CN110586163A - Preparation method of molybdenum oxide-loaded nitrogen-defect carbon nitride composite photocatalyst - Google Patents
Preparation method of molybdenum oxide-loaded nitrogen-defect carbon nitride composite photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011941 photocatalyst Substances 0.000 title abstract description 9
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title abstract description 8
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910000476 molybdenum oxide Inorganic materials 0.000 title abstract description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001354 calcination Methods 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 7
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 7
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 231100000956 nontoxicity Toxicity 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 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 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical group [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical group [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- BHXXYEMYLOPVDL-UHFFFAOYSA-N [N].O=[Mo] Chemical compound [N].O=[Mo] BHXXYEMYLOPVDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- 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
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- 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
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- 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
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Abstract
The invention discloses a preparation method of a molybdenum oxide-loaded nitrogen-defect carbon nitride composite photocatalyst. Grinding dicyanodiamide, drying, placing into an alumina crucible, covering with a semi-closed cover, heating, calcining, and naturally cooling to room temperature to obtain g-C3N4‑x(ii) a Adding ammonium molybdate into a solution formed by mixing distilled water and ethanol, performing ultrasonic dispersion at room temperature, drying, calcining in a muffle furnace, and cooling to room temperature to obtain MoO3(ii) a Mixing the obtained products, placing the mixture in a muffle furnace for calcining, and naturally cooling to room temperature after the calcining is finished to obtain MoO3/g‑C3N4‑x. The method has the advantages of simple and safe process steps, cheap and easily-obtained raw materials, no toxicity, no harm, convenience for batch production and accordance with environment-friendly requirements. Degradation of RhB under visible light shows excellentPhotocatalytic activity.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a molybdenum oxide-loaded nitrogen-defect carbon nitride composite photocatalyst.
Background
The existing photocatalysis technology is a new pollution treatment technology and has the advantages of high reaction efficiency, mild reaction conditions and the like for the degradation of macromolecular organic pollutants. Carbon nitride (C)3N4) Is a non-metal semiconductor catalyst, and the forbidden band width of the catalyst is 2.7 eV. Wherein the graphite-like carbon nitride (g-C)3N4) Has good chemical stability, safety, no toxicity and low price, and gradually draws the attention of researchers in the field of photocatalysis in recent years. In terms of chemical properties, g-C3N4Has excellent physical property and photoelectric property, and gradually replaces TiO in various fields2And put into use. However, pure g-C3N4The photocatalytic efficiency under visible light is not high, and the reason for this is that g-C3N4The absorption range of visible light is limited, and photo-generated carriers are easy to recombine, so that the photocatalytic activity is reduced. However, the utilization rate of sunlight by the traditional photocatalytic technology is low, and the development of visible light response semiconductor photocatalytic materials is a hot problem in the current photocatalytic research field.
Studies have shown that in g-C3N4Introduction of nitrogen vacancy into the structure to form a nitrogen defect (Nitrogen Deficient, hereinafter referred to as N)4-x) The visible light absorption range of the material and the separating capacity of photon-generated carriers can be expanded, and the photocatalytic efficiency of the material can be effectively improved. Additionally, molybdenum oxide (MoO)3) As a wide-band-gap p-type semiconductor photocatalytic material, the band gap is 2.7-3eV, and visible light can be more fully utilized for photocatalytic degradation. Further, MoO3No toxicity, low preparation cost and good physical and chemical stability. Therefore, MoO3With nitrogen defect g-C3N4(g-C3N4-x) Compounding to prepare molybdenum oxide nitrogen defect carbon nitride (MoO)3/g-C3N4-x) The composite catalyst can effectively improve the visible light utilization efficiency of the photocatalytic material.
Disclosure of Invention
The invention aims to provide MoO3/g-C3N4-xThe preparation method of the composite photocatalyst has the advantages of simple and safe process, cheap and easily-obtained raw materials, no toxicity, no harm, convenience for batch production and environmental friendliness; the obtained catalyst has more excellent visible light absorption capacity and photocatalytic performance, and particularly shows excellent photocatalytic activity when rhodamine B is degraded under visible light.
In order to achieve the purpose, the technical scheme is as follows:
MoO (MoO)3/g-C3N4-xThe preparation method of the composite catalyst comprises the following steps:
1) grinding dicyanodiamide, drying, placing into an alumina crucible, covering with a semi-closed cover, heating, calcining, and naturally cooling to room temperature to obtain g-C3N4-x；
2) Adding ammonium molybdate into a solution formed by mixing distilled water and ethanol, performing ultrasonic dispersion at room temperature, drying, calcining in a muffle furnace, and cooling to room temperature to obtain MoO3；
3) Mixing the products obtained in the step 1 and the step 2, placing the mixture in a muffle furnace for calcining, and naturally cooling to room temperature after the calcining is finished to obtain MoO3/g-C3N4-x。
According to the scheme, the drying temperature in the step 1) is 50-65 ℃.
According to the scheme, the calcining temperature in the step 1) is 600 ℃, the calcining time is 3-5h, and the heating rate is 2-2.5 ℃/min.
According to the scheme, the volume ratio of the distilled water to the ethanol in the step 2) is 1: 1.
According to the scheme, the ultrasonic time in the step 2) is 3-5h, and the power is 90-100W.
According to the scheme, the calcining temperature in the step 2) is 400 ℃, the calcining time is 1.5-2h, and the heating rate is 2-4 ℃/min.
According to the scheme, g-C in step 3)3N4-xAnd MoO3The mass ratio of (1) to (0.01-0.05).
According to the scheme, the calcination temperature in the step 3) is 350-400 ℃, the calcination time is 3-5h, and the heating rate is 2-10 ℃/min.
In order to improve the photocatalytic activity of the material, the invention uses ND-g-C3N4And MoO3Composite, compared with ordinary g-C3N4、MoO3Iso-material, MoO3/g-C3N4-xThe composite material can effectively overcome the defect of high recombination rate of electron-hole, improve the separation efficiency of electron-hole, generate more photoelectrons and improve lightAnd (3) catalytic activity.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a MoO3/g-C3N4-xThe preparation method of the composite photocatalyst has the advantages of simple and safe process steps, cheap and easily-obtained raw materials, no toxicity, no harm, convenience for batch production and environmental friendliness.
MoO prepared by the invention3/g-C3N4-xThe composite photocatalyst is used for degrading rhodamine B (RhB) under visible light. The RhB is degraded under visible light, and the excellent photocatalytic activity is shown.
Drawings
FIG. 1: example 0.01MoO3/g-C3N4-x、0.003MoO3/g-C3N4-x、0.005MoO3/g-C3N4-xWith MoO3、g-C3N4-x、g-C3N4Comparing the degradation effect of RhB;
FIG. 2: example 2 g-C3N4-x(a)、MoO3(b)、0.03MoO3/g-C3N4-x(c) TEM image of (A), and 0.03MoO3/g-C3N4-xThe HAADF-STEM diagram of (d. distribution of all elements; e.Mo; f.O);
FIG. 3: example 0.01MoO3/g-C3N4-x、0.03MoO3/g-C3N4-x、0.05MoO3/g-C3N4-xWith MoO3、g-C3N4-x、g-C3N4XRD test analysis result of (1);
FIG. 4: example 0.01MoO3/g-C3N4-x、0.03MoO3/g-C3N4-x、0.05MoO3/g-C3N4-xWith MoO3、g-C3N4-xThe analysis result of the Uv-vis test of (1);
FIG. 5: example 2 0.03MoO3/g-C3N4-xXPS test results of (a. full spectrum, b.c1s, c.n1s, d.mo3d e.o1s); g-C3N4-xAnd MoO3XPS valence band spectrum (f);
FIG. 6: example 2 0.03MoO3/g-C3N4-x、MoO3、g-C3N4-xAnd g-C3N4The ESR analysis result (a. superoxide radical signal; b. hydroxyl radical signal) of (1).
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
Step 1: grinding 5g of dicyandiamide, placing the ground dicyandiamide in a 50 ℃ oven for drying for 12h, placing the ground dicyandiamide in an alumina crucible, placing the alumina crucible in a muffle furnace for calcining, wherein the calcining temperature is 600 ℃, the calcining time is 3h, and the heating rate is 2 ℃/min. Naturally standing after calcining and sintering, cooling to room temperature, and grinding to obtain powdery g-C3N4-x；
Step 2: putting 1g of ammonium molybdate into a mixed solution of distilled water and ethanol in a volume ratio of 1:1, ultrasonically oscillating for 3h (90W), drying, and then putting into a muffle furnace for calcining at 400 ℃ for 1.5h at a heating rate of 2 ℃/min to obtain MoO3；
And step 3: 1g of g-C obtained in step 1 are taken3N4-xAnd 0.01g of MoO obtained in step 23Uniformly mixing, calcining in a muffle furnace at 350 deg.C for 3h at 2 deg.C/min, and naturally cooling to room temperature to obtain 0.01MoO3/g-C3N4-x。
Example 2
Step 1: grinding 5g of dicyandiamide, placing the ground dicyandiamide in a 60 ℃ oven for drying for 12h, placing the ground dicyandiamide in an alumina crucible, placing the alumina crucible in a muffle furnace for calcining, wherein the calcining temperature is 600 ℃, the calcining time is 4h, and the heating rate is 2.5 ℃/min. Naturally standing after calcining and sintering, cooling to room temperature, and grinding to obtain powdery g-C3N4-x；
Step 2: 1g of ammonium molybdate is put into a mixed solution of distilled water and ethanol with the volume ratio of 1:1, the solution is ultrasonically vibrated for 4 hours (100W), and the ammonium molybdate is dried and then placedCalcining in a muffle furnace at 400 ℃ for 1.8h at a heating rate of 3 ℃/min to obtain MoO3；
And step 3: 1g of g-C obtained in step 1 are taken3N4-xAnd 0.03g of MoO obtained in step 23Uniformly mixing, placing in a muffle furnace for calcining at 375 ℃ for 4h at a heating rate of 2 ℃/min, and naturally cooling to room temperature after calcining to obtain 0.03MoO3/g-C3N4-x。
Example 3
Step 1: grinding 5g of dicyandiamide, placing the ground dicyandiamide in a 65 ℃ oven for drying for 12h, placing the ground dicyandiamide in an alumina crucible, placing the alumina crucible in a muffle furnace for calcining, wherein the calcining temperature is 600 ℃, the calcining time is 5h, and the heating rate is 2.5 ℃/min. Naturally standing after calcining and sintering, cooling to room temperature, and grinding to obtain powdery g-C3N4-x；
Step 2: putting 1g of ammonium molybdate into a mixed solution of distilled water and ethanol in a volume ratio of 1:1, ultrasonically oscillating for 5h (100W), drying, and then putting into a muffle furnace for calcining at 400 ℃ for 2h at a heating rate of 4 ℃/min to obtain MoO3；
And step 3: 1g of g-C obtained in step 1 are taken3N4-xAnd 0.05g of MoO obtained in step 23Uniformly mixing, calcining in a muffle furnace at 400 deg.C for 5h at a temperature rise rate of 5 deg.C/min, and naturally cooling to room temperature to obtain 0.05MoO3/g-C3N4-x。
Example 4
Step 1: grinding 5g dicyanodiamide, placing the ground dicyanodiamide in a 65 ℃ oven for drying for 12h, placing the dried dicyanodiamide in an alumina crucible, calcining for 4h at 600 ℃, and raising the temperature at the rate of 2.5 ℃/min. Naturally standing after calcining and sintering, cooling to room temperature, and grinding to obtain powdery g-C3N4。
As shown in FIG. 1, the reaction conditions were 0.01g of 0.01MoO obtained in example 1, example 2 and example 3, respectively3/g-C3N4-x、0.03MoO3/g-C3N4-x、0.05MoO3/g-C3N4-x、MoO3、g-C3N4-xAnd g-C3N4. The light source used is a 500W long-arc xenon lamp, and the solution is 100mL of 10mg/L RhB solution. From the decrease in the RhB solution concentration, 0.01MoO can be seen3/g-C3N4-x、0.03MoO3/g-C3N4-xAnd 0.05MoO3/g-C3N4-xThe degradation rate of RhB is remarkably improved, wherein 0.003MoO3/g-C3N4-xThe effect is optimal.
As shown in FIG. 2, 0.03MoO is observed by TEM3/g-C3N4-xCubic crystal form MoO in composite material3The crystals are interpenetrated in layers g-C3N4-xThe surface of the material. In addition, at 0.03MoO3/g-C3N4-xCan be seen in the HAADF-STEM diagram of (A), at 0.03MoO3/g-C3N4-xMo and O are uniformly distributed on the composite material, and MoO is further proved3And g-C3N4-xThe two materials are successfully compounded together, and the original structure and appearance of the two substances are not influenced.
As shown in FIG. 3, it can be seen from the XRD data that the MoO at 0.01MoO3/g-C3N4-x、0.03MoO3/g-C3N4-x、0.05MoO3/g-C3N4-x、MoO3And g-C3N4-xg-C was observed in all3N4-xThe PDF card number is 87-1526; at 0.05MoO3/g-C3N4-xIn which significant MoO was observed3The number of the PDF card is 35-0609; 0.01MoO3/g-C3N4-xAnd 0.03MoO3/g-C3N4-xIn the middle, it is not easy to observe MoO3The main reason for the diffraction peaks matching with the characteristic peaks of the crystals is that the doping amount is extremely low, so that the diffraction peaks are too small to be observed easily.
As shown in FIG. 4, MoO can be seen from the Uv-vis data3Has an absorption edge of about 430nm and different MoO ratios3/g-C3N4-xComposite materialAbsorption edge of (2) and g-C3N4-xClose, all are about 500 nm; in addition, the forbidden band width is calculated through a Kubelka-Munk formula in the right graph, and MoO can be obtained3The forbidden band width of (A) is 2.94 eV.
As shown in FIG. 5, it can be seen from the XPS chart that four elements of C, N, Mo and O are all present in 0.03MoO3/g-C3N4-xIn a composite material. Wherein the binding energy of C1s is 286.04Ev, which can be considered to constitute a C-N bond; the binding energies of N1s at 396.62 and 398.32eV correspond to C-N bond and sp, respectively3A hybridized N atom; mo and g-C3N4-xCompounding of (2) with O1s and Mo3d3/2And Mo3d5/2The peaks of (a) produce a shift and convolution phenomena, indicating that the recombination of the material changes the electron density and the local environment around the element. UPS test result shows MoO3And g-C3N4-xThe valence bands of (a) are 2.90 and 1.64eV, respectively.
As shown in FIG. 6, the ESR measurement result showed 0.03MoO3/g-C3N4The-x composite photocatalyst generates superoxide radical and hydroxyl radical in the process of photocatalytic reaction; and the response capability of the two free radicals is obviously stronger, which proves that more free radicals are generated, and indirectly proves that 0.03MoO3/g-C3N4The-x composite photocatalyst has higher photocatalytic activity.
Claims (8)
1. MoO (MoO)3/g-C3N4-xThe preparation method of the composite catalyst is characterized by comprising the following steps:
1) grinding dicyanodiamide, drying, placing into an alumina crucible, covering with a semi-closed cover, heating, calcining, and naturally cooling to room temperature to obtain g-C3N4-x；
2) Adding ammonium molybdate into a solution formed by mixing distilled water and ethanol, performing ultrasonic dispersion at room temperature, drying, calcining in a muffle furnace, and cooling to room temperature to obtain MoO3；
3) Mixing the products obtained in the step 1 and the step 2, placing the mixture in a muffle furnace for calcining, and naturally cooling to room temperature after the calcining is finished to obtain MoO3/g-C3N4-x。
2. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the drying temperature in the step 1) is 50-65 ℃.
3. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the calcining temperature in the step 1) is 600 ℃, the calcining time is 3-5h, and the heating rate is 2-2.5 ℃/min.
4. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the volume ratio of distilled water to ethanol in the step 2) is 1: 1.
5. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the ultrasonic time in the step 2) is 3-5h, and the power is 90-100W.
6. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the calcining temperature in the step 2) is 400 ℃, the calcining time is 1.5-2h, and the heating rate is 2-4 ℃/min.
7. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that g-C in the step 3)3N4-xAnd MoO3The mass ratio of (1) to (0.01-0.05).
8. The MoO of claim 13/g-C3N4-xThe preparation method of the composite catalyst is characterized in that the calcination temperature in the step 3) is 350-400 ℃, the calcination time is 3-5h, and the heating rate is 2-5 ℃/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111437866A (en) * | 2020-04-28 | 2020-07-24 | 陕西科技大学 | Double-defect heterojunction photocatalyst and preparation method and application thereof |
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| CN111545169A (en) * | 2020-05-19 | 2020-08-18 | 西南科技大学 | Method for preparing hypha/molybdenum oxide adsorption-catalysis material by utilizing biological enrichment |
| CN111545169B (en) * | 2020-05-19 | 2022-05-17 | 西南科技大学 | Method for preparing hypha/molybdenum oxide adsorption-catalysis material by utilizing biological enrichment |
| CN111807336A (en) * | 2020-07-18 | 2020-10-23 | 郑州航空工业管理学院 | Amorphous molybdenum oxide nanodot/two-dimensional carbon nitride nanosheet with photocatalysis and photothermal conversion performances and preparation method thereof |
| CN111807336B (en) * | 2020-07-18 | 2022-12-20 | 郑州航空工业管理学院 | Amorphous molybdenum oxide nanodot/two-dimensional carbon nitride nanosheet with photocatalysis and photothermal conversion performances and preparation method thereof |
| CN111974433A (en) * | 2020-07-30 | 2020-11-24 | 徐州工程学院 | Preparation method and application of mortise and tenon structure composite photocatalytic material |
| CN111974433B (en) * | 2020-07-30 | 2022-10-25 | 徐州工程学院 | Preparation method and application of mortise and tenon structure composite photocatalytic material |
| CN114210354A (en) * | 2021-09-22 | 2022-03-22 | 吉林医药学院 | Method for improving graphite phase carbon nitride photocatalytic performance |
| CN113751048A (en) * | 2021-10-15 | 2021-12-07 | 阜阳师范大学 | Molybdenum trioxide in-situ intercalation carbon nitride composite catalyst and preparation method thereof |
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