CN112246272A - Has a defect g-C3N4Preparation method of nanosheet photocatalyst - Google Patents
Has a defect g-C3N4Preparation method of nanosheet photocatalyst Download PDFInfo
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- CN112246272A CN112246272A CN202011152023.6A CN202011152023A CN112246272A CN 112246272 A CN112246272 A CN 112246272A CN 202011152023 A CN202011152023 A CN 202011152023A CN 112246272 A CN112246272 A CN 112246272A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 47
- 239000002135 nanosheet Substances 0.000 title claims abstract description 41
- 230000007547 defect Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 38
- 238000001354 calcination Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 19
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 230000005291 magnetic effect Effects 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 230000002950 deficient Effects 0.000 claims description 9
- 239000003403 water pollutant Substances 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000003242 anti bacterial agent Substances 0.000 abstract description 3
- 229940088710 antibiotic agent Drugs 0.000 abstract description 3
- 239000000975 dye Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 4
- 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 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a method for preparing a composition with defects of g-C3N4A preparation method of a nano-sheet photocatalyst belongs to the technical field of preparation of semiconductor photocatalytic materials. The method comprises the following steps: 1) weighing melamine, placing the melamine in a crucible, heating and calcining in a muffle furnace, calcining at the temperature of 500-580 ℃ for 1-6h, cooling to room temperature, and grinding into powder; 2) taking the powder sample obtained in the step 1), placing the powder sample in a magnetic boat, heating and calcining the powder sample in a muffle furnace again, calcining the powder sample at 480-620 ℃ for 1-6h, cooling the powder sample to room temperature, and grinding the powder sample into powder to obtain the powder with the defect g-C3N4A nanosheet photocatalyst. The application adjusts and controls the temperature to enable the block g-C3N4Stripping into nanosheets and constructing defects, so that the nanosheets have higher photocatalytic performance. The preparation method has simple operation and high repeatability, and the prepared g-C with defects3N4The nano-sheet photocatalyst shows higher degradation activity for degradation of dyes and antibiotics.
Description
Technical Field
The invention belongs to the technical field of preparation of semiconductor photocatalytic materials, and particularly relates to a photocatalyst with a defect g-C3N4A preparation method of a nanosheet photocatalyst.
Background
The water body pollution is caused by the fact that industrial wastewater, domestic sewage, other wastes and the like enter a water body and exceed the self-purification capacity of the water body. The waste materials including chemical dyes, antibiotics and the like enter the water body, pollute the water body environment, poison aquatic organisms and seriously affect the life health and safety of human beings. The traditional physical, chemical and biological methods are low in sewage treatment efficiency, easy to generate secondary pollutants and limited in application range. Therefore, the search for new solutions has become a focus of researchers. In recent years, the photocatalysis technology is concerned by people, pollutants can be degraded only by light, and the photocatalyst is stable and can be recycled, so that the consumption of materials and energy is greatly reduced. Graphite-like phase carbon nitrogen (g-C)3N4) Is just one halfThe conductor photocatalyst has the characteristics of no toxicity, stability and low cost, the band gap is about 2.7eV, the visible light absorption performance is good, but the defect that the photo-generated electron-hole pair is fast in recombination, the specific surface area is small and the like is overcome, and the photocatalytic activity is limited. Therefore, it is necessary to modify it to improve the photocatalytic activity. At present, although there are many preparation methods including a hydrothermal-assisted synthesis method and the like, each of these methods has advantages and disadvantages.
The basic steps of the hydrothermal auxiliary synthesis method are as follows: the raw materials and a certain amount of solvent are added into a high-pressure closed reaction tank, the required temperature is reached according to a certain heating rate, and some reactions which are difficult to occur under the atmospheric condition of normal pressure can react in the specific low-temperature high-pressure solvent, so that the phenomena of nucleation and growth occur, and the required catalyst material is obtained. In the process of the synthesis method, the solvent can not only dissolve the uniformly mixed precursor but also be used as a medium to transfer pressure, so that the same pressure is maintained in the reaction tank. The hydrothermal assisted synthesis method has the advantages that the synthesis conditions such as the pressure in a reaction tank, the temperature and the time of reaction and the like can be controlled by adding the solvent, and the nucleation rate and direction of material crystals can be artificially controlled according to the expected target, so that the morphological structure and the properties of the product are changed. However, this method has a disadvantage that the reaction process requires high pressure and thus the reaction synthesizer is required to be strict.
Disclosure of Invention
In view of the above problems in the prior art, the technical problem to be solved by the present invention is to provide a method for producing a product with g-C defect3N4A preparation method of a nanosheet photocatalyst.
Para graphite-like phase carbon nitrogen (g-C)3N4) For g-C, the treatment can be carried out by hydrothermal treatment, acid etching, alkali etching and adjusting process3N4The morphology of the film is regulated and controlled. These methods are mainly carried out by subjecting the block g-C to3N4Exfoliation is performed to form 2D (gauze) or 3D (petal, nanotube) structures. The spatial dissimilarity exhibited by these morphologies allows the photogenerated electron-hole pairs to be rapidly addressedSeparation and transfer, increasing quantum efficiency; and simultaneously, the light absorption capacity and the adsorption performance are enhanced.
The application synthesizes g-C with defects by a two-step method3N4Nanosheet photocatalyst, bulk g-C3N4The defects and the nanosheet structure are presented through stripping, the operation is simple, and the repeatability is high.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
has a defect g-C3N4The preparation method of the nanosheet photocatalyst comprises the following steps:
1) weighing melamine, placing the melamine in a crucible, heating and calcining the melamine in a muffle furnace, naturally cooling the melamine to room temperature after the heating and calcining are finished, and grinding the melamine into powder;
2) taking the powder sample obtained in the step 1), placing the powder sample in a magnetic boat, heating and calcining the powder sample in a muffle furnace again, naturally cooling the powder sample to room temperature after the calcination, and grinding the powder sample into powder to obtain the product with the defect g-C3N4A nanosheet photocatalyst.
Further, in the step 1), the heating rate is 2 ℃/min, the calcination temperature is 500-.
Preferably, in step 1), the calcination temperature is 520 ℃ and the calcination time is 2 h.
Further, in the step 2), the temperature rise rate is 5 ℃/min, the calcination temperature is 480 ℃ and 620 ℃, and the calcination time is 1-6 h.
Preferably, in the step 2), the calcination temperature is 600-620 ℃ and the calcination time is 4 h.
Preferably, in the step 2), the calcining temperature is 600 ℃ and the calcining time is 4 h.
The preparation method can obtain the product with the defect of g-C3N4A nanosheet photocatalyst.
Prepared with g-C having defects3N4The application of the nanosheet photocatalyst in photocatalytic degradation of water pollutants.
Has the advantages that: compared with the prior art, the invention has the advantages that:
1) book (I)The application adopts a direct calcination method to directly obtain the blocky g-C3N4Calcining without adding any substance or loss of sample, increasing defect sites and increasing g-C by regulating and controlling temperature3N4The block structure is stripped to change the structure from block to nano-sheet, thereby obtaining the nano-sheet with the defect g-C3N4The muffle furnace used in the preparation process of the nanosheet photocatalyst is simple to operate, the danger coefficient is low, and the preparation method is simple and efficient;
2) compared with the composite photocatalyst which is easy to separate two phases in the reaction process to cause activity reduction, the composite photocatalyst prepared by the method has the defect of g-C3N4The nano-sheet photocatalyst has high stability, does not have the problem of separation, and can be repeatedly used;
3) the raw material is melamine, so that the price is low, and the economic cost is low;
4) g-C with defects prepared in the present application3N4The nanosheet photocatalyst shows high degradation activity for degradation of dyes and antibiotics, and has a wide application prospect in degradation of water pollutants.
Drawings
FIG. 1 shows defects g-C prepared in example 13N4Transmission electron microscopy of nanoplatelet photocatalyst;
FIG. 2 is g-C bulk prepared in example 13N4Photocatalyst and Defect g-C3N4Electron paramagnetic resonance plot of nanosheet photocatalyst;
FIG. 3 is g-C of the bulk prepared in example 13N4Transmission electron microscopy of the photocatalyst;
FIG. 4 is g-C of the bulk prepared in example 13N4Photocatalyst and Defect g-C3N4And (3) a degradation rate diagram of the nanosheet photocatalyst for rhodamine B (RhB).
Detailed Description
The invention is further described with reference to specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. It is intended to cover by the present invention all such modifications as come within the scope of the invention as defined by the appended claims.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. The melamine used in the present invention was commercially available in analytical purity.
Example 1
2g of melamine were weighed, ground to a powder thoroughly, placed in a 20mL crucible, placed in a muffle furnace, brought to 520 ℃ at a heating rate of 2 ℃/min and held at this temperature for 2 h. After cooling to room temperature, taking out and fully grinding to powder. 0.5g of the obtained powdery sample is uniformly spread on a magnetic boat, and is heated to 600 ℃ in a muffle furnace at the heating rate of 5 ℃/min and is kept at the temperature for 4 hours. After cooling to room temperature, taking out and fully grinding to powder. Defective g-C is obtained3N4A nanosheet photocatalyst.
FIG. 1 shows defects g-C prepared in example 13N4And (3) a transmission electron microscope photo of the nanosheet photocatalyst, wherein the sample is in an ultrathin nearly transparent nanosheet structure.
FIG. 2 is g-C bulk prepared in example 13N4Photocatalyst and Defect g-C3N4Electron paramagnetic resonance image of nanosheet photocatalyst, in which the change in signal intensity confirms the defect g-C3N4The defect sites of the nanosheet photocatalyst are significantly increased.
FIG. 3 is g-C of the bulk prepared in example 13N4Transmission electron micrograph of the photocatalyst, from which the bulk g-C can be seen3N4The sample exhibited a thicker bulk-like structure, in sharp contrast to fig. 1.
FIG. 4 is g-C of the bulk prepared in example 13N4Photocatalyst and Defect g-C3N4The degradation rate diagram of the nano-sheet photocatalyst on rhodamine B (RhB) can be seen, and the defects g-C can be seen from the diagram3N4Nano-sheet photocatalyst for treating pollutantsHigh efficiency degradation.
Example 2
2g of melamine were weighed, ground to a powder thoroughly, placed in a 20mL crucible, placed in a muffle furnace, brought to 520 ℃ at a heating rate of 2 ℃/min and held at this temperature for 2 h. After cooling to room temperature, taking out and fully grinding to powder. 0.5g of the obtained powdery sample is uniformly spread on a magnetic boat, and is heated to 620 ℃ in a muffle furnace at a heating rate of 5 ℃/min and is kept at the temperature for 4 hours. After cooling to room temperature, taking out and fully grinding to powder. Defective g-C is obtained3N4A nanosheet photocatalyst.
Example 3
2g of melamine were weighed, ground to a powder thoroughly, placed in a 20mL crucible, placed in a muffle furnace, brought to 580 ℃ at a heating rate of 2 ℃/min and held at this temperature for 6 h. After cooling to room temperature, taking out and fully grinding to powder. 0.5g of the obtained powdery sample is uniformly spread on a magnetic boat, and is heated to 480 ℃ in a muffle furnace at the heating rate of 5 ℃/min and kept at the temperature for 6 hours. After cooling to room temperature, taking out and fully grinding to powder. Defective g-C is obtained3N4A nanosheet photocatalyst.
Example 4
2g of melamine were weighed, ground to a powder thoroughly, placed in a 20mL crucible, placed in a muffle furnace, brought to 500 ℃ at a heating rate of 2 ℃/min and held at this temperature for 4 h. After cooling to room temperature, taking out and fully grinding to powder. 0.5g of the obtained powdery sample is uniformly spread on a magnetic boat, and is heated to 620 ℃ in a muffle furnace at the heating rate of 5 ℃/min and is kept at the temperature for 2 h. After cooling to room temperature, taking out and fully grinding to powder. Defective g-C is obtained3N4A nanosheet photocatalyst.
Example 5
2g of melamine were weighed, ground to a powder thoroughly, placed in a 20mL crucible, placed in a muffle furnace, brought to 550 ℃ at a heating rate of 2 ℃/min and held at this temperature for 3 h. Cooling to room temperatureThen, the mixture is taken out and fully ground into powder. 0.5g of the obtained powdery sample is uniformly spread on a magnetic boat, and is heated to 550 ℃ in a muffle furnace at the heating rate of 5 ℃/min and is kept at the temperature for 5 hours. After cooling to room temperature, taking out and fully grinding to powder. Defective g-C is obtained3N4A nanosheet photocatalyst.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to yield one or more new ranges of values, which ranges of values are to be considered as specifically disclosed herein.
Claims (7)
1. Has a defect g-C3N4The preparation method of the nanosheet photocatalyst is characterized by comprising the following steps of:
1) weighing melamine, placing the melamine in a crucible, heating and calcining the melamine in a muffle furnace, naturally cooling the melamine to room temperature after the heating and calcining are finished, and grinding the melamine into powder;
2) taking the powder sample obtained in the step 1), placing the powder sample in a magnetic boat, heating and calcining the powder sample again in a muffle furnace, naturally cooling the powder sample to room temperature after the calcination, and grinding the powder sample into powder to obtain the g-C with the defects3N4A nanosheet photocatalyst.
2. The defective g-C of claim 13N4The preparation method of the nanosheet photocatalyst is characterized in that in the step 1), the heating rate is 2 ℃/min, the calcination temperature is 500-.
3. The defective g-C of claim 23N4The preparation method of the nanosheet photocatalyst is characterized in that in the step 1), the heating rate is 2 ℃/min, the calcination temperature is 520 ℃, and the calcination time is 2 h.
4. The defective g-C of claim 13N4The preparation method of the nano-sheet photocatalyst is characterized in that in the step 2), the heating rate is 5 ℃/min, the calcination temperature is 480-620 ℃, and the calcination time is 1-6 h.
5. The defective g-C of claim 43N4The preparation method of the nanosheet photocatalyst is characterized in that in the step 2), the heating rate is 5 ℃/min, the calcination temperature is 600 ℃, and the calcination time is 4 h.
6. The product of the process of any one of claims 1 to 5 having a defect g-C3N4A nanosheet photocatalyst.
7. The method of claim 6 having a defect of g-C3N4The application of the nanosheet photocatalyst in photocatalytic degradation of water pollutants.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112958141A (en) * | 2021-03-17 | 2021-06-15 | 桂林电子科技大学 | Oxygen-containing g-C3N4Preparation method and application of nanosheet photocatalyst |
| CN113086955A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Preparation method of carbon-deficient carbon nitride material for photocatalytic nitrogen fixation |
| CN113321818A (en) * | 2021-05-11 | 2021-08-31 | 中山大学 | Composite hydrogel and preparation method and application thereof |
| CN113830742A (en) * | 2021-07-16 | 2021-12-24 | 中国科学技术大学 | Ultrathin carbon nitride nanosheet rich in nitrogen defects, preparation method of ultrathin carbon nitride nanosheet and method for preparing hydrogen peroxide through photocatalysis |
| CN115646528A (en) * | 2022-10-30 | 2023-01-31 | 西北工业大学 | High-yield preparation of defect-rich graphite carbon nitride photocatalyst by taking pine as control agent |
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| CN108380237A (en) * | 2018-05-04 | 2018-08-10 | 辽宁大学 | Nitrogen defect graphite phase carbon nitride nanosheet photocatalyst and the preparation method and application thereof |
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Patent Citations (1)
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| CN108380237A (en) * | 2018-05-04 | 2018-08-10 | 辽宁大学 | Nitrogen defect graphite phase carbon nitride nanosheet photocatalyst and the preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112958141A (en) * | 2021-03-17 | 2021-06-15 | 桂林电子科技大学 | Oxygen-containing g-C3N4Preparation method and application of nanosheet photocatalyst |
| CN113086955A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Preparation method of carbon-deficient carbon nitride material for photocatalytic nitrogen fixation |
| CN113321818A (en) * | 2021-05-11 | 2021-08-31 | 中山大学 | Composite hydrogel and preparation method and application thereof |
| CN113830742A (en) * | 2021-07-16 | 2021-12-24 | 中国科学技术大学 | Ultrathin carbon nitride nanosheet rich in nitrogen defects, preparation method of ultrathin carbon nitride nanosheet and method for preparing hydrogen peroxide through photocatalysis |
| CN115646528A (en) * | 2022-10-30 | 2023-01-31 | 西北工业大学 | High-yield preparation of defect-rich graphite carbon nitride photocatalyst by taking pine as control agent |
| CN115646528B (en) * | 2022-10-30 | 2024-01-30 | 西北工业大学 | Method for preparing defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as control agent |
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