CN110652995A - VC/g-C3N4Method for preparing photocatalyst - Google Patents
VC/g-C3N4Method for preparing photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- 238000001354 calcination Methods 0.000 claims abstract description 43
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 10
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 10
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 10
- 239000008103 glucose Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 48
- 229910052573 porcelain Inorganic materials 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 238000011068 loading method Methods 0.000 claims description 18
- 238000007873 sieving Methods 0.000 claims description 18
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 18
- 239000001257 hydrogen Substances 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 16
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
VC/g-C3N4The preparation method of the photocatalyst comprises the steps of mixing and grinding dicyandiamide, ammonium bicarbonate and ammonium metavanadate uniformly, calcining in a tubular furnace, and ball-milling to obtain VC powder; mixing and grinding VC powder, citric acid, glucose and dicyandiamide, and calcining in a tubular furnace; ball milling after calcining to obtain VC/g-C3N4A photocatalyst. The raw materials of the invention form g-C after being calcined by a tube furnace3N4A substrate, wherein VC is uniformly attached on the substrate to form a nano-scale photocatalyst phase VC/g-C3N4The composite material has the advantages of simple preparation process, easily controlled conditions, low production cost and easy industrial production. The introduced VC cocatalyst can be used for increasing active sites during photocatalytic hydrogen production and improving the hydrogen production efficiency.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to VC/g-C3N4A preparation method of the photocatalyst.
Background
In order to meet the increasingly serious challenges of energy shortage and environmental pollution, the development of renewable energy and clean energy is a continuous pursuit of the scientific and technological community, the production of the photocatalytic technology just accords with the sustainable development concept, and the research and development of low-cost and high-performance photocatalytic materials are the subject to be urgently explored by researchers.
Various types of photocatalysts have been developed to date, and g-C was confirmed by the subject group of professor morning in the morning of the university of Fuzhou3N4Non-metallic semiconductors can catalyze the production of hydrogen from water under illumination [ Wang, x; maeda, k.; thomas, a.; takanabe, k.; xin, g.; carlsson, j.m.; domen, k.; antonietti, M.A Metal-Free polymeric Photocatalyst for Hydrogen Production from Water under Visiblelight. Nat. Mater.2009,8,76-80.]，g-C3N4Is widely used in the field of photocatalysis. It is a polymer composed of elements abundant on earth, and has a suitable forbidden band width suitable for absorbing and utilizing visible light, and is excellent in thermal stability and chemical stability. The material has important application in photoelectrochemical energy conversion and energy storage materials, including solar cells, ion batteries, catalysts, supercapacitors and detectors, and the like [ Liu, J., Wang, H., Antonietti, M.Graphic carbon nitride "loaded": insulating applications beyond and/or in catalysis],2016,45(8):2308-2326]。
However, the rapid recombination of photogenerated electron-hole pairs greatly reduces the photocatalytic performance, scientists are constantly exploring various modification methods to improve g-C3N4Efficiency of photolyzing water to produce hydrogen, such as increasing defect vacancies to increase active sites thereof to increase hydrogen production [ Junying Liu, Wenjian Fan, Zhododong Wei, et, al3N4 achieved by a molten salt post-treatment approach[J].Applied Catalysis B:Environmental,18July 2018,0296-3373]Or introducing other semiconductor material and compounding to reduce forbidden band width, so as to expand the absorption range of visible light to improve hydrogen generation [ Kelin He, Jun Xie, Zhuohong Yang, et, al2 production over g-C3N4 nanosheets under visible light[J].Catalysis Science&Technology,2017,7,1193]。
Disclosure of Invention
The invention aims to provide VC/g-C with simple preparation process and photocatalytic hydrogen production capability3N4A preparation method of the photocatalyst. I.e. the raw material is calcined to form g-C3N4The substrate and VC are uniformly attached to the substrate to form a nano-scale photocatalyst phase.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 1 to 8: (1-5): (1-6) mixing to obtain a mixture;
2) grinding the mixture evenly, sieving the mixture by a 40-60 mesh sieve, loading the mixture into a porcelain boat, and heating the porcelain boat from room temperature to 400-1200 ℃ in a tubular furnace at the heating rate of 2-10 ℃/min for calcination;
3) calcining, naturally cooling with a furnace, and ball-milling to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 1-6: (1-4): (1-5): (2-8) mixing the raw materials according to the mass ratio to obtain a mixture;
5) grinding the mixture, sieving with a 40-60 mesh sieve, loading into a porcelain boat, and calcining at the temperature rising rate of 2-10 ℃/min from room temperature to 350-900 ℃ in a tube furnace;
6) calcining, naturally cooling with the furnace, and ball milling to obtain VC/g-C3N4A photocatalyst.
The grinding time of the step 2) is 60-80 min.
The calcination time of the step 2) is 1-6 h.
And 3) ball-milling for 3h-5h at the rotating speed of 200rpm-400rpm, and ball-milling for 4h-10h at the rotating speed of 400rpm-600rpm to obtain VC powder.
The grinding time of the step 5) is 70-120 min.
The calcination time of the step 5) is 1-5 h.
The ball milling in the step 6) is carried out for 4h-8h at the rotating speed of 300rpm-800 rpm.
The preparation method of the invention has the following beneficial effects:
1. the raw materials of the invention form g-C after being calcined by a tube furnace3N4A substrate, wherein VC is uniformly attached on the substrate to form a nano-scale photocatalyst phase VC/g-C3N4The composite material has the advantages of simple preparation process, easily controlled conditions, low production cost and easy industrial production.
2. The invention provides a method for preparing VC/g-C3N4The method of (2) forms a porous g-C3N4The nano-sheet can be used for increasing active sites during photocatalytic hydrogen production and improving the hydrogen production efficiency.
3. VC/g-C prepared by the invention3N4The composite material has a photocatalytic function, can perform photolysis on water to produce hydrogen after 2 hours under the illumination condition, and adopts LabSolar 6A equipment to carry out VC/g-C3N4And (4) carrying out a photocatalysis effect test, wherein the test result shows that the photocatalyst has the capability of hydrolyzing water to produce hydrogen.
Drawings
FIG. 1 shows VC/g-C prepared in example 1 of the present invention3N4X-ray diffraction analysis diagram, in which the abscissa is the 2 θ angle and the ordinate is the absorption intensity.
FIG. 2a is VC/g-C prepared in example 1 of the present invention3N4Scan at 400 nm.
FIG. 2b shows VC/g-C prepared in example 1 of the present invention3N4Scanning at 100 nm.
FIG. 3 is VC/g-C prepared in example 1 of the present invention3N4The hydrogen production performance diagram of (1), wherein the abscissa is the number of samples and the ordinate is the hydrogen production.
The specific implementation mode is as follows:
example 1:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 1: 3: 2 to obtain a mixture;
2) grinding the mixture for 60min, sieving with a 60-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 2 ℃/min from room temperature to 600 ℃ for 3 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 5 hours at the rotating speed of 200rpm, and then ball-milling for 4 hours at the speed of 500rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 1: 3: 2: 5 to obtain a mixture;
5) grinding the mixture for 100min, sieving with a 60-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 2 ℃/min from room temperature to 450 ℃ for 2 h;
6) after calcining, naturally cooling along with the furnace, and ball-milling for 4 hours at the rotating speed of 400rpm to obtain VC/g-C3N4A photocatalyst.
FIG. 1 shows VC/g-C3N4X-ray diffraction patterns of (1) at 13 ℃ and 27 ℃ respectively corresponding to g-C3N4The (100) and (002) crystal planes of (a) and (b), and VC/g-C3N4Can accurately correspond to VC PDF #73-0476, and shows that VC/g-C is successfully prepared3N4A photocatalyst.
FIG. 2 shows VC/g-C3N4A figure shows the sheet-like and perforated g-C3N4In an amorphous state, VC is attached in bulk to g-C3N4On the upper, b is a partial enlarged view of a diagram a, which more clearly shows that the block VC is flaky and porous g-C3N4Further indicates successful preparation of VC/g-C3N4A photocatalyst.
FIG. 3 shows VC/g-C3N4In which the pure phases g-C3N4The hydrogen production performance is 10.6 mu molg-1h-1Pure phase VC detects no hydrogen production, but successfully compounds VC/g-C3N4The hydrogen production performance is 260.4 mu molg-1h-1Hydrogen generating performance toolThe improvement is obvious.
Example 2:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 1: 4: 3, mixing to obtain a mixture;
2) grinding the mixture for 70min, sieving with a 50-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 2 ℃/min from room temperature to 500 ℃ for 2 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 5 hours at the rotating speed of 200rpm, and then ball-milling for 4 hours at the speed of 500rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 1: 2: 2: 3, mixing to obtain a mixture;
5) grinding the mixture for 70min, sieving with a 50-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 5 ℃/min from room temperature to 500 ℃ for 3 h;
6) after calcining, naturally cooling the mixture along with the furnace, and ball-milling the mixture for 6 hours at the rotating speed of 500rpm to obtain VC/g-C3N4A photocatalyst.
Example 3:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 1: 3: 5 to obtain a mixture;
2) grinding the mixture for 65min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 5 ℃/min from room temperature to 800 ℃ for 2 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 4h at the rotating speed of 300rpm, and then ball-milling for 4h at the speed of 600rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 2: 2: 4: 6 to obtain a mixture;
5) grinding the mixture for 90min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rising rate of 10 ℃/min from room temperature to 600 ℃ for 4 h;
6) after calcining, naturally cooling the mixture along with the furnace, and ball-milling the mixture for 4 hours at the rotating speed of 600rpm to obtain VC/g-C3N4A photocatalyst.
Example 4:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 3: 1: 4 to obtain a mixture;
2) grinding the mixture for 80min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 8 ℃/min from room temperature to 400 ℃ for 6 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 3h at the rotating speed of 400rpm, and then ball-milling for 10h at the speed of 600rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 4: 4: 3: 4 to obtain a mixture;
5) grinding the mixture for 110min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rising rate of 8 ℃/min from room temperature to 900 ℃ for 1 h;
6) after calcining, naturally cooling the mixture along with the furnace, and ball-milling the mixture for 8 hours at the rotating speed of 300rpm to obtain VC/g-C3N4A photocatalyst.
Example 5:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 5: 3: 1 to obtain a mixture;
2) grinding the mixture for 75min, sieving with a 60-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 4 ℃/min from room temperature to 1200 ℃ for 1 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 4h at the rotating speed of 300rpm, and then ball-milling for 8h at the speed of 500rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 6: 3: 5: 8 to obtain a mixture;
5) grinding the mixture for 80min, sieving with a 60-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 6 ℃/min from room temperature to 800 ℃ for 2 h;
6) after calcining, naturally cooling along with the furnace, and ball-milling for 5 hours at the rotating speed of 700rpm to obtain VC/g-C3N4A photocatalyst.
Example 6:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 8: 5: 6 to obtain a mixture;
2) grinding the mixture for 80min, sieving with a 50-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rise rate of 6 ℃/min from room temperature to 1000 ℃ for 3 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 5 hours at the rotating speed of 200rpm, and then ball-milling for 6 hours at the speed of 400rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 3: 1: 1: 2 to obtain a mixture;
5) grinding the mixture for 120min, sieving with a 50-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rising rate of 3 ℃/min from room temperature to 350 ℃ for 5 h;
6) after calcining, naturally cooling the mixture along with the furnace, and ball-milling the mixture for 6 hours at the rotating speed of 500rpm to obtain VC/g-C3N4A photocatalyst.
Example 7:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 6: 2: 3, mixing to obtain a mixture;
2) grinding the mixture for 70min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rising rate of 10 ℃/min from room temperature to 900 ℃ for 5 h;
3) after calcining, naturally cooling along with the furnace, ball-milling for 3h at the rotating speed of 300rpm, and then ball-milling for 5h at the speed of 400rpm to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 5: 2: 3: 7 to obtain a mixture;
5) grinding the mixture for 100min, sieving with a 40-mesh sieve, loading into a porcelain boat, and calcining in a tube furnace at a temperature rising rate of 9 ℃/min from room temperature to 700 ℃ for 2 h;
6) after calcining, naturally cooling along with the furnace, and ball-milling at the rotating speed of 800rpm for 4 hours to obtain VC/g-C3N4A photocatalyst.
Claims (7)
1. VC/g-C3N4The preparation method of the photocatalyst is characterized by comprising the following steps:
1) firstly, according to the weight ratio of dicyandiamide: ammonium bicarbonate: ammonium metavanadate ═ 1 to 8: (1-5): (1-6) mixing to obtain a mixture;
2) grinding the mixture evenly, sieving the mixture by a 40-60 mesh sieve, loading the mixture into a porcelain boat, and heating the porcelain boat from room temperature to 400-1200 ℃ in a tubular furnace at the heating rate of 2-10 ℃/min for calcination;
3) calcining, naturally cooling with a furnace, and ball-milling to obtain VC powder;
4) according to VC powder: citric acid: glucose: dicyandiamide ═ 1-6: (1-4): (1-5): (2-8) mixing the raw materials according to the mass ratio to obtain a mixture;
5) grinding the mixture, sieving with a 40-60 mesh sieve, loading into a porcelain boat, and calcining at the temperature rising rate of 2-10 ℃/min from room temperature to 350-900 ℃ in a tube furnace;
6) calcining, naturally cooling with the furnace, and ball milling to obtain VC/g-C3N4A photocatalyst.
2. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized by comprising the following steps: the grinding time of the step 2) is 60-80 min.
3. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized by comprising the following steps: the calcination time of the step 2) is 1-6 h.
4. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized by comprising the following steps: and 3) ball-milling for 3h-5h at the rotating speed of 200rpm-400rpm, and ball-milling for 4h-10h at the rotating speed of 400rpm-600rpm to obtain VC powder.
5. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized by comprising the following steps: the grinding time of the step 5) is 70-120 min.
6. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized by comprising the following steps: the calcination time of the step 5) is 1-5 h.
7. VC/g-C according to claim 13N4The preparation method of the photocatalyst is characterized in thatIn the following steps: the ball milling in the step 6) is carried out for 4h-8h at the rotating speed of 300rpm-800 rpm.
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Cited By (3)
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