycol or dimethylformamide.
4. The preparation method of aromatic ring and cyano co-doped carbon nitride nanosheet according to claim 1, wherein the p-aminobenzaldehyde in step (2) is replaceable with p-aminobenzaldehyde or p-aminobenzoic acid.
5. The preparation method of aromatic ring and cyano co-doped carbon nitride nanosheet according to claim 1, wherein the heating temperature in step (2) is 160-220 ℃.
6. The method for preparing carbon nitride nanosheets co-doped with aromatic rings and cyano groups according to claim 1, wherein the heating in step (2) is for a period of 12 hours.
7. An aromatic ring and cyano co-doped carbon nitride nanosheet, which is characterized by being prepared by the method of any one of claims 1-6.
8. Use of carbon nitride nanoplates co-doped with aromatic rings and cyano groups according to claim 7 in the field of photocatalysis.
9. The application of the carbon nitride nanosheet co-doped with aromatic ring and cyano group according to claim 8, wherein the carbon nitride nanosheet is applied to photocatalytic decomposition of water to produce hydrogen gas.
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