CN110787821A - Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with burr-like structure and preparation method and application thereof - Google Patents
Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with burr-like structure and preparation method and application thereof Download PDFInfo
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- CN110787821A CN110787821A CN201910854312.1A CN201910854312A CN110787821A CN 110787821 A CN110787821 A CN 110787821A CN 201910854312 A CN201910854312 A CN 201910854312A CN 110787821 A CN110787821 A CN 110787821A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 92
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 80
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 63
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 46
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- 238000000034 method Methods 0.000 claims abstract description 38
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
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- 238000009826 distribution Methods 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
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- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 description 2
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- FIULVSVIAAKQJG-UHFFFAOYSA-N C(C(=C)C)(=O)O.C(CC)[K] Chemical compound C(C(=C)C)(=O)O.C(CC)[K] FIULVSVIAAKQJG-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910015667 MoO4 Inorganic materials 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
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- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a preparation method of a graphite phase nitrogen carbide/cadmium sulfide photocatalytic nano composite material with a burr spherical structure, which comprises the following steps: s1: the urea is subjected to thermal polycondensation to obtain graphite-phase nitrogen carbide; s2: adding graphite phase nitrogen carbide and cadmium sulfide precursors with the mass percent of 0-4 wt% into a proper amount of ethylene glycol, uniformly stirring and dispersing by ultrasound to obtain precursor reaction liquid; s3: and (3) rapidly synthesizing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure by the precursor reaction solution through a microwave-assisted heating method. The graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure, which is prepared by the invention, has the advantages of high-efficiency hydrogen production, low price, easy obtainment, environment friendliness and the like, and has great potential in the field of industrialization of hydrogen production by photolysis.
Description
Technical Field
The invention belongs to the field of photocatalytic nano materials, and particularly relates to a graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nano composite material with a burr spherical structure, a preparation method and application thereof.
Background
The generation of clean hydrogen energy by solar catalytic water cracking is considered to be one of the most promising strategies to solve global energy dilemma and environmental problems. To date, many semiconductors have been developed as potential candidates for this targeted photocatalytic reaction, such as metal oxides, metal sulfides, metal oxynitrides, and the like. However, most semiconductors such as TiO2，SrTiO3ZnS, etc. can only respond to approximately 4% of the ultraviolet radiation of solar energy. Therefore, it is still a great challenge to develop a photocatalyst that can effectively utilize solar energy and be practically applied.
Metal sulfide semiconductors have proven to be good candidates for visible light catalyzed hydrogen production due to appropriate band gap and catalytic properties. In particular, CdS with a band gap of 2.4eV has attracted much attention as the most promising photocatalyst because it can absorb visible light widely, is low in cost, and has an appropriate band edge potential. However, the problem with the CdS only material is that photo-generated charges quickly recombine and photo-etching is severe. To overcome these disadvantages, various strategies have been applied to construct various metal sulfides, surface modification, and semiconductor synthesis; research has shown that surface modification with a cocatalyst is an effective method for regulating and controlling the migration path of photogenerated charge carriers and reducing the activation barrier of redox reactions. For example:
CN103316693A discloses a preparation method of photocatalyst Cd/CdS containing a catalyst promoter Cd. According to the method, metal simple substance Cd is introduced into CdS as a cocatalyst, photo-generated electron and hole pairs can be effectively separated, the hydrogen production efficiency of the CdS through photocatalysis is greatly improved, and the application of the CdS in hydrogen production reaction through photocatalytic water decomposition is expanded; the efficient photocatalytic Cd/CdS is directly synthesized by adopting photochemistry, has relatively stable structure and performance, and can be recycled in the photocatalytic decomposition hydrogen production reaction. The method is simple, low in cost, high in yield and good in industrialization prospect.
CN103920505A discloses a visible light photocatalytic high-efficiency hydrogen production cadmium sulfide inverse opal structure and a preparation method thereof. The method is characterized in that polystyrene-methyl methacrylate-3-sulfoacid propyl potassium methacrylate template pellets are used as a template, cadmium sulfide nanocrystals are used as fillers, and the template pellets are prepared by deposition and calcination. The method has the advantages that the synthesis condition of the cadmium sulfide inverse opal structure is simple, the cost is low, the repeatability is high, the prepared sample is complete in shape, the inverse opal structure has remarkable advantages in the aspect of photolysis water to produce hydrogen, and the method has wide and potential energy application prospects.
CN104607231A discloses a carbon nitride photocatalyst with a three-dimensional ordered macroporous structure and a preparation method thereof. The carbon nitride photocatalyst has a regularly arranged three-dimensional ordered porous morphology, a macroporous cavity is spherical, and the diameter of the macroporous cavity is 100 nm-300 nm; the distance between two adjacent macroporous sphere centers is 110 nm-350 nm. The scanning electron microscope picture of the carbon nitride photocatalyst shows that the carbon nitride photocatalyst has a three-dimensional ordered macroporous structure, a macroporous cavity is spherical, and the diameter of the macroporous cavity is 100 nm-300 nm; the macroporous structure has a higher specific surface area, and other materials can be loaded in the cavity of the ordered macropores, the mass transfer is easy, and the photo-generated carriers can be quickly separated in the reaction. The structure of the carbon nitride photocatalyst obviously improves the photocatalytic performance of the catalyst, has higher performance of photolyzing water to produce hydrogen under visible light, and realizes efficient solar energy hydrolysis to produce hydrogen.
CN105772041A discloses a photocatalytic hydrogen production promoter, a photocatalytic system and a method for producing hydrogen. The cocatalyst is CoP and Co2P、Fe2P、FeP、Cu3One or a mixture of more than two of P, ZnP, MoP and MnP. Also discloses a photocatalytic system containing the photocatalytic hydrogen production promoter, which comprises: a semiconductor,Cocatalyst, electron sacrificial agent and water. The method has the advantages of extremely high hydrogen production efficiency of the photocatalytic system, no need of adding a surface stabilizer, low cost, no need of degassing and more benefit for practical application.
CN107282075A discloses a preparation method of a composite photocatalyst of bismuth molybdate and cadmium sulfide. The bismuth molybdate and cadmium sulfide composite photocatalyst prepared by the method has a large-area contact interface, is beneficial to carrier separation, has stable structures and band gap matching, improves photocatalytic activity, has stable catalytic effect, and has excellent performance of photolyzing water to produce hydrogen, photodegrading organic pollutants, heavy metal ions and reducing carbon dioxide. The method has the advantages of common raw materials, simple preparation operation flow, easy realization of process parameters, low cost, simple and convenient operation, high yield and long cycle service life, and has wide application prospect and industrialization prospect in the fields of hydrogen production by photolysis of water, organic pollutant photodegradation, reduction of heavy metal ions and carbon dioxide and the like.
CN109201115A discloses a photocatalytic hydrogen production catalyst with HKUST-1 as a precursor, a preparation method and application thereof. The preparation method comprises the steps of firstly preparing HKUST-1; heating the prepared HKUST-1 to 300-; the method for decomposing water to produce hydrogen by using the photocatalytic hydrogen production catalyst comprises the steps of dispersing the photocatalyst in a mixed solution of water and a sacrificial reagent, removing air in a reaction system, and reacting for 4-8 hours under visible light, wherein the wavelength range of the visible light is 420-700 nm. The photocatalytic hydrogen production catalyst provided by the method can generate hydrogen under the visible light condition at normal temperature and normal pressure, and has the characteristics of high catalytic activity and good hydrogen production stability; and the catalyst has wide raw material source, low price and simple preparation method, and is suitable for large-scale production.
CN109999886A discloses a titanium dioxide/graphite phase carbon nitride Z-shaped heterojunction photocatalytic hydrogen production catalyst, a preparation method and application thereof. According to the method, the existence of the Z-shaped heterojunction enables the photocatalyst to have a wider light absorption range, so that more photo-generated electron-hole pairs can be generated; secondly, the existence of the Z-shaped heterojunction leads the photocatalyst to have better separation efficiency and transport efficiency of electron hole pairs; thereby obviously improving the efficiency of the catalytic photolysis of the hydrogen. The preparation method of the catalyst is simple, and the compounding of the titanium dioxide and the graphite phase carbon nitride is realized by adopting a solution-assisted assembly mode, so that the titanium dioxide and the graphite phase carbon nitride in the prepared catalyst have stronger interaction, and the catalyst is favorable for charge separation and transportation, thereby further improving the catalytic activity of the catalyst.
CN104959153A discloses a novel photocatalytic hydrogen production auxiliary agent, which is nano layered NiMoS, and a photocatalyst with a CdS @ NiMoS spiral structure is formed by modifying a one-dimensional rod-shaped CdS main catalyst. The preparation method of the photocatalyst realizes the synthesis of the spiral composite nano photocatalyst by a two-step hydrothermal technology, firstly CdS nano rods with uniform size and regular appearance are synthesized in an ethylenediamine system, and then Na nano rods are subjected to hydrothermal pressurization2MoO4、Ni(NO3)2Reacting with thiourea to synthesize corresponding layered sulfide NiMoS, and forming heterostructure CdS @ NiMoS with nano-rod-shaped CdS. The catalyst shows excellent photocatalytic hydrogen production performance, and the yield of the seawater hydrogen production can reach 19.147 mmol/g-1·h-1And a new catalyst research and development idea is provided for new energy development.
However, none of the substances prepared in the above methods has realized a catalyst morphology of a burred spherical structure, so that the specific surface area thereof is insufficient, and the reaction efficiency with water in the photocatalytic reaction is affected, and thus there is a need for improvement.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention aims to provide the preparation method of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr-shaped structure, the method has the technical effects of simplicity, rapidness, greenness and low cost, and the synthesized graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material has good hydrogen production performance.
In order to achieve the above object, a first technical solution of the present invention is to provide a method for preparing a graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burred spherical structure, comprising the following steps:
s1: the urea is subjected to thermal polycondensation to obtain graphite-phase nitrogen carbide;
s2: adding graphite phase nitrogen carbide and cadmium sulfide precursors with the mass percent of 0-4 wt% into a proper amount of ethylene glycol, uniformly stirring and dispersing by ultrasound to obtain precursor reaction liquid;
s3: and (3) rapidly synthesizing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure by the precursor reaction solution through a microwave-assisted heating method.
In the method for preparing the burr-spherical-structure graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material, in step S1, the graphite-phase nitrogen carbide is obtained by calcining urea at 550 ℃ for 3 hours.
In the method for preparing the burr-spherical-structure graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material, in step S1, the graphite-phase nitrogen carbide is g-phase graphite-phase nitrogen carbide (g-C)3N4)。
In the preparation method of the burr-spherical-structure graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material, in step S2, the mass percentage ratio of the graphite-phase nitrogen carbide to the cadmium sulfide precursor is 0.5 wt%.
In the preparation method of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure, in step S3, the microwave-assisted heating method is a synthesis method which is simple and convenient to operate and rapid in reaction.
In the preparation method of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure, the step S3 is specifically as follows:
s3-1: heating the precursor reaction solution obtained in the step S2 from room temperature to 90 ℃ under the microwave power of 200W, and keeping the temperature for 10 minutes to obtain a first reaction solution;
s3-2: continuously heating the first reaction solution to 160 ℃, and keeping the temperature for 10 minutes to obtain a second reaction solution;
s3-3: naturally cooling the second reaction solution to room temperature, centrifuging at the centrifugal speed of 18000rpm for 5 minutes, dispersing the obtained precipitate with absolute ethanol and high-purity water successively, centrifuging for 3-5 times, and vacuum drying at 60 ℃ for 8 hours to obtain the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite with the burr spherical structure, wherein the name of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite is CN 0.5.
The inventor finds that when the preparation method is adopted, the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nano composite material with the burr spherical structure can be obtained, and when certain process parameters such as raw material dosage ratio, microwave power, constant temperature time and the like are changed, the photocatalytic composite material with the shape can not be obtained.
In a second aspect, the present invention relates to a graphite phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burr spherical structure obtained by the above preparation method.
The inventor finds that the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure has excellent photocatalytic performance, so that the composite material can be applied to the technical field of photolysis hydrogen production, and has good application prospect and industrialization potential.
Thus, in a third aspect, the present invention relates to the use of the burred-spheroidal structured graphitic-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material for photolytic hydrogen production.
The method is further characterized in that: adding ultrapure water into a photocatalytic nano composite material, dispersing the photocatalytic nano composite material by using ultrasound, adding lactic acid after the ultrapure water is completely dissolved, uniformly mixing, transferring the reaction liquid into a reactor, introducing inert gas after vacuum deoxygenation, using a simulated sunlight xenon lamp as a light source, filtering stray light by using an optical filter below 420nm, and finally detecting the generated H by using gas chromatography2。
In the photolytic hydrogen production method, the mass-to-volume ratio of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure to water is 1:2.05mg/ml, and the mass-to-volume ratio of the nanocomposite material to lactic acid is 1:0.23 mg/ml.
The inventor finds that the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure and the specific morphology, which is obtained by the invention, can be used for preparing hydrogen by photolysis of water under the illumination condition, has a very excellent hydrogen production rate, provides a brand-new and efficient photolysis composite material for hydrogen production by photolysis, and has great application potential and industrial value in the industrial field.
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 introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 shows g-C obtained in example 1 of the present invention3N4Low power SEM image (i.e., fig. 1(a)) and TEM image (i.e., fig. 1(b)) of the sample;
FIG. 2 is a low power SEM photograph (i.e., FIG. 2(a)), TEM photograph (i.e., inset of FIG. 2(a)), and HR-TEM photograph (i.e., FIG. 2(b)) of a sample prepared in example 1 of the present invention;
FIG. 3 shows the g-C values of different mass percentages obtained in example 1 of the present invention3N4Low magnification SEM image of/CdS sample, wherein (a) CN0, (b) CN0.25, (c) CN0.5, (d) CN0.75, (e) CN1, (f) CN2, (g) CN3, (h) CN 4;
FIG. 4 shows g-C obtained in example 1 of the present invention3N4(4 wt%)/CdS heterojunction samples STEM-HAADF and EDX plots;
FIG. 5 shows g-C obtained in example 1 of the present invention3N4(i.e., FIG. 5(a)) and different mass percentages of g-C3N4XRD pattern of/CdS sample (i.e. FIG. 5 (b));
FIG. 6 shows g-C obtained in example 1 of the present invention3N4(8 wt%)/CdS nanocomposite with high resolution XPS spectra, wherein (a) C1S, (b) N1S, (C) S2 p, (d) Cd 3d, and (e) XPS holo-spectrumA spectrum;
FIG. 7 shows the g-C values obtained in example 1 of the present invention in different mass percentages3N4UV-visible absorption spectrum of/CdS sample, in which BaSO4Absorption as a blank;
FIG. 8 shows the g-C values obtained in example 1 of the present invention in different mass percentages3N4Nitrogen adsorption-desorption isotherms and corresponding pore size distributions for the/CdS samples (inset);
FIG. 9 shows g-C obtained in example 1 of the present invention3N4And g-C of different mass percentages3N4I-t curves for CdS samples, where (a) CdS (b) CN0.5(C) CN1(d) CN2 and (e) g-C3N4；
FIG. 10 shows the g-C values obtained in example 1 of the present invention in different mass percentages3N4The hydrogen production efficiency of the water by photocatalytic cracking of the/CdS sample is shown in the figure.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1
S1: urea is subjected to thermal polycondensation to obtain carbonitride;
s2: adding graphite phase nitrogen carbide and cadmium sulfide precursors with the mass percent ratio of 0.50 wt% into a proper amount of ethylene glycol, uniformly stirring and ultrasonically dispersing to obtain precursor reaction liquid;
s3: rapidly synthesizing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure by the precursor reaction solution through a microwave-assisted heating method, which comprises the following steps:
s3-1: heating the precursor reaction solution obtained in the step S2 from room temperature to 90 ℃ under the microwave power of 200W, and keeping the temperature for 10 minutes to obtain a first reaction solution;
s3-2: continuously heating the first reaction solution to 160 ℃, and keeping the temperature for 10 minutes to obtain a second reaction solution;
s3-3: naturally cooling the second reaction solution to room temperature, centrifuging at the centrifugal speed of 18000rpm for 5 minutes, dispersing the obtained precipitate with absolute ethanol and high-purity water successively, centrifuging for 3-5 times, and vacuum drying at 60 ℃ for 8 hours to obtain the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite with the burr spherical structure, wherein the name of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite is CN 0.5.
Examples 2 to 9: examination of raw material dosage ratio
Graphite phase nitrogen carbide (g-C) with different mass ratios shown in Table 1 below was used except in step S13N4) And cadmium sulfide precursor (CdS), the same procedure was followed as in example 1 to carry out examples 2 to 9, using the raw material ratios and composite material designations as given in table 1 below.
TABLE 1 composite materials prepared with different raw material ratios
Microscopic characterization
The graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure obtained in example 1 was subjected to microscopic characterization by a plurality of different means, and the results were as follows:
1. as can be seen from the low-power Scanning Electron Microscope (SEM) image of fig. 1(a), the graphite phase carbon nitride has a lamellar stacking structure and a graphene-like structure, and the structure is formed by stacking and agglomerating a plurality of thin layers. As can be seen from the Transmission Electron Micrograph (TEM) of FIG. 1(b), the graphite-phase carbonitride compound had a distinct lamellar structure, which is consistent with that shown by the scanning electron microscope of FIG. 1 (a).
2. As can be seen from the Scanning Electron Microscope (SEM) of fig. 2(a), it is a burr-like spherical structure, the particle size is about 200 to 300nm, the particle size is uniform, the particle surface has needle-like protrusions, the length and width are about several tens of nanometers different, and the distribution is uniform; FIG. 2(a) is an inset showing the morphology observed by Transmission Electron Microscopy (TEM) with surface acicular protrusions observed as lattice fringes. FIG. 2(b) shows that the lattice spacing was measured to be 0.316nm, corresponding to the (101) crystal plane of the CdS material. The burr spherical structure provides larger specific surface area and more catalytic active sites for photocatalysis, thereby improving the photocatalytic performance.
3. As can be seen from a Scanning Electron Microscope (SEM) image in FIG. 3, the loading morphologies (burr-like spherical structures) with different contents have no obvious difference, are good and are uniformly dispersed. To further prove that carbon-nitrogen compounds are indeed coated on the outer layer, an element distribution test is required.
4. As can be seen from the energy spectrum (EDX) of fig. 4, we can more intuitively obtain the types of elements contained in the sample and their distribution, and as can be seen from the lower part of fig. 4, the sample contains four elements, i.e., S, Cd, C, and N, the content of S, Cd element accounts for a larger proportion, and the content of C, N element accounts for a smaller proportion. Fig. 4 is a STEM-HAADF diagram of the material from which the distribution range of the above four elements can be observed, the four elements are relatively uniformly distributed, and S, Cd elements are darker in color and more distributed; C. the color of the N element is lighter, and the distribution is less; therefore, the different distribution amounts of the element components of the material with the load ratio can be judged, and are caused by different contents of the components.
5. As can be seen from the XRD pattern of fig. 5, the single crystal diffraction pattern in fig. 5(a) shows that the graphite phase carbonitride is surely generated from two distinct characteristic peaks, which are located at about 13 ° and 27 ° and correspond to the peaks of the elements of the graphite phase carbonitride. In addition to the characteristic peaks of carbon and nitrogen compounds (two characteristic peaks at 13.2 degrees and 27.4 degrees, corresponding to (100) and (002) crystal planes), the characteristic peak of cadmium sulfide also appears in FIG. 5(b), which correspondingly characterizes the card JCPDS: 41-1049. The XRD diffraction pattern of CdS of a sample (a) obtained by taking single CED as a cadmium source is completely consistent with that of a standard PDF card-JCPDS 41-1049, and respectively corresponds to crystal faces (100), (002), (101), (102), (110), (103) and (112). The characteristic peak corresponding to the crystal face of the carbon nitrogen material (002) in the composite material is coincided with the characteristic peak corresponding to the crystal face of the CdS (101), and the peak intensity is increased along with the increase of the load capacity, which proves that g-C exists3N4。
6. From the X-ray photoelectron spectroscopy (XPS) of FIG. 6, we can obtain the microwave-assisted heating synthesized g-C from FIG. 6(a)3N4(8 wt%)/CdS nano-composite photocatalyst contains five elements of Cd, S, C, N and O, and all XPS peaks and reported g-C of a sample can be deduced from FIG. 63N4XPS peaks of/CdS complexes are consistent, therefore EDS and XPS analysis can confirm g-C3N4And forming the/CdS composite material.
7. As can be seen from the UV-vis diffuse absorption spectrum of FIG. 7, the g-C prepared according to the present invention is comparable to that reported in the literature3N4Showing a broader absorption range. In this work, g-C3N4Is synthesized by adopting a copolymerization method, and the crystallinity of the material is enhanced in the copolymerization process to change the electronic structure, so that g-C3N4The optical absorption range is expanded. And g-C3N4The coating does not change the burr spherical structure of the CdS nano material, and the optical absorption of the composite material is enhanced, so that the photocatalytic performance is improved.
8. As can be seen from the nitrogen adsorption-desorption isotherms and the corresponding pore size distributions (inset) of fig. 8, the nitrogen adsorption-desorption isotherms of the three samples are similar and all these are type IV with hysteresis loops indicating the presence of mesopores according to the IUPAC classification. Furthermore, the adsorption branch of these isotherms increases rapidly at relative pressures close to 1, which bears some similarities to the type II isotherms. Therefore, the sample also has large macropores. All hysteresis loops can be classified as H3 type, indicating the presence of slit-like holes. As can be seen from the inset of FIG. 8, the original CdS nanoprobe spheres contained mesopores (6-50nm) and macropores (50-110 nm). Small amount of g-C3N4The presence of (0.5 wt%) can introduce many small mesopores (2-10nm) and thus reduce the average pore size from 38.7 (for CN0) to 20.5nm (for CN 0.5). By considering that the pore volume of all samples did not change significantly, the SBET of CN0.5 would increase accordingly. However, g-C3N4Further increases in content may lead to the adhesion and aggregation of CdS nano-burl spheres, which in turn reduces the small mesopores (see the pore size distribution of CN 4), which then increases the average pore size. Therefore, the specific surface area of the sample will decrease. And 0.5 wt% g-C3N4the/CdS has large specific surface area and is beneficial to light absorptionThereby promoting photocatalysis and improving photocatalysis performance.
9. As can be seen from the i-t curve of fig. 9, (b) CN0.5 was confirmed to separate the photoinduced electrons and holes more effectively than the other groups. Photoelectrochemical measurements are commonly used to qualitatively study the excitation and transfer of photogenerated charge carriers in photocatalysts. Thus, having 0.5 wt% g-C3N4The most efficient charge separation can be achieved with the samples of/CdS, consistent with the photocatalytic activity measurements and the discussion above.
10. From the efficiency diagram of photocatalytic water splitting hydrogen production in FIG. 10, when the mass load ratio of graphite-phase carbon nitride is 0.5 wt%, g-C rapidly synthesized by microwave-assisted heating3N4Compared with other load proportions, the performance of the/CdS nano composite photocatalyst is better, and the hydrogen production efficiency is 2.76mmol/g/h after 20h of reaction. When the loading amount is too large, the active site is covered to cause a decrease in activity.
Therefore, the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure has excellent photocatalytic hydrogen production performance and can be applied to the technical field of photocatalytic hydrogen production.
Photolysis water hydrogen production performance test
1. The graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure obtained in the example 1 is used for hydrogen production by photolysis of water, and the specific treatment method comprises the following steps:
adding ultrapure water into a photocatalytic nano composite material, dispersing the photocatalytic nano composite material by using ultrasound, adding lactic acid after the ultrapure water is completely dissolved, uniformly mixing, transferring the reaction liquid into a reactor, introducing inert gas after vacuum deoxygenation, using a simulated sunlight xenon lamp as a light source, filtering stray light by using an optical filter below 420nm, and finally detecting the generated H by using gas chromatography2。
When the mass load proportion of the graphite phase carbon nitride is 0.5 wt%, the g-C is quickly synthesized by microwave-assisted heating3N4Compared with other load proportions, the performance of the/CdS nano composite photocatalyst is better, and the hydrogen production efficiency is 2.76mmol/g/h after 20h of reaction.
In summary, it can be seen from all the above embodiments that the preparation method of the present invention obtains the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burr spherical structure through the synergistic combination and coordination of specific process steps, process parameters, and the like, and the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material has good hydrogen production performance by photolysis of water.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (9)
1. A preparation method of a graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burred spherical structure is characterized by comprising the following steps:
s1: the urea is subjected to thermal polycondensation to obtain graphite-phase nitrogen carbide;
s2: adding graphite phase nitrogen carbide and cadmium sulfide precursors with the mass percentage of 0.01-4 wt% into a proper amount of ethylene glycol, uniformly stirring and ultrasonically dispersing to obtain precursor reaction liquid;
s3: and (3) rapidly synthesizing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure by the precursor reaction solution through a microwave-assisted heating method.
2. The method for preparing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure according to claim 1, wherein the method comprises the following steps: in step S1, the graphite phase nitrogen carbide is obtained by calcining urea at 550 ℃ for 3 hours.
3. The method for preparing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure according to claim 1, wherein the method comprises the following steps: in step S1, the graphite phase nitrogen carbide is g-phase graphite phase nitrogen carbide with the chemical formula of g-C3N4。
4. The method for preparing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure according to claim 1, wherein the method comprises the following steps: in step S2, the mass percentage of the graphite phase nitrogen carbide and cadmium sulfide precursor is 0.01-4 wt%.
5. The method for preparing the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burred spherical structure according to claim 1, wherein the step S3 is as follows:
s3-1: heating the precursor reaction solution obtained in the step S2 from room temperature to 90 ℃ under the microwave power of 200W, and keeping the temperature for 10 minutes to obtain a first reaction solution;
s3-2: continuously heating the first reaction solution to 160 ℃, and keeping the temperature for 10 minutes to obtain a second reaction solution;
s3-3: naturally cooling the second reaction solution to room temperature, centrifuging at the centrifugal speed of 18000rpm for 5 minutes, dispersing the obtained precipitate with absolute ethanol and high-purity water successively, centrifuging for 3-5 times, and vacuum drying at 60 ℃ for 8 hours to obtain the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite with the burr spherical structure.
6. A graphite phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burr spherical structure obtained by the preparation method as set forth in any one of claims 1 to 6.
7. Use of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with a burred spherical structure according to claim 6 as a photocatalyst in hydrogen production by photolysis of water.
8. Use according to claim 7, comprising: adding the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure into ultrapure water, performing ultrasonic dispersion, adding lactic acid after the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material is completely dissolved, uniformly mixing, transferring reaction liquid into a reactor, introducing inert gas after vacuum deoxygenation, filtering impure light by using an optical filter below 420nm under a light source, and performing photocatalytic water preparation on hydrogen.
9. Use according to claim 7, comprising: the mass volume ratio of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure to water is 1:2.05mg/ml, and the mass volume ratio of the graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with the burr spherical structure to lactic acid is 1:0.23 mg/ml.
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