CN113769772B - Hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 Photocatalytic material and preparation method and application thereof - Google Patents
Hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 Photocatalytic material and preparation method and application thereof Download PDFInfo
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract description 3
- 229910000484 niobium oxide Inorganic materials 0.000 abstract description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 abstract description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000010955 niobium Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
The invention discloses Nb-Mo codoped g-C treated by hydrochloric acid 3 N 4 A photocatalytic material, a preparation method and application thereof. Adding niobium oxide and molybdenum oxide powder into distilled water, then adding melamine, magnetically stirring at 80 ℃, and performing ultrasonic treatment to obtain a mixed solution; dropwise adding a hydrochloric acid solution into the obtained mixed solution, uniformly stirring by magnetic force, and drying to obtain a precursor; grinding the precursor, and calcining at high temperature in nitrogen atmosphere to obtain the target product Nb-Mo/g-C 3 N 4 A photocatalytic material. Nb-Mo ion co-doping g-C treated by hydrochloric acid prepared by using method of the invention 3 N 4 Photocatalytic material, improved g-C 3 N 4 The method has the advantages of low cost and easy operation, and can degrade organic pollutants by natural light under the condition of natural light.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to high-activity Nb-Mo/g-C 3 N 4 A photocatalytic material and a preparation method and application thereof.
Background
Over the past decades, excessive emissions of toxic gases have created serious environmental problems that threaten human health. Various adsorbents have been studied to detect and remove toxic gases. Wherein the graphite carbon nitride (g-C) 3 N 4 ) A graphene-like porous layered material has attracted much interest because of its ease of synthesis, attractive electronic band structure, non-toxicity and high stability. Such organic semiconductors have shown tremendous potential applications in a variety of fields, including photocatalytic water splitting, photoreduction of carbon dioxide, organic pollutantsPhotolysis, solar energy conversion, and sensors. However, its inherent structure results in high electron-hole recombination rate and low photocatalytic activity, limiting its industrial application.
Disclosure of Invention
To solve the above problems, it is an object of the present invention to provide a hydrochloric acid-treated Nb-Mo co-doped g-C 3 N 4 The method is easy to operate, simple, convenient, low in cost, mild in condition and favorable for large-scale production.
The technical scheme adopted by the invention is as follows: hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The photocatalytic material is doped with 0.25-0.5% of Nb ions and Mo ions in molar percentage, wherein the ratio of Nb ions to Mo ions = 1.
Hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The preparation method of the photocatalytic material comprises the following steps:
1) Adding niobium oxide and molybdenum oxide powder into distilled water, then adding melamine, magnetically stirring at 80 ℃, and performing ultrasonic treatment to obtain a mixed solution;
2) Dropwise adding a hydrochloric acid solution into the mixed solution obtained in the step 1), uniformly stirring by magnetic force, and drying to obtain a precursor;
3) Grinding the precursor, and calcining at high temperature in nitrogen atmosphere to obtain the target product Nb-Mo/g-C 3 N 4 A photocatalytic material.
Further, in the above preparation method, step 1), the niobium oxide is Nb 2 O 5 (ii) a The molybdenum oxide is MoO 3 。
Further, the above-mentioned preparation process, step 1), is carried out in a molar ratio of Nb 2 O 5 :MoO 3 Melamine = (0.00125-0.0025): 0.0025-0.005): 1.
Further, in the preparation method, step 2), the drying temperature is 80 ℃.
Further, in the above preparation method, the molar ratio of hydrochloric acid to melamine = 0.345.
Further, in the above preparation method, step 3), the high temperature calcination is carried out at 550 ℃ for 2h.
Further, in the preparation method, the heating rate of the high-temperature calcination is 3 ℃/min.
The invention provides hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The application of the photocatalytic material in the catalytic degradation of gas pollutants under visible light.
Further, the gaseous contaminant is isopropanol.
The invention has the beneficial effects that:
1. the invention provides hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The photocatalytic material successfully constructs a doping structure with larger specific surface area, the structure can more easily move charges, and the photocatalytic activity can be effectively improved.
2. The hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The preparation method of the photocatalytic material has the advantages of cheap and easily obtained raw materials, simple and convenient operation, greatly reduced cost, no toxicity, no environmental pollution and green chemistry.
3. The invention increases g-C 3 N 4 The specific surface area of (a) is to improve photocatalytic performance by increasing reaction sites and promoting bulk charge separation. In order to obtain a larger specific surface area, modification and doping are effective and simple methods for improving the photocatalytic performance, because the modification and doping can cause the change of the specific surface area, the invention adopts Nb-Mo ion co-doping to generate lattice defects, so that atoms in lattices are easier to migrate, the sensitivity to visible light is further improved, and the photocatalytic reaction efficiency is improved.
Drawings
FIG. 1 shows 0.5% of Nb-Mo/g-C of the photocatalyst prepared in example 1 3 N 4 、0.25％Nb-Mo/g-C 3 N 4 And pure g-C 3 N 4 XRD comparison pattern of (a).
FIG. 2 shows the 0.5% Nb-Mo/g-C ratio of different photocatalysts of example 2 3 N 4 、0.25％Nb-Mo/g-C 3 N 4 And pure g-C 3 N 4 The acetone production rate of (2) is shown in the graph.
Detailed Description
Example 1
Hydrochloric acid treated Nb-Mo codoped g-C 3 N 4 Photocatalytic Material (0.5% by volume Nb-Mo/g-C 3 N 4 )
The preparation method comprises the following steps:
1) Adding 0.0093g (0.0001 mol) Nb 2 O 5 And 0.0288g (0.0002 mol) of MoO 3 Adding the mixture into 45.5mL of distilled water, then adding 5g (0.04 mol) of melamine, magnetically stirring the mixture for 1h at the temperature of 80 ℃, and performing ultrasonic treatment for 1h to obtain a mixed solution;
2) Dropwise adding 4.5mL of hydrochloric acid solution into the mixed solution obtained in the step 1), uniformly stirring by magnetic force, putting into a drying oven, and drying at 80 ℃ for 12h to obtain a precursor;
3) Grinding the precursor obtained in the step 2), heating to 550 ℃ at the heating rate of 3 ℃/min in the nitrogen environment, and calcining at 550 ℃ for 2h to obtain the target product Nb-Mo co-doped g-C treated by hydrochloric acid 3 N 4 Photocatalytic material, in mol%, containing 0.5% of Nb and Mo, sample designation 0.5% 3 N 4 。
(II) hydrochloric acid treated Nb-Mo Co-doping g-C 3 N 4 Photocatalytic Material (0.25% Nb-Mo/g-C 3 N 4 )
The preparation method comprises the following steps:
1) 0.0046g (0.00005 mol) of Nb 2 O 5 And 0.0144g (0.0001 mol) MoO 3 Adding the mixture into 45.5mL of distilled water, then adding 5g (0.04 mol) of melamine, magnetically stirring the mixture for 1h at the temperature of 80 ℃, and performing ultrasonic treatment for 1h to obtain a mixed solution;
2) Dropwise adding 4.5mL of hydrochloric acid solution into the mixed solution obtained in the step 1), magnetically stirring uniformly, putting into a drying oven, and drying for 12 hours at 80 ℃ to obtain a precursor;
3) Grinding the precursor obtained in the step 2), heating to 550 ℃ at a heating rate of 3 ℃/min in a nitrogen environment, and calcining at 550 ℃ for 2h to obtain the target product, namely the Nb-Mo co-doped g-C treated by hydrochloric acid 3 N 4 Photocatalytic material, in mol%, containing 0.25% of Nb and Mo, sample number 0.25％Nb-Mo/g-C 3 N 4 。
(III) comparative example pure g-C 3 N 4 Photocatalytic material
The preparation method comprises the following steps: placing 5g of melamine in a crucible, heating to 550 ℃ at the heating rate of 3 ℃/min in a nitrogen environment, and calcining for 2h to obtain pure g-C 3 N 4 A photocatalytic material.
(IV) detection
FIG. 1 shows the content of Nb-Mo/g-C in sample 0.5% 3 N 4 Sample 0.25% Nb-Mo/g-C 3 N 4 And pure g-C 3 N 4 XRD test pattern of (1), sample 2.5% 3 N 4 And sample 0.5% Nb-Mo/g-C 3 N 4 Two diffraction peaks at 13.1 ℃ and 27.3 ℃ with pure g-C 3 N 4 Diffraction peaks coincide, and the main peak of the doped g-C3N4 catalyst still remains, indicating that the crystal structure is not changed. No compounds of Nb and Mo were observed in the doped g-C3N4 material, indicating that Nb and Mo are embedded in the g-C3N4 crystal planes in ionic form.
Example 2 application
Effect of different catalysts on catalytic degradation of isopropanol under visible light
The test process is as follows: filtering out ultraviolet simulated sunlight with 300W xenon lamp as light source, adjusting photocurrent to 18mA position, adjusting light intensity center to irradiate sample surface, fixing position, and respectively removing the residue from the sample by 0.5% Nb-Mo/g-C prepared in example 1 3 N 4 、 0.25％Nb-Mo/g-C 3 N 4 And pure g-C 3 N 4 Is placed in a 4cm container 2 In the glass tank, the glass tanks carrying the photocatalyst were placed in 325cm each 3 And finally, injecting 5ul of isopropanol liquid into the reactor, waiting for 2 hours until the isopropanol is completely volatilized into gas, starting timing after 20 minutes of illumination, and extracting one needle of the sample every 20 minutes for testing. The peak area of acetone generated by degrading isopropanol is recorded, and the concentration change point line graph of acetone generated by degrading isopropanol is calculated, and the result is shown in figure 2.
As can be seen from FIG. 2, the hydrochloric acid treatment produced according to the present invention had a content of 0.5% of Nb-Mo/g-C 3 N 4 g photo catalytic material has an acetone generation concentration which continuously increases along with time and is all higher than pure g-C 3 N 4 The effect is good. g-C prepared by the invention 3 N 4 Not only improves the photocatalytic activity, but also improves the yield to 1.5 times, improves the g-C 3 N 4 Photocatalytic performance.
Claims (4)
1. Hydrochloric acid treated Nb-Mo co-doped g-C 3 N 4 The preparation method of the photocatalytic material is characterized in that the Nb-Mo codoped g-C treated by hydrochloric acid 3 N 4 The photocatalytic material is doped with 0.5 percent of Nb ions and Mo ions according to molar percentage, wherein the Nb ions and the Mo ions are in a molar ratio of (1):
1) Mixing Nb with 2 O 5 And MoO 3 Adding the powder into distilled water, then adding melamine, magnetically stirring at 80 ℃, and performing ultrasonic treatment to obtain a mixed solution; in terms of mole ratio, nb 2 O 5 : MoO 3 Melamine = 0.00125-0.0025: 0.0025-0.005: 1;
2) Dropwise adding a hydrochloric acid solution into the mixed solution obtained in the step 1), uniformly stirring by magnetic force, and drying to obtain a precursor; hydrochloric acid to melamine =0.345 to 1 in molar ratio;
3) Grinding the precursor, and calcining at 550 ℃ for 2h in nitrogen atmosphere to obtain the target product Nb-Mo/g-C 3 N 4 A photocatalytic material.
2. The method of claim 1, wherein the drying temperature in step 2) is 80 ℃.
3. The method of claim 1, wherein the high temperature calcination is carried out at a temperature increase rate of 3 ℃/min.
4. Hydrochloric acid treated Nb-Mo co-doped g-C prepared according to the method of claim 1 3 N 4 Use of a photocatalytic material for the catalytic degradation of gaseous pollutants under visible light, characterized in that said gas isThe contaminant is isopropanol.
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