CN115646528B - Method for preparing defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as control agent - Google Patents
Method for preparing defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as control agent Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 230000007547 defect Effects 0.000 title claims abstract description 36
- 235000008331 Pinus X rigitaeda Nutrition 0.000 title claims abstract description 31
- 235000011613 Pinus brutia Nutrition 0.000 title claims abstract description 31
- 241000018646 Pinus brutia Species 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 15
- 239000010439 graphite Substances 0.000 title claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000006260 foam Substances 0.000 claims abstract description 30
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 30
- 239000002023 wood Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 19
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 230000002950 deficient Effects 0.000 claims description 3
- 230000002596 correlated effect Effects 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000001257 hydrogen Substances 0.000 abstract description 14
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000002360 preparation method Methods 0.000 abstract description 12
- 239000007789 gas Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 230000007423 decrease Effects 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 13
- 239000000463 material Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 230000008859 change Effects 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
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Classifications
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention relates to a high-yield preparation method of a defect-rich graphite carbon nitride photocatalyst by taking pine as a control agent, which comprises the steps of horizontally placing yellow graphite carbon nitride powder subjected to primary calcination in a crucible, placing foam nickel above the yellow graphite carbon nitride powder, placing pine blocks with different masses, and carrying out integral secondary calcination to obtain defect-rich g-C 3 N 4 (Cv‑g‑C 3 N 4 ). At different stages of temperature rise, pine wood releases different gases to pass through porous foam nickel, thereby realizing the g-C of the bottom of the crucible 3 N 4 Is effective in modification of (3). The light grey Cv-g-C obtained 3 N 4 Exhibit smaller microscopic morphology dimensions, higher specific surface area to expose more catalytically active sites, and Cv-g-C as pine usage increases 3 N 4 The carbon-nitrogen defects in the crystal face gradually increase, and the repeated arrangement and the stacking size of the molecular layers in the crystal face gradually decrease. Finally, the photocatalyst shows the photocatalytic hydrogen production performance which is higher than that of pure g-C 3 N 4 About 20 times higher. Compared with the disclosed method, the method has the advantages of simplicity, small occupied space, economy and capability of preparing the hydrogen-producing photocatalyst with controllable size defects on a large scale.
Description
Technical Field
The invention belongs to the field of photocatalytic functional materials, and relates to a method for preparing a defective graphite carbon nitride photocatalyst with high yield by taking pine as a control agent.
Background
The shortage of energy is a major problem facing the future human society, and the photocatalysis technology is expected to meet the energy demand by utilizing clean and endless solar energy, so as to realize the development strategy of carbon neutralization. In recent years, a semiconductor material of graphite-phase carbon nitride (g-C 3 N 4 ) Because of rich reserves of the constituent elements, simple preparation and high physical and chemical heat stabilityQualitative and other advantages, and the method has attracted extensive attention of students in the field of photocatalysis. However, the lower catalytic activity limits further practical applications because the material has a small specific surface area, insufficient absorption of visible light and high photo-generated carrier recombination rate, so researchers overcome the above three problems by various modification means, thereby improving the photocatalytic performance. The micro morphology of the nano material shows smaller morphology, can effectively increase the specific surface area of the nano material, so that the catalytic active site is increased, and then the small-size g-C prepared by most methods at present is prepared 3 N 4 The yield of (2) is low, particularly after the secondary heat peeling, less than 10%. On the other hand, defect engineering can effectively introduce defects in the material to change the electronic band structure and light absorption of a semiconductor by doping and vacancy, however, most of the current methods require calcining in a tube furnace and under inert atmosphere to introduce carbon vacancies and the like, which is high in energy consumption and uneconomical, and the tube furnace occupies a large experimental space and is unfavorable for mass production. Thus, a simple way is chosen to produce g-C with controllable defects and dimensions 3 N 4 To change the light absorption and electronic energy band structure, and to obtain higher yield to realize large-scale production, and to perform solar energy conversion to produce hydrogen is particularly important.
Document 1"Niu P,Zhang L,Liu G et al.Graphene-Like Carbon Nitride Nanosheets for Improved Photocatalytic Activities [ J]Advanced Functional Materials,2012,22,4763-4770 "discloses a process for preparing g-C having a high specific surface area 3 N 4 A method for preparing nano-sheets. The method comprises the step of adding g-C 3 N 4 Placing the powder in air for secondary calcination to obtain g-C 3 N 4 The intra-and inter-layer dimensions of (c) become smaller, thereby increasing the specific surface area of the material and thus the photocatalytic hydrogen production performance. Due to g-C 3 N 4 The nano-sheets prepared by the method have lower yield and usually act at 5% by continuous oxidation and pyrolysis in air.
Document 2"Li S,Zeng Y,Wang C et al.Effective photocatalytic H 2 O 2 production under visible light irradiation at g-C 3 N 4 modulated by carbon vacancies[J]Applied Catalysis B Environmental 2016,190,26-35 "discloses a process for preparing carbon vacancies g-C 3 N 4 Is a method of (2). The method is carried out by directly subjecting g-C 3 N 4 Placing in a tube furnace, calcining under inert atmosphere of high purity argon for two hours to obtain g-C 3 N 4 Certain carbon defects are generated inside the photocatalyst, the light absorption capacity is enhanced, and H is generated by photocatalysis 2 O 2 Is not limited to the above-described embodiments. However, the preparation method is energy-consuming and uneconomical, and requires the inert gas to be introduced into the tube furnace to change g-C 3 N 4 Ambient calcination environment.
Disclosed is the simultaneous preparation of g-C with vacancy defects and morphology control 3 N 4 In the method (C), although the secondary calcination method directly placed in air can obtain g-C with high specific surface area 3 N 4 But the productivity is very low, and it is difficult to meet the requirement of large-scale practical production. In addition, some calcination under a protective atmosphere requires a large experimental space. If the reagent is directly introduced with g-C 3 N 4 Mixing and secondary calcination can introduce vacancies and change the morphology of the material, but the reagent and g-C 3 N 4 Direct contact and inadequate mixing between them can lead to g-C 3 N 4 The internal defects are not uniform and the size is not controllable. Thus, an economical, inexpensive, does not occupy a large space, can be mass-produced and does not interact with g-C 3 N 4 Optimization of g-C by direct contact materials 3 N 4 The characteristics of each aspect are of great significance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent, which directly calcines g-C after one time 3 N 4 Placing at the bottom of crucible, placing dried pine wood at the upper part of crucible and supporting it with foam nickel, and performing secondary calcination to obtain the final product with controllable carbon and nitrogen defects and small-sized morphologyg-C of (2) 3 N 4 . During the gradual heating process, the pine wood releases different gases such as CO and H at different stages 2 O and CO 2 And (3) waiting for gas, changing the original calcination environment, and selecting wood with different qualities and adopting the mode of non-direct contact can effectively realize the defect and morphology controllability.
Technical proposal
A method for preparing a defective graphite-rich carbon nitride photocatalyst with high yield by taking pine as a control agent is characterized by comprising the following steps:
step 1: placing melamine powder into a covered crucible, heating to 520-580 ℃ in a muffle furnace at a heating rate of 2-5 ℃/min, preserving heat for 2-4 h at the temperature, cooling to room temperature, and grinding yellow blocks into powder g-C 3 N 4 ；
Step 2: will g-C 3 N 4 Placing the powder at the bottom of a crucible, shearing foam nickel into a circular shape, and clamping the foam nickel at the position below the top of the crucible; the diameter of the foam nickel in the circular shape is matched with the diameter of the crucible;
step 3: placing the dried pine wood pieces on foam nickel, capping the crucible, placing the whole body in a muffle furnace, heating to 520-580 ℃ at a heating rate of 2-5 ℃/min, preserving the temperature for 2-4 h, cooling to room temperature, and obtaining the light gray powder at the bottom, which is rich in defects g-C 3 N 4 (Cv-g-C 3 N 4 ) I.e., a defect-rich graphitic carbon nitride photocatalyst.
The circular shaped nickel foam is at a position 1cm below the top of the crucible.
The dried pine wood pieces were small pieces of 5mg per piece.
The foam nickel is porous foam nickel.
The introduced carbon-nitrogen defect is positively correlated with the added quality of pine wood chips.
Advantageous effects
The invention provides a method for preparing a defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent, which comprises the steps of calcining yellow graphite carbon nitride (g-C) 3 N 4 ) Spreading the powder in a covered crucible, placing foam nickel at a position below the upper part of the crucible, placing pine wood blocks with different mass on the foam nickel, and calcining for the whole to obtain defect-rich g-C 3 N 4 (Cv-g-C 3 N 4 ). At different stages of temperature rise, pine wood releases different gases to pass through porous foam nickel, thereby realizing the g-C of the bottom of the crucible 3 N 4 Is effective in modification of (3). The light grey Cv-g-C obtained 3 N 4 Exhibit smaller microscopic morphology dimensions, higher specific surface area to expose more catalytically active sites, and Cv-g-C as pine usage increases 3 N 4 The carbon-nitrogen defects in the crystal face gradually increase, and the repeated arrangement and the stacking size of the molecular layers in the crystal face gradually decrease. Finally, the photocatalyst shows the photocatalytic hydrogen production performance which is higher than that of pure g-C 3 N 4 About 20 times higher. Compared with the method for preparing the carbon nitride photocatalyst with defects and high specific surface area, the method has the advantages of simplicity, small occupied space, economy and capability of preparing the hydrogen-producing photocatalyst with controllable size defects on a large scale.
The beneficial effects of the invention are as follows: the method realizes secondary calcination in a simple crucible only, takes cheap and economical pine as a control material of calcination atmosphere, and prevents the wood from g-C by supporting the wood through porous foam nickel 3 N 4 Is characterized in that the wood generates different gases at different stages in the process of thermal decomposition, and can effectively and uniformly pair g-C 3 N 4 Modification is performed. After secondary calcination, cv-g-C 3 N 4 The yield of (C) is about 95%, and the semi-closed environment effectively inhibits Cv-g-C 3 N 4 Is a thermal decomposition of (a). The photocatalyst has smaller size and shape and larger specific surface area, and gradually reduces the size with the increase of the wood consumption, and increases the carbon and nitrogen defects compared with g-C 3 N 4 Shows higher photocatalytic hydrogen production performance.
Drawings
FIG. 1 shows the preparation of Cv-g-C according to example II of the present invention 3 N 4 Schematic representation of the photocatalyst.
FIG. 2 is a schematic illustration of the present inventionExample two prepared g-C 3 N 4 And Cv-g-C 3 N 4 Scanning Electron Microscope (SEM) pictures of the photocatalyst.
In FIG. 3, curve 1 and curve 2 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 Nitrogen adsorption desorption-curve of photocatalyst.
In FIG. 4, curve 3 and curve 4 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 X-ray photoelectron (XPS) C1s spectrum of the photocatalyst.
In FIG. 5, curve 5 and curve 6 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 The hydrogen production performance of the photocatalyst is compared with that of the photocatalyst.
In the figure: 1.g-C 3 N 4 Nitrogen adsorption-desorption curves of (2); cv-g-C 3 N 4 Nitrogen adsorption-desorption curve of photocatalyst; 3.g-C 3 N 4 XPS C1s profile; cv-g-C 3 N 4 XPS C1s spectrum curve of the photocatalyst; g-C 3 N 4 Hydrogen production performance curve of (2); cv-g-C 3 N 4 Hydrogen production performance curves of (2).
Detailed Description
The invention will now be further described with reference to examples, figures:
embodiment one:
(1) 10g of melamine powder is placed in a covered crucible, heated to 580 ℃ in a muffle furnace at a heating rate of 5 ℃/min and kept at that temperature for 2 hours, cooled to room temperature, and the yellow block is ground into powder which is recorded as g-C 3 N 4 。
(2) 1g of g-C in step one 3 N 4 The powder was placed at the bottom of a 100ml crucible, and the nickel foam was cut into round shapes, just clamped 1cm below the top of the crucible.
(3) Cutting dried pine wood chips into 5mg of small wood blocks for later use, uniformly placing the small wood blocks with the total mass of 25mg on the foam nickel, covering a crucible, and placing the whole body in a muffle furnace again at 5 DEG CHeating to 580 deg.C at a heating rate of/min, maintaining the temperature for 2 hr, cooling to room temperature, and collecting light gray powder as carbon defect g-C 3 N 4 (Cv-g-C 3 N 4 )。
Embodiment two:
(1) 10g of melamine powder is placed in a covered crucible, heated to 550 ℃ in a muffle furnace at a heating rate of 3.5 ℃/min and kept at that temperature for 3 hours, cooled to room temperature, and the yellow block is ground into powder which is recorded as g-C 3 N 4 。
(2) 1.5g of g-C from step one was taken 3 N 4 The powder was placed at the bottom of a 100ml crucible, and the nickel foam was cut into round shapes, just clamped 1cm below the top of the crucible.
(3) Cutting dried pine wood chips into 5mg of small wood blocks for later use, uniformly placing the small wood blocks with the total mass of 50mg on foam nickel, covering a crucible, then placing the whole body in a muffle furnace again, heating to 550 ℃ at a heating rate of 3.5 ℃/min, preserving heat at the temperature for 3 hours, cooling to room temperature, and obtaining light gray powder at the bottom, namely the carbon defect g-C 3 N 4 (Cv-g-C 3 N 4 )。
Embodiment III:
(1) 10g of melamine powder is placed in a covered crucible, heated to 520 ℃ in a muffle furnace at a heating rate of 2 ℃/min and kept at that temperature for 4 hours, cooled to room temperature, and the yellow block is ground into powder which is recorded as g-C 3 N 4 。
(2) Taking 2g of g-C in the first step 3 N 4 The powder was placed at the bottom of a 100ml crucible, and the nickel foam was cut into round shapes, just clamped 1cm below the top of the crucible.
(3) Cutting dried pine wood chips into 5mg of small wood blocks for later use, uniformly placing the small wood blocks with the total mass of 100mg on foam nickel, covering a crucible, then placing the whole body in a muffle furnace again, heating to 520 ℃ at a heating rate of 2 ℃/min, preserving heat at the temperature for 4 hours, cooling to room temperature, and obtaining light gray powder at the bottom, namely the carbon defect g-C 3 N 4 (Cv-g-C 3 N 4 )。
The beneficial effects of the invention show through the embodiment drawings that the photocatalyst shows smaller size morphology and larger specific surface area, the size gradually decreases with the increase of the wood consumption, and the carbon and nitrogen defects increase, compared with g-C 3 N 4 Shows higher photocatalytic hydrogen production performance.
FIG. 1 shows the preparation of Cv-g-C according to example II of the present invention 3 N 4 Schematic representation of the photocatalyst. It can be seen that the method is a simple, small-space-occupation method for preparing Cv-g-C by using economic pine wood to assist secondary calcination 3 N 4 A photocatalyst. In the calcination process, various mixed gases are uniformly distributed in the crucible, and porous foam nickel can enable the gases to reach the position of the catalyst below from the upper part of the crucible, and due to the small pore size of the foam nickel, loose wood solids which are not completely calcined cannot fall into the lower part of the crucible from the upper part of the foam nickel, and cannot pollute Cv-g-C below 3 N 4 。
FIG. 2 is a graph of g-C prepared in example II of the present invention 3 N 4 And Cv-g-C 3 N 4 SEM pictures of the photocatalyst. From the figure, g-C can be seen 3 N 4 Is a messy stacked bulk, and is formed by mixing gas at Cv-g-C 3 N 4 The internal effects, which show smaller particle morphologies, and such morphologies become smaller as wood usage increases.
In FIG. 3, curve 1 and curve 2 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 Nitrogen adsorption-desorption curve of photocatalyst. From the figure, cv-g-C can be seen 3 N 4 Is at a higher position, and the specific surface area is 84m by calculation 2 G, compared with g-C 3 N 4 The lifting is about 7 times. The high specific surface area corresponds to its smaller size in the SEM image.
In FIG. 4, curve 3 and curve 4 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 XPS C1s energy spectrum of photocatalyst. The peak of the binding energy at 288.0eV corresponds to the carbon nitride materialSp of (2) 2 The hybridized carbon atom N-C=N, which can be seen in Cv-g-C 3 N 4 The shift of this peak to a lower position in the middle indicates that Cv-g-C 3 N 4 Carbon vacancies exist in the material.
In FIG. 5, curve 5 and curve 6 are respectively the preparation of g-C according to example II of the present invention 3 N 4 And Cv-g-C 3 N 4 The hydrogen production performance of the photocatalyst is compared with that of the photocatalyst. It can be seen that Cv-g-C after 4 hours of hydrogen production test 3 N 4 Exhibits higher photocatalytic hydrogen production performance, about g-C 3 N 4 20 times of (3).
Claims (5)
1. A method for preparing a defective graphite-rich carbon nitride photocatalyst with high yield by taking pine as a control agent is characterized by comprising the following steps:
step 1: placing melamine powder into a covered crucible, heating to 520-580 ℃ in a muffle furnace at a heating rate of 2-5 ℃/min, preserving heat for 2-4 h at the temperature, cooling to room temperature, and grinding yellow blocks into powder g-C 3 N 4 ；
Step 2: will g-C 3 N 4 Placing the powder at the bottom of a crucible, shearing foam nickel into a circular shape, and clamping the foam nickel at the position below the top of the crucible; the diameter of the foam nickel in the circular shape is matched with the diameter of the crucible;
step 3: placing the dried pine wood pieces on foam nickel, capping the crucible, placing the whole body in a muffle furnace, heating to 520-580 ℃ at a heating rate of 2-5 ℃/min, preserving the temperature for 2-4 h, cooling to room temperature, and obtaining the light gray powder at the bottom, which is rich in defects g-C 3 N 4 (Cv-g-C 3 N 4 ) I.e., a defect-rich graphitic carbon nitride photocatalyst.
2. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent according to claim 1, which is characterized in that: the circular shaped nickel foam is at a position 1cm below the top of the crucible.
3. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent according to claim 1, which is characterized in that: the dried pine wood pieces were small pieces of 5mg per piece.
4. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent according to claim 1, which is characterized in that: the foam nickel is porous foam nickel.
5. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by taking pine as a control agent according to claim 1, which is characterized in that: the introduced carbon-nitrogen defect is positively correlated with the added quality of pine wood chips.
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