CN111203258A - Photocatalyst S-C3N4Preparation method and application of - Google Patents
Photocatalyst S-C3N4Preparation method and application of Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title abstract 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 abstract description 44
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 44
- 230000015556 catabolic process Effects 0.000 claims abstract description 34
- 238000006731 degradation reaction Methods 0.000 claims abstract description 34
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 claims description 21
- 239000010453 quartz Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000012425 OXONE® Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical group [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 claims description 8
- 239000002135 nanosheet Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 11
- 239000002351 wastewater Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000000593 degrading effect Effects 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 230000003213 activating effect Effects 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 239000002060 nanoflake Substances 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 238000009303 advanced oxidation process reaction Methods 0.000 description 6
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 6
- 239000012265 solid product Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000006385 ozonation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Images
Classifications
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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—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the technical field of semiconductor photocatalysis, and provides a photocatalyst S-C3N4The preparation method and the application thereof. Calcining urea as raw material in muffle furnace in air atmosphere to synthesize B-C3N4Then with B-C3N4The raw materials are subjected to secondary calcination in a muffle furnace to obtain blocky B-C3N4Preparing to obtain the S-C in the shape of nano-flakes3N4. The change from block to ultrathin nanometer sheet can effectively increase the S-C of the semiconductor photocatalyst3N4The active site number on the surface improves the capability of activating PMS, thereby generating more SO4‑H; on the other hand, C3N4The photocatalytic property of the photocatalyst can cause the photocatalyst to generate partial OH‑Thereby further promoting the degradation of the dye wastewater. The method is used for catalyzing and degrading rhodamine B, S-C3N4By using SO4‑And OH‑The catalytic degradation performance under visible light conditions is improved by the two effects, so that the degradation performance of rhodamine B is improved. The preparation method is simple, rapid, green and environment-friendly, and can be used for large-scale production.
Description
Technical Field
The invention belongs to the technical field of semiconductor photocatalysis, and particularly relates to a photocatalyst S-C3N4The preparation method and the application thereof.
Background
Compared with the traditional sewage treatmentIn comparison to physical technologies, Advanced Oxidation Processes (AOPs) are an effective method of degrading pollutants. AOPs are processes that generate and use transition species, primarily hydroxyl radicals. In general, AOPs can be classified as ozone (O)3) Hydrogen peroxide (H) and hydrogen peroxide2O2) Hydrogen peroxide (H) and hydrogen peroxide2O2And O3Combinations of (a) catalytic ozonation, photocatalytic processes associated with oxidation, and Ultrasonic (US) -based AOPs.
In recent years, sulfate type AOPs (S-AOPs) are SO-dependent4-Has higher oxidation-reduction potential, longer service life and wider pH adaptability, and is widely concerned. To date, S-AOPs have been used to treat post-asphalt oxidation wastewater to degrade Volatile Organic Compounds (VOCs) and non-biodegradable compounds. Therefore, the S-AOPs can be an effective technology for degrading dye wastewater such as RhB (rhodamine B).
In general, Persulfate (PS) activation and Peroxymonosulfate (PMS) activation can generate SO4-To prepare the compound. There are various methods for activating PS or PMS, such as ultraviolet radiation, ultrasound, alkalinity, heat, activation of transition metal ions, metal oxides, and carbon-based materials, and the like. Among them, carbon-based materials are widely favored because of their non-toxicity, economy, and good chemical stability.
Graphitic carbon nitride (g-C)3N4) Is considered to be an excellent carbon-based material because it has a narrow band gap, is easy to prepare, has a wide source of raw materials, is inexpensive, and excites g-C with visible light3N4The conduction band electrons of (b) activate the PMS. But block-shaped g-C3N4The catalytic effect is greatly reduced due to factors such as large bulk phase, small specific surface area, few exposed active sites and the like.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a photocatalyst S-C3N4By applying to the massive B-C3N4And carrying out secondary calcination to increase the number of surface active sites of the rhodamine B (RhB), thereby improving the catalytic effect of the rhodamine B (RhB).
The present invention providesA photocatalyst S-C3N4The production method of (2), having such a feature, comprising the steps of: step 1, putting urea as a raw material into a muffle furnace, calcining for 1-3 h at 500-550 ℃ in the air atmosphere to obtain B-C3N4(ii) a Step 2, mixing B-C3N4Placing the mixture in a muffle furnace, calcining the mixture for 1 to 3 hours at the temperature of between 450 and 550 ℃ in the air atmosphere to prepare the photocatalyst S-C3N4。
The photocatalyst S-C provided by the invention3N4The production method of (2) may further have the following features: in the step 1, the urea is placed in a quartz boat and placed in a muffle furnace for calcination.
The invention also provides a photocatalyst S-C3N4Having the feature of being formed by a photocatalyst S-C3N4Is prepared by the preparation method of (1), wherein, the photocatalyst S-C3N4Is of a nanosheet structure.
The invention also provides a photocatalyst S-C3N4Application in catalyzing rhodamine B.
The photocatalyst S-C provided by the invention3N4The application of the compound in catalyzing rhodamine B can also have the following characteristics: wherein, the photocatalyst S-C3N4The application of the catalytic rhodamine B is as follows: adding a photocatalyst S-C into a rhodamine B solution3N4And carrying out dark reaction until the rhodamine B solution reaches adsorption-desorption balance, adding peroxymonosulfate into the rhodamine B solution, and carrying out catalytic degradation on the rhodamine B under the irradiation of a xenon lamp.
The photocatalyst S-C provided by the invention3N4The application of the compound in catalyzing rhodamine B can also have the following characteristics: wherein, rhodamine B and photocatalyst S-C3N4And the mass ratio of the peroxymonosulfate is 2: 15: 2.
the photocatalyst S-C provided by the invention3N4The application of the compound in catalyzing rhodamine B can also have the following characteristics: wherein the Peroxymonosulfate (PMS) is peroxymonosulfatePotassium hydrogen sulfate or potassium hydrogen persulfate.
Action and Effect of the invention
The photocatalyst S-C provided by the invention3N4In the air atmosphere, the urea is used as a raw material and calcined in a muffle furnace to synthesize the B-C3N4Then with B-C3N4The photocatalyst S-C is prepared by secondary calcination of the raw material in a muffle furnace3N4. After secondary calcination, the block B-C is obtained3N4Preparing to obtain the S-C in the shape of nano-flakes3N4. The change from block to ultrathin nanometer sheet can effectively increase the S-C of the semiconductor photocatalyst3N4The active site number on the surface improves the capability of activating PMS, thereby generating more SO4-Greatly improving the capability of photocatalytic degradation of dye wastewater; on the other hand, C3N4The photocatalytic property of the photocatalyst can cause the photocatalyst to generate partial OH-Thereby further promoting the degradation of the dye wastewater. It is used for catalyzing and degrading rhodamine B, thinner S-C3N4The nano-sheet can utilize SO at the same time4-And OH-The catalytic degradation performance under visible light conditions is improved by the two effects, so that the degradation performance of rhodamine B is improved. The preparation method is simple, rapid, green and environment-friendly, can be used for large-scale production, and the catalyst has high-efficiency catalytic performance under the irradiation of visible light.
Drawings
FIG. 1 shows B to C in example 13N4Scanning Electron Micrograph (SEM) of (a);
FIG. 2 shows S-C in example 13N4Scanning Electron Micrograph (SEM) of (a);
FIG. 3 shows S-C in example 13N4X-ray diffraction spectrum (XRD); FIG. 4 is a graph showing the catalytic degradation performance in application examples 1 to 8.
Detailed Description
In order to make the technical means, creation features, achievement objects and effects of the invention easy to understand, the following embodiments and the accompanying drawings are combinedFor a photocatalyst S-C of the present invention3N4The preparation method and the application are specifically described.
The raw materials and reagents used in the following examples can be purchased from conventional commercial sources unless otherwise specified.
The photocatalyst S-C provided by the invention3N4The preparation method specifically comprises the following steps:
step 1, calcining urea serving as a raw material in a muffle furnace to synthesize B-C3N4；
Step 2, mixing B-C3N4Calcining in a muffle furnace to obtain the photocatalyst S-C3N4。
Wherein, in the step 1, the urea is put into a quartz boat and is calcined for 1h to 3h at 500 ℃ to 550 ℃ in a muffle furnace under the air atmosphere to obtain blocky graphite carbon nitride (g-C)3N4) I.e. B-C3N4。
In step 2, B to C are added3N4Calcining the mixture for 1 to 3 hours at the temperature of between 450 and 550 ℃ in a muffle furnace in the air atmosphere to prepare the photocatalyst S-C3N4。
The prepared photocatalyst S-C3N4The rhodamine B catalyst is of a nanosheet structure, and is applied to catalyzing rhodamine B by the following specific operations: adding a photocatalyst S-C3N4 into the rhodamine B solution, carrying out dark reaction until the rhodamine B solution reaches adsorption-desorption balance (namely the absorbance of the rhodamine B solution does not change obviously any more), adding peroxymonosulfate into the rhodamine B solution, and carrying out catalytic degradation on the rhodamine B under the irradiation of a xenon lamp.
Rhodamine B and photocatalyst S-C3N4And the mass ratio of the peroxymonosulfate is 2: 15: 2, the peroxymonosulfate is potassium peroxymonosulfate or potassium peroxymonosulfate.
< example 1>
Step 1, weighing 10g of urea, placing the urea in a quartz boat, covering the quartz boat with a cover, placing the quartz boat in a muffle furnace, calcining the urea at 500-550 ℃ for 2h in the air atmosphere, naturally cooling the urea in the muffle furnace, and cooling the reaction temperature to room temperatureThe solid product of (2) is taken out and collected to obtain blocky graphite carbon nitride (g-C)3N4) I.e. B-C3N4。
Step 2, 0.5g of B-C is taken3N4Putting the quartz boat in a quartz boat, covering the quartz boat with a cover, putting the quartz boat in a muffle furnace, calcining the quartz boat for 2 hours at 450-550 ℃ in the air atmosphere, naturally cooling the quartz boat in the muffle furnace, taking out a solid product in the muffle furnace when the reaction temperature is reduced to room temperature, and collecting the solid product to obtain the photocatalyst S-C3N4。
For B-C obtained in step 13N4And S-C obtained in step 23N4Performing scanning electron microscope detection, and detecting S-C3N4X-ray diffraction detection (XRD) is carried out, and the detection result is shown in figures 1-3.
FIG. 1 shows B to C in example 13N4Scanning Electron Micrograph (SEM) of (a); FIG. 2 shows S-C in example 13N4Scanning Electron Micrograph (SEM) of (a).
As can be seen from FIGS. 1 and 2, after the second calcination, S-C3N4Compared with bulk B-C3N4There are more, thinner nanoplatelets, meaning that there are more exposed active sites.
FIG. 3 shows S-C in example 13N4In which the abscissa represents the 2 theta angle (X-ray incident angle) in degrees (°) and the ordinate represents the diffraction Intensity (Intensity) in a.u.
As can be seen from FIG. 3, two peaks are observed in the graph, indicating a successful conversion of urea to B-C3N4The strong peak at 27.9 degrees corresponds to a (110) crystal face and belongs to an interlaminar stacking structure of aromatic compounds; the weak peak at 13.16 ° corresponds to the (100) plane, belonging to the in-plane repeat period of the triazine ring. After the secondary calcination, the diffraction peak intensity is increased due to thinning of the nanosheet, which proves that S-C3N4The successful preparation.
< comparative example 1>
This comparative example serves as a comparative test to example 1.
Weighing 10g of urea on stonePutting the quartz boat in a muffle furnace after covering the quartz boat with a cover, calcining the quartz boat for 2 hours at 500-550 ℃ in the air atmosphere, naturally cooling the quartz boat in the muffle furnace, taking out solid products in the muffle furnace when the reaction temperature is reduced to room temperature, and collecting the solid products to obtain blocky graphite carbon nitride (g-C)3N4) I.e. B-C3N4。
The photocatalyst S-C prepared in example 13N4And B to C prepared in comparative example 13N4The catalysts were used in application examples 1 to 8, respectively, and the specific experimental operations were as follows. Wherein, the Peroxymonosulfate (PMS) is potassium peroxymonosulfate.
< application example 1>
Firstly, 100mL of 20mg/L rhodamine B (RhB) solution is added into a reactor, and then a photocatalyst S-C is added3N415mg, after dark reaction for 30min, the solution reaches adsorption-desorption balance (namely the absorbance of the rhodamine B solution is not changed obviously any more), then 20mgPMS is added into the solution, a 500W xenon lamp is used, visible light with the wavelength of more than 420nm is selected for irradiation, and the distance between a light source and the reaction system is 10 cm. Samples were taken before the start of the reaction (original RhB solution), after the end of the dark reaction (0min), after 5, 10, 20, 30, 45, 60min of light illumination and the samples were measured by uv spectrophotometer. The degradation results are shown in FIG. 4 at 1.
< application example 2>
Compared with application example 1, the application example adopts 15mg of B-C3N4The same applies to the other conditions for the catalyst. The degradation results are shown in fig. 4, 2.
< application example 3>
Compared with application example 1, the application example adopts 15mg of S-C3N4PMS is not added as a catalyst, and the other conditions are the same. The degradation results are shown in fig. 4, 3.
< application example 4>
Compared with application example 1, the application example adopts 15mg of B-C3N4PMS is not added as a catalyst, and the rest conditions are the same. The degradation results are shown in fig. 4.
< application example 5>
And applications thereofExample 1 in comparison, the present application example used 15mg of S-C3N4As a catalyst, no light irradiation was used, and the other conditions were the same. The degradation results are shown in fig. 4, 5.
< application example 6>
Compared with application example 1, the application example adopts 15mg of B-C3N4As a catalyst, no light irradiation was used, and the other conditions were the same. The degradation results are shown in fig. 4 at 6.
< application example 7>
Compared with the application example 1, the application example adopts 20mg of PMS, does not add a catalyst, has no light irradiation, and has the same other conditions. The degradation results are shown in fig. 4 at 7.
< application example 8>
Compared with the application example 1, the application example adopts visible light irradiation, does not add PMS or catalyst, and has the same other conditions. The degradation results are shown in fig. 4 at 8.
FIG. 4 is a graph showing the catalytic degradation performance in application examples 1 to 8. Wherein the abscissa represents the catalytic reaction time in min and the ordinate represents the degradation rate in%.
As can be seen from FIG. 4, the application examples 5-8 have almost no degradation effect, and the highest degradation rate is only 20%; the degradation effect of the application examples 3 and 4 is improved to 70-90%, and the degradation effect of the application example 1 can reach 100% within 30 min. This fully illustrates the photocatalyst S-C3N4Excellent catalytic degradation performance. Equal amount of S-C3N4Catalysts and B-C3N4Catalyst, S-C, either from the viewpoint of degradation rate or degradation effect3N4The catalytic degradation performance of the catalyst is obviously superior to that of B-C3N4Catalytic degradation performance of (3). And under whatever experimental conditions S-C3N4The catalytic degradation performance of the catalyst is obviously superior to that of B-C3N4Catalytic degradation performance of (3).
Effects and effects of the embodiments
The photocatalyst S-C provided by the embodiment of the invention3N4The preparation method of (1) is that in the air atmosphere, urea is used as raw material and is calcined and synthesized in a muffle furnaceB-C3N4Then with B-C3N4The photocatalyst S-C is prepared by secondary calcination of the raw material in a muffle furnace3N4. After secondary calcination, the block B-C3N4S-C converted into nanosheets3N4. The change from block to ultrathin nanometer sheet can effectively increase the S-C of the semiconductor photocatalyst3N4The active site number on the surface improves the capability of activating PMS, thereby generating more SO4-Greatly improving the capability of photocatalytic degradation of dye wastewater; on the other hand, C3N4The photocatalytic property of the photocatalyst can cause the photocatalyst to generate partial OH-Thereby further promoting the degradation of the dye wastewater. It is used for catalyzing and degrading rhodamine B, thinner S-C3N4The nano-sheet can utilize SO at the same time4-And OH-The catalytic degradation performance under visible light conditions is improved by the two effects, so that the degradation performance of rhodamine B is improved. The preparation method is simple, rapid, green and environment-friendly, can be used for large-scale production, and the catalyst has high-efficiency catalytic performance under the irradiation of visible light.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
In the application example of the invention, potassium Peroxymonosulfate (PMS) is selected to be used, and other peroxymonosulfates can achieve the same technical effect as potassium peroxymonosulfate, such as potassium peroxymonosulfate.
Claims (7)
1. Photocatalyst S-C3N4The preparation method is characterized by comprising the following steps:
step 1, putting urea as a raw material into a muffle furnace, calcining for 1-3 h at 500-550 ℃ in the air atmosphere to obtain B-C3N4；
Step 2, mixing the B-C3N4Placing the mixture in a muffle furnace, calcining the mixture for 1 to 3 hours at the temperature of between 450 and 550 ℃ in the air atmosphere to prepare the photocatalyst S-C3N4。
2. Photocatalyst S-C according to claim 13N4The preparation method is characterized by comprising the following steps:
in the step 1, the urea is placed in a quartz boat and placed in the muffle furnace for calcination.
3. Photocatalyst S-C3N4Characterized by comprising the photocatalyst S-C described in claim 1 or 23N4The preparation method of (A) is to prepare,
wherein the photocatalyst S-C3N4Is of a nanosheet structure.
4. Photocatalyst S-C3N4The application of the photocatalyst in catalyzing rhodamine B is characterized in that the photocatalyst S-C3N4Is a photocatalyst S-C as described in claim 33N4。
5. The photocatalyst S-C of claim 43N4The application of the compound in catalyzing rhodamine B is characterized in that:
wherein the photocatalyst S-C3N4The application of the catalytic rhodamine B is as follows: adding the photocatalyst S-C into a rhodamine B solution3N4And carrying out dark reaction until the rhodamine B solution reaches adsorption-desorption balance, adding peroxymonosulfate into the rhodamine B solution, and carrying out catalytic degradation on the rhodamine B under the irradiation of a xenon lamp.
6. Photocatalyst S-C according to claim 53N4The application of the compound in catalyzing rhodamine B is characterized in that:
wherein, the rhodamine B and the photocatalyst S-C3N4And the mass ratio of the peroxymonosulfate is 2: 15: 2.
7. photocatalyst S-C according to claim 53N4The application of the compound in catalyzing rhodamine B is characterized in that:
wherein the peroxymonosulfate is potassium peroxymonosulfate or potassium peroxymonosulfate.
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