CN114558600A - Mixed-dimension S-doped g-C3N4Base van der waals heterojunction photocatalyst and preparation method and application thereof - Google Patents
Mixed-dimension S-doped g-C3N4Base van der waals heterojunction photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 32
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002244 precipitate Substances 0.000 claims abstract description 22
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 claims abstract description 11
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000007146 photocatalysis Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 7
- 230000000593 degrading effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 8
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- 238000001035 drying Methods 0.000 description 4
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- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 229910052724 xenon Inorganic materials 0.000 description 2
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- 241000282414 Homo sapiens Species 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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Abstract
The invention discloses a mixed dimension S-doped g-C3N4A base van der Waals heterojunction photocatalyst, a preparation method and an application thereof belong to the technical field of material preparation. Dissolving melamine and cyanuric acid by dimethyl sulfoxide respectively to obtain clear solutions; the solution of melamine acid was added dropwise to the melamine solution to give as g-C3N4White precipitate of the basic van der waals heterojunction photocatalyst precursor; mixing the white precipitate precursor with trithiocyanuric acid, and calcining the mixed substance in a muffle furnace to obtain mixed dimension S-doped g-C3N4A base van der waals heterojunction photocatalyst. The catalyst can be applied to the field of photocatalysis, and the method can be obtained by changing reaction conditionsg-C doped with S in different proportions3N4The van der waals heterojunction photocatalyst has the advantages of simple process operation, stable structure and high repeatability, and can meet the requirements of laboratories and industries.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to mixed-dimension S-doped g-C3N4A base van der Waals heterojunction photocatalyst, a preparation method and application thereof.
Background
In the current society, global economic science and technology is turning to high-quality development from high-speed growth, the speed of the industrialized urbanization process is accelerated, the living standard of people is gradually improved, but the back of the continuous improvement of economic strength is often accompanied with the overuse of resources and energy. Meanwhile, the environmental pollution problem caused by energy development and exploitation also increasingly threatens the survival and development of human beings and other biological species; serious pollution events not only cause health problems, but also cause social problems. How to solve this problem has become a serious issue in the development of today. In many research fields, solar energy with the advantages of cleanness, reproducibility, easy availability and the like is the focus of research. How to efficiently utilize solar energy to directly decompose pollutants and directly convert energy into clean chemical energy and electric energy has great strategic significance. The photocatalysis technology is one of the most direct and effective methods for solving the problems of environmental pollution, energy shortage and the like of researchers by utilizing solar energy and taking advantage of the unique advantages of green, pollution-free and inexhaustible energy sources.
Graphite-like phase carbon nitrogen (g-C)3N4) Is a non-metal semiconductor photocatalystThe photocatalyst has the characteristics of no toxicity, stability and low cost, has a band gap of about 2.7eV, has good visible light absorption performance, but also has the defects of quick recombination of a photo-generated electron-hole pair, small specific surface area and the like, and limits the photocatalytic activity. The Van der Waals heterojunction photocatalyst is physically assembled together through relatively weak Van der Waals interaction force (intermolecular interaction force), does not depend on chemical bonds, is not limited by the lattice matching degree of materials, and brings new eosin for improving the performance of the photocatalyst material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a mixed-dimension S-doped g-C3N4A preparation method of a base van der Waals heterojunction photocatalyst. Another technical problem to be solved by the invention is to provide a mixed dimension S doped g-C3N4A base van der waals heterojunction photocatalyst. The invention also aims to provide a mixed-dimension S-doped g-C3N4The application of the base van der Waals heterojunction photocatalyst. The method has simple synthesis steps and convenient operation, and can prepare the S-doped g-C with different proportions by changing the reaction conditions3N4The base Van der Waals heterojunction photocatalyst has wide application prospect.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
mixed-dimension S-doped g-C3N4The preparation method of the Van der Waals heterojunction photocatalyst comprises the following steps:
(1) dissolving melamine and cyanuric acid by using dimethyl sulfoxide respectively to obtain a completely clarified melamine solution and a completely clarified cyanuric acid solution respectively;
(2) dropwise adding a melamine solution into the melamine solution to react to obtain the product as g-C3N4White precipitate of a precursor of a van der waals heterojunction photocatalyst;
(3) mixing the white precipitate precursor obtained in the step (2) with trithiocyanuric acid, and calcining the mixed substance in a muffle furnace to obtain mixed dimension SHetero g-C3N4A base van der waals heterojunction photocatalyst.
The mixed dimension S is doped with g-C3N4A preparation method of a van der Waals heterojunction photocatalyst comprises the steps of (2) continuously stirring and dropwise adding a melamine solution into the melamine solution at room temperature, then continuously stirring for 20-120 min, allowing white precipitate to appear, washing and drying the precipitate to obtain g-C3N4White precipitate of the base van der waals heterojunction photocatalyst precursor.
The mixed dimension S is doped with g-C3N4The preparation method of the van der Waals heterojunction photocatalyst comprises the step (3) of mixing the white precipitate precursor and trithiocyanuric acid according to the mass ratio of 1: 5-5: 1.
The mixed dimension S is doped with g-C3N4The preparation method of the van der Waals heterojunction photocatalyst comprises the steps of mixing the white precipitate precursor and trithiocyanuric acid in the step (3), calcining in a muffle furnace at 500-600 ℃, and preserving heat for 2-6 hours.
The mixed dimension S is doped with g-C3N4The preparation method of the base van der Waals heterojunction photocatalyst comprises the steps that the concentration of a melamine solution is 0.025g/ml, and the concentration of a melamine solution is 0.05 g/ml.
Mixed-dimension S-doped g-C prepared by the method3N4A base van der waals heterojunction photocatalyst.
The photocatalyst is applied to photocatalytic hydrogen production and photocatalytic degradation of rhodamine B dye.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) the invention can prepare S-doped g-C with different proportions by changing reaction conditions3N4The van der waals heterojunction photocatalyst has the advantages of simple process operation, high photocatalytic performance and good repeatability, and can meet the requirements of laboratories and industries.
(2) Mixed-dimension S-doped g-C prepared by the invention3N4The van der waals heterojunction photocatalyst has high-efficiency photocatalytic hydrogen production and dye degradation performance.
Drawings
FIG. 1 shows mixed-dimension S-doped g-C obtained in example 13N4XRD pattern of the van der waals heterojunction photocatalyst (CNCNS);
FIG. 2 shows mixed-dimension S-doped g-C obtained in example 13N4A base van der waals heterojunction photocatalyst (CNCNS) SEM image;
FIG. 3 shows mixed-dimension S-doped g-C obtained in example 13N4A degradation rate diagram of rhodamine B degraded by the base Van der Waals heterojunction photocatalyst;
FIG. 4 is a mixed dimension S doped g-C3N4A graph of hydrogen production performance of the photocatalysis of the base Van der Waals heterojunction photocatalyst;
FIG. 5 shows mixed-dimension S-doped g-C prepared in example 13N4And (3) photocatalytic degradation of rhodamine B cyclic graph by the aid of the van der Waals heterojunction photocatalyst.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
Mixed-dimension S-doped g-C3N4The preparation method of the van der waals heterojunction photocatalyst comprises the following steps:
(1) dissolving 1.0g of melamine and 1.0g of cyanuric acid in 40ml of dimethyl sulfoxide and 20ml of dimethyl sulfoxide respectively to obtain a completely clear melamine solution and a completely clear cyanuric acid solution respectively;
(2) dripping a melamine solution into the melamine solution under the condition of stirring, then continuously stirring for 20min to obtain white precipitate, washing and drying;
(3) mixing the white precipitate precursor and trithiocyanuric acid according to the mass ratio of 2:1, and calcining in a muffle furnace at 520 ℃ to obtain 2D/3D mixed dimension S doped g-C3N4A basic van der waals heterojunction photocatalyst (CNCNS).
FIG. 1 illustrates that the material prepared is g-C3N42D g-C doped with S3N4(CNS) and flower-like g-C3N4(CN) the peak strength is significantly reduced, inhibiting the growth of the crystal structure due to the formation of Van der Waals heterojunctions. FIG. 2 illustrates S doping g-C3N4The base van der Waals heterojunction photocatalyst has the structural characteristics of 2D/3D mixed dimension.
Measuring the prepared mixed dimension S-doped g-C in a photocatalytic reaction hydrogen production system3N4The photocatalytic hydrogen production performance of the van der waals heterojunction photocatalyst is that a 300w xenon lamp is selected as a light source in a reaction system, and the temperature of the system is kept at 6 ℃ by circulating cooling water. Photocatalyst (mixed dimension S prepared by the method is doped with g-C)3N4Van der waals heterojunction photocatalyst), 3% H14Cl6O6Pt and triethanolamine are mixed in an aqueous solution. H was determined by on-line gas chromatography (GC 7920, Ar as carrier gas, TCD detector)2The measurement results are shown in fig. 4. As a result, compared with CNS and CN, the photocatalytic hydrogen production performance is respectively improved by 6 times and 8 times.
Example 2
Mixed-dimension S-doped g-C3N4The preparation method of the van der waals heterojunction photocatalyst comprises the following steps:
(1) dissolving 1.0g of melamine and 1.0g of cyanuric acid in 40ml of dimethyl sulfoxide and 20ml of dimethyl sulfoxide respectively to obtain a completely clear melamine solution and a completely clear cyanuric acid solution respectively;
(2) dripping a melamine solution into the melamine solution under the condition of stirring, then continuously stirring for 20min to obtain white precipitate, washing and drying;
(3) mixing a white precipitate precursor and trithiocyanuric acid according to a mass ratio of 1:1, and calcining in a muffle furnace at 520 ℃ to obtain mixed dimension S-doped g-C3N4A base van der waals heterojunction photocatalyst.
Example 3
Mixed-dimension S-doped g-C3N4The preparation method of the van der waals heterojunction photocatalyst comprises the following steps:
(1) dissolving 1.0g of melamine and 1.0g of cyanuric acid in 40ml of dimethyl sulfoxide and 20ml of dimethyl sulfoxide respectively to obtain a completely clear melamine solution and a completely clear melamine solution respectively;
(2) dripping a melamine solution into the melamine solution under the condition of stirring, then continuously stirring for 20min to obtain white precipitate, washing and drying;
(3) mixing a white precipitate precursor and trithiocyanuric acid according to a mass ratio of 3:1, and calcining in a muffle furnace at 520 ℃ to obtain mixed dimension S-doped g-C3N4A base van der waals heterojunction photocatalyst.
Measuring the mixed dimension S doped g-C prepared in the photocatalytic reaction system3N4The reaction system adopts a 250w xenon lamp as a light source, and the temperature of the system is kept at about 20 ℃ by circulating cooling water. About 10mg of photocatalyst (mixed dimension S prepared above is doped with g-C)3N4A van der waals heterojunction photocatalyst) is mixed in 10mg/L rhodamine B solution for degrading rhodamine B dye. And measuring the absorbance of the rhodamine B solution by using an ultraviolet visible spectrophotometer (Lambda 950,200nm-800 nm). As shown in FIG. 3 (the graph 1:1, 2:1 and 3:1 in FIG. 3 respectively represent the change curves of the catalytic effects of the photocatalysts prepared in the embodiments 2, 1 and 3), the rhodamine B is obviously degraded along with the prolonging of time, and the degradation is basically completed in about 80min, which indicates that the prepared mixed dimension S is doped with g-C3N4The base van der waals heterojunction photocatalyst has extremely high degradation performance.
FIG. 5 shows mixed-dimension S-doped g-C from example 13N4And (3) photocatalytic degradation of rhodamine B cyclic graph by the aid of the van der Waals heterojunction photocatalyst. As can be seen from fig. 5, the photocatalyst still has a good catalytic effect after being cycled for many times, which indicates that the photocatalyst can be reused.
Claims (7)
1. Mixed-dimension S-doped g-C3N4The preparation method of the van der waals heterojunction photocatalyst is characterized by comprising the following steps of:
(1) dissolving melamine and cyanuric acid by using dimethyl sulfoxide respectively to obtain a completely clarified melamine solution and a completely clarified cyanuric acid solution respectively;
(2) dropwise adding a melamine solution into the melamine solution to react to obtain the product as g-C3N4White precipitate of a precursor of a van der waals heterojunction photocatalyst;
(3) mixing the white precipitate precursor obtained in the step (2) with trithiocyanuric acid, and calcining the mixed substance in a muffle furnace to obtain mixed dimension S doped g-C3N4A base van der waals heterojunction photocatalyst.
2. The mixed-dimension S-doped g-C of claim 13N4The preparation method of the van der Waals heterojunction photocatalyst is characterized in that in the step (2), under the condition of room temperature, the melamine solution is continuously stirred and dropwise added into the melamine solution, then the mixture is continuously stirred for 20-120 min, white precipitates appear, and the precipitates are washed and dried to obtain the g-C3N4White precipitate of the base van der waals heterojunction photocatalyst precursor.
3. The mixed-dimension S-doped g-C of claim 13N4The preparation method of the van der Waals heterojunction photocatalyst is characterized in that in the step (3), the white precipitate precursor and trithiocyanuric acid are mixed according to the mass ratio of 1: 5-5: 1.
4. The mixed-dimension S-doped g-C of claim 13N4The preparation method of the van der Waals heterojunction photocatalyst is characterized in that in the step (3), the white precipitate precursor and trithiocyanuric acid are mixed, placed in a muffle furnace for calcination at 500-600 ℃, and kept warm for 2-6 h.
5. The mixed-dimension S-doped g-C of claim 13N4The preparation method of the van der Waals heterojunction photocatalyst is characterized in that the concentration of a melamine solution is 0.025g/ml, and the concentration of a melamine solution is 0.05 g/ml.
6. Mixed-dimension S-doped g-C produced by the method of any one of claims 1-53N4A base van der waals heterojunction photocatalyst.
7. The application of the photocatalyst in the photocatalysis of hydrogen production and the photocatalysis of degrading rhodamine B dye in claim 6.
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| TING FEI等: "A 3D peony-like sulfur-doped carbon nitride synthesized by self-assembly for efficient photocatalytic hydrogen production", INTERNATIONAL JOURNAL OF HYDROGEN ENERGY, vol. 46, pages 20481 - 20491 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115254172A (en) * | 2022-08-29 | 2022-11-01 | 江苏科技大学 | Vesicular g-C 3 N 4 Photocatalyst and preparation method thereof |
| CN115254172B (en) * | 2022-08-29 | 2023-12-19 | 江苏科技大学 | Vesicle-shaped g-C 3 N 4 Photocatalyst and preparation method thereof |
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