CN111715270A - Foamed g-C3N4Photocatalytic material, preparation method and application - Google Patents
Foamed g-C3N4Photocatalytic material, preparation method and application Download PDFInfo
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- CN111715270A CN111715270A CN202010673137.9A CN202010673137A CN111715270A CN 111715270 A CN111715270 A CN 111715270A CN 202010673137 A CN202010673137 A CN 202010673137A CN 111715270 A CN111715270 A CN 111715270A
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 230000001699 photocatalysis Effects 0.000 claims abstract description 39
- 238000001354 calcination Methods 0.000 claims abstract description 23
- 239000004202 carbamide Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 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 abstract description 15
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000006260 foam Substances 0.000 claims description 8
- 238000006731 degradation reaction Methods 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 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
- B01J27/25—Nitrates
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- B01J35/39—
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- B01J35/613—
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- B01J35/633—
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- B01J35/638—
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- B01J35/647—
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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 provides a foamed g-C3N4A photocatalytic material, a preparation method and application, belonging to the technical field of preparation of novel environment-friendly materials. The method comprises the steps of calcining urea by using an arc-shaped crucible with a cover as a raw material, wherein the calcining comprises two stages of heating-up calcining and constant-temperature calcining, the heating-up calcining is firstly carried out, the heating-up rate is 5-30 ℃/min, and the urea is heated to 500-570 ℃; then constant temperature calcination is carried out, 500Calcining at-570 deg.C for 2-4 hr, cooling to room temperature to obtain foamed g-C3N4A photocatalytic material. Foamed g-C made by the invention3N4The specific surface area is large and is as high as 81.9m2The rhodamine B photocatalyst has the advantages of strong photocatalytic activity and the like, can be used for rapidly degrading the rhodamine B dye through photocatalysis, and can efficiently remove the dye in water.
Description
Technical Field
The invention belongs to the technical field of preparation of novel environment-friendly materials, and relates to a foamy g-C3N4Method for producing photocatalytic material, and foamed g-C3N4A photocatalytic material and application thereof, in particular to a foamy g-C3N4The application of the photocatalytic material in processing rhodamine B.
Background
Nowadays, environmental pollution is serious, environmental problems are increasingly prominent, a photocatalytic technology is a low-cost and environment-friendly green energy and environment treatment technology, and research on a harmless photocatalyst with high photocatalytic performance has become a wide research hotspot at present.
g-C3N4The photocatalyst has a wider absorption spectrum range due to the unique optical performance of the photocatalyst, can play a role in common visible light, and has the advantages of higher thermal stability, chemical stability, easiness in preparation and the like. g-C from urea3N4Has a larger specific surface area but a lower urea yield. Preparation of C by the related art3N4However, it is fired to produce g-C from urea3N4When the crucible is required to be wrapped by tinfoil paper, the C can be prepared3N4And when the temperature rising program exceeds 8 ℃/min, the g-C prepared finally3N4The amount of the solid is less and less, even all the solid is run off, little solid can not be left, and g-C can not be obtained3N4The invention overcomes the defects, does not need to be wrapped by tinfoil paper, has high-speed temperature rise program, and successfully prepares the foam g-C3N4。
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing g-C by using urea as a raw material3N4The method of the photocatalyst is simple and has excellent photocatalytic performance. Overcomes some research defects existing before, and prepares C by burning urea3N4In the process, a large amount of C can be prepared without any package on the crucible3N4And g-C3N4Is in foam shape, has large specific surface area which is as high as 81.9m2And/g, strong photocatalytic performance.
In order to solve the technical problems, the invention adopts the technical scheme that:
foamed g-C3N4The method of the photocatalytic material is characterized in that urea is used as a raw material, an arc-shaped crucible with a cover is adopted to calcine the urea, the calcination comprises two stages of heating calcination and constant-temperature calcination, the heating calcination is firstly carried out, the heating rate is 5-30 ℃/min, and the urea is heated to 500-570 ℃; then carrying out constant temperature calcination, continuing calcination for 2-4h at the temperature of 500-570 ℃, cooling to room temperature to obtain foamed g-C3N4A photocatalytic material.
Further, 10g of urea needs to be fired in 20, 25, 30 or 40ml curved covered crucibles.
Further, the heating rate is 13-17 ℃/min. Preferably, the rate of temperature rise is 15 ℃/min.
Furthermore, the fixed temperature is 550 ℃, and the constant-temperature calcination time is 3 hours.
Foamed g-C3N4Application of photocatalytic material, and foamed g-C prepared by using method3N4And the photocatalytic material is used for removing the rhodamine B dye.
The application method comprises the following steps: adding foamed g-C into rhodamine B solution3N4And carrying out ultrasonic dispersion on the photocatalytic material, then carrying out dark adsorption, carrying out light treatment after adsorption balance is achieved, and finally finishing degradation of the dye.
The foamed g-C3N4The addition amount of the photocatalytic material is that foam-shaped g-C is added into every 50mL of rhodamine B solution3N410mg of the photocatalytic material, wherein the concentration of the rhodamine B solution is 10 mg/L.
The ultrasonic time is 15-60 s; the light intensity of the tungsten lamp is 50W, and the light adding treatment time is 60 min.
The invention has the beneficial effects that: can prepare the required g-C by using a small amount of urea3N4And shaped like a foam, prepared g-C3N4The comparison area is large, and the maximum comparison area reaches 81.9m2Preparation of g foam g-C3N4The photocatalysis capability is strong, and the complete degradation of the rhodamine B dye can be basically completed within one hour.
Drawings
FIG. 1 shows the foamed g-C prepared in this example3N4TEM image with temperature rise rate of 15 ℃/min, as shown in figure 1, the foamed g-C prepared by the invention3N4The material has a two-dimensional layered structure.
FIG. 2 shows the foamed g-C prepared in this example3N4A Bet graph with a temperature rise rate of 15 ℃/min, wherein (a) is foamed g-C3N4The aperture distribution diagram (b) is a partial enlarged view of (a). As can be seen from the figure, the resulting foam g-C3N4The pore diameters were 3nm and 30nm, and the pore volume at 3nm was 0.07cc/g and that at 30nm was 1.45 cc/g.
FIG. 3 foam-like g-C prepared at different ramp rates3N4And (3) a photocatalytic material degradation removal rate effect diagram.
FIG. 4 foam-like g-C prepared at different ramp rates3N4Degradation of the photocatalytic material and concentration effect.
Detailed Description
Example 1
The following detailed description of the invention refers to the accompanying drawings.
Foamed g-C of the invention3N4The preparation method of the material comprises the following steps:
5 parts of urea, 10g each, were weighed into 30ml arc crucibles with covers, the urea was spread out in the crucibles, the covers were then covered, and the samples were placed in muffle furnaces for programmed calcination. The specific method of calcining is 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min, heating the urea to 550 ℃, and then keeping the temperature at 550 ℃ for calcining for 3h at constant temperature. The samples were collected and stored by cooling to room temperature.
FIG. 1 is a view of the present examplePrepared foam g-C3N4TEM images of the material. As shown in FIG. 1, the foamed g-C prepared by the present invention3N4Has a two-dimensional layered structure.
FIG. 2 shows the foamed g-C prepared in this example3N4The Bet graph with the heating rate of 15 ℃/min shows that the prepared foam-shaped g-C3N4The pore diameter was 3nm and 30nm, the pore volume at 3nm was 0.07cc/g, and the pore volume at 30nm was 1.45 cc/g.
Example 2
Foamed g-C of the invention3N4The application of the material in degrading dye rhodamine B comprises the following steps:
weighing foamed g-C prepared by different temperature gradients3N4Adding 10mg of the material into 50ml of the solution (with the concentration of 10mg/L), and performing ultrasonic diffusion for 15-60s to obtain foamed g-C3N4The material can be fully dispersed in the solution, and is firstly stirred for 30min in a shading way to carry out dark adsorption. Then, the light is added to carry out the photocatalytic reaction. FIG. 3 and FIG. 4 are the foam-like g-C3N4And (3) a degradation effect graph of the material. Foamed g-C prepared by the invention3N4The material can completely degrade rhodamine B dye within one hour of illumination, wherein the dark adsorption efficiency is improved by nearly 10% when the temperature rise rate is 15 ℃/min, the photocatalytic capacity after the light is added is improved by nearly 20%, and the prepared foam g-C3N4The material has the fastest degradation rate. Foamed g-C prepared by the invention3N4The material has good treatment effect on rhodamine B dye, and provides convenience for the subsequent photocatalytic material developed on the basis.
The above provides a foamed g-C3N4The photocatalytic material and its detailed preparation method, the principle and implementation of the present invention are illustrated herein by using specific examples, and the above description of the examples is only for the purpose of helping understanding the method of the present invention and its core idea, it should be noted that, for those skilled in the art, the present invention can also be implemented without departing from the principle of the present inventionThe invention is subject to several improvements and modifications, which also fall within the scope of protection of the claims of the present invention.
Claims (10)
1. Foamed g-C3N4The method for preparing the photocatalytic material is characterized in that urea is used as a raw material, an arc-shaped crucible with a cover is adopted to calcine the urea, the calcination comprises two stages of heating calcination and constant-temperature calcination, the heating calcination is firstly carried out, the heating rate is 5-30 ℃/min, and the urea is heated to 500-570 ℃; then carrying out constant temperature calcination, continuing calcination for 2-4h at the temperature of 500-570 ℃, cooling to room temperature to obtain foamed g-C3N4A photocatalytic material.
2. A foamed g-C according to claim 13N4Method for photocatalytic material, characterized in that 10g of urea needs to be fired in 20, 25, 30 or 40ml curved covered crucibles.
3. A foamed g-C according to claim 13N4The method for preparing the photocatalytic material is characterized in that the temperature rise rate is 13-17 ℃/min.
4. A foamed g-C according to claim 33N4The method for preparing the photocatalytic material is characterized in that the temperature rise rate is 15 ℃/min.
5. A foamed g-C according to claim 1, 2, 3 or 43N4The method for preparing the photocatalytic material is characterized in that the fixed temperature is 550 ℃, and the constant-temperature calcination time is 3 hours.
6. Foamed g-C3N4The photocatalytic material is characterized in that the foamed g-C3N4Photocatalytic material obtainable by the process according to any one of claims 1 to 5.
7. Foamed g-C3N4Use of a photocatalytic material, characterized in that it is obtained in the form of a foam g-C obtained by the process according to any one of claims 1 to 53N4And the photocatalytic material is used for removing the rhodamine B dye.
8. A foamed g-C according to claim 73N4The application of the photocatalytic material is characterized in that the application method comprises the following steps: adding foamed g-C into rhodamine B solution3N4And carrying out ultrasonic dispersion on the photocatalytic material, then carrying out dark adsorption, carrying out light treatment after adsorption balance is achieved, and finally finishing degradation of the dye.
9. A foamed g-C according to claim 83N4Use of a photocatalytic material, characterized in that said foamed g-C3N4The addition amount of the photocatalytic material is that foam-shaped g-C is added into every 50mL of rhodamine B solution3N410mg of the photocatalytic material, wherein the concentration of the rhodamine B solution is 10 mg/L.
10. A foamed g-C according to claim 8 or 93N4The application of the photocatalytic material is characterized in that the ultrasonic time is 15-60 s; the light intensity of the tungsten lamp is 50W, and the light adding treatment time is 60 min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010673137.9A CN111715270A (en) | 2020-07-14 | 2020-07-14 | Foamed g-C3N4Photocatalytic material, preparation method and application |
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| CN202010673137.9A CN111715270A (en) | 2020-07-14 | 2020-07-14 | Foamed g-C3N4Photocatalytic material, preparation method and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112892575A (en) * | 2021-01-26 | 2021-06-04 | 大连理工大学 | Metal monoatomic catalytic material M-C for activating soluble oxidant3N4Preparation method and application of |
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| CN103301867A (en) * | 2013-06-25 | 2013-09-18 | 重庆工商大学 | Inorganic ion doped carbon nitride photocatalyst and preparation method thereof |
| CN106824247A (en) * | 2017-02-28 | 2017-06-13 | 陕西科技大学 | A kind of bismuth tungstate/carbonitride/bismuth phosphate composite photo-catalyst and its preparation method and application |
| CN107252701A (en) * | 2017-07-12 | 2017-10-17 | 西华师范大学 | A kind of high activity graphite phase carbon nitride material and preparation method thereof |
| CN107876079A (en) * | 2017-11-16 | 2018-04-06 | 三峡大学 | A kind of preparation method and applications of sulfur doping Zinc oxide quantum dot modification porous graphite phase nitrogen carbide composite |
| US20180305231A1 (en) * | 2017-04-19 | 2018-10-25 | King Abdulaziz University | Composite, a method of making thereof, and a method for degrading a pollutant |
-
2020
- 2020-07-14 CN CN202010673137.9A patent/CN111715270A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301867A (en) * | 2013-06-25 | 2013-09-18 | 重庆工商大学 | Inorganic ion doped carbon nitride photocatalyst and preparation method thereof |
| CN106824247A (en) * | 2017-02-28 | 2017-06-13 | 陕西科技大学 | A kind of bismuth tungstate/carbonitride/bismuth phosphate composite photo-catalyst and its preparation method and application |
| US20180305231A1 (en) * | 2017-04-19 | 2018-10-25 | King Abdulaziz University | Composite, a method of making thereof, and a method for degrading a pollutant |
| CN107252701A (en) * | 2017-07-12 | 2017-10-17 | 西华师范大学 | A kind of high activity graphite phase carbon nitride material and preparation method thereof |
| CN107876079A (en) * | 2017-11-16 | 2018-04-06 | 三峡大学 | A kind of preparation method and applications of sulfur doping Zinc oxide quantum dot modification porous graphite phase nitrogen carbide composite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112892575A (en) * | 2021-01-26 | 2021-06-04 | 大连理工大学 | Metal monoatomic catalytic material M-C for activating soluble oxidant3N4Preparation method and application of |
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