CN115646528A - High-yield preparation of defect-rich graphite carbon nitride photocatalyst by taking pine as control agent - Google Patents
High-yield preparation of defect-rich graphite carbon nitride photocatalyst by taking pine as control agent Download PDFInfo
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- CN115646528A CN115646528A CN202211341082.7A CN202211341082A CN115646528A CN 115646528 A CN115646528 A CN 115646528A CN 202211341082 A CN202211341082 A CN 202211341082A CN 115646528 A CN115646528 A CN 115646528A
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- 230000007547 defect Effects 0.000 title claims abstract description 39
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 235000008331 Pinus X rigitaeda Nutrition 0.000 title claims abstract description 32
- 235000011613 Pinus brutia Nutrition 0.000 title claims abstract description 32
- 241000018646 Pinus brutia Species 0.000 title claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 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 16
- 239000010439 graphite Substances 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002023 wood Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000006260 foam Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 230000002596 correlated effect Effects 0.000 claims description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- 238000004519 manufacturing process Methods 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 12
- 239000007789 gas Substances 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 239000012298 atmosphere Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000000969 carrier Substances 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
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 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
- 239000002052 molecular layer Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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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
-
- 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 defect-rich graphite carbon nitride photocatalyst prepared by taking pine as a control agent, wherein yellow graphite carbon nitride powder calcined once is horizontally placed in a crucible, foamed nickel is placed above the yellow graphite carbon nitride powder, pine blocks with different masses are placed, and the whole body is calcined twice to obtain defect-rich g-C 3 N 4 (Cv‑g‑C 3 N 4 ). In different stages of temperature rise, the pine releases different gases to penetrate through the porous foamed nickel, thereby realizing the g-C of the bottom of the crucible 3 N 4 Effective modification of (1). The light gray color Cv-g-C obtained 3 N 4 Exhibits smaller micro-morphology size, higher specific surface area to expose more catalytic active sites, and Cv-g-C as the usage amount of pine wood increases 3 N 4 The defect of medium carbon and nitrogen graduallyIncreasing, the repeat arrangement in the crystal plane and the stack size of the molecular layers gradually decrease. Finally, the photocatalytic hydrogen production performance of the photocatalyst 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 large-scale preparation of the hydrogen-producing photocatalyst with controllable size defects.
Description
Technical Field
The invention belongs to the field of photocatalytic functional materials, and relates to a high-yield defect-rich graphite carbon nitride photocatalyst prepared by taking pine as a control agent.
Background
Energy shortage is a major problem facing the future human society, and the photocatalytic technology is expected to meet the energy demand by utilizing clean endless solar energy to realize the development strategy of carbon neutralization. In recent years, a semiconductor material graphite phase carbon nitride (g-C) 3 N 4 ) The photocatalyst has the advantages of rich reserves of the components, simple preparation, high physicochemical thermal stability and the like, thereby causing wide attention of scholars in the field of photocatalysis. However, the lower catalytic activity limits further practical applications because of the small specific surface area of the material, the insufficient absorption of visible light and the high recombination rate of photogenerated carriers, so researchers overcome the above three problems by various modification means to improve the photocatalytic performance. The micro-morphology of the nano material shows smaller morphology which can effectively increase the specific surface area of the nano material, thereby increasing the catalytic active sites, and then, the small-size g-C prepared by most of the current methods 3 N 4 The yield of (2) is low, and particularly after the secondary thermal peeling, the yield is less than 10%. On the other hand, defect engineering can effectively introduce defects into the material to change the electronic band structure and light absorption of the semiconductor through doping and vacancy, however, most of the current methods require calcination to introduce carbon vacancy and the like in a tube furnace under an inert atmosphere, which is energy-intensive, uneconomical, and the tube furnace needs to occupy a large experimental space and is not favorable for mass production. Therefore, a simple method is selected to prepare the g-C with rich defects and controllable size 3 N 4 The application of hydrogen production to change the light absorption and electronic energy band structure, achieve high yield and realize large-scale production and solar energy conversion becomes important.
The disclosed simultaneous preparation of g-C with vacancy defects and controlled morphology 3 N 4 The method of (1) wherein the g-C particles having a high specific surface area are obtained by a double calcination method in which the particles are directly placed in the air 3 N 4 However, the yield is very low, and it is difficult to meet the requirement of large-scale practical production. In addition, some calcinations under a protective atmosphere require a large experimental space. If the reagent is introduced directly with g-C 3 N 4 The mixing and the secondary calcination can introduce vacancies and change the shape of the material, but the reagent and the g-C 3 N 4 Direct contact between and insufficient mixing can result in g-C 3 N 4 Internal defects are not uniform and the size is not controllable. Thus, an economical, inexpensive, large space-occupying, mass-producible and free of g-C is used 3 N 4 Optimization of g-C by direct contact of materials 3 N 4 The characteristics of all aspects have significance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a high-yield preparation method of a defect-rich graphite carbon nitride photocatalyst by taking pine as a control agent, and the method directly uses the g-C obtained after primary calcination 3 N 4 Placing in the bottom of the crucible, placing dried pine in the upper part of the crucible and supporting it with foamed nickel, and performing secondary calcination to obtain g-C with controllable carbon and nitrogen defects and small-size morphology 3 N 4 . During the gradual heating process, the pine wood will release different gases, such as CO and H, in different stages 2 O and CO 2 The original calcination environment is changed by the gases, wood with different qualities is selected and the mode of non-direct contact can effectively realize the controllability of defects and appearances.
Technical scheme
A high-yield defect-rich graphite carbon nitride photocatalyst prepared by taking pine as a control agent is characterized by comprising the following steps:
step 1: putting 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 a yellow block into powder of g-C 3 N 4 ；
Step 2: g to C 3 N 4 Placing the powder at the bottom of the crucible, cutting the foamed nickel into a circular shape, and clamping the circular shape at the position below the top of the crucible; the diameter of the circular foam nickel is matched with that of the crucible;
and step 3: placing the dried pine wood pieces on foamed nickel, covering a crucible, then placing the whole crucible in a muffle furnace to be heated to 520-580 ℃ at the heating rate of 2-5 ℃/min, preserving the heat for 2-4 h at the temperature, and cooling to room temperature to obtain the powder with light gray bottom as the rich defect g-C 3 N 4 (Cv-g-C 3 N 4 ) I.e., defect-rich graphitic carbon nitride photocatalysts.
The circular shape of the nickel foam is at a position 1cm below the top of the crucible.
The dried pine pieces were 5mg of small wood pieces per piece.
The foam nickel is porous foam nickel.
The introduced carbon and nitrogen defects are positively correlated with the added mass of the pine wood chips.
Advantageous effects
The invention provides a high-yield defect-rich graphite carbon nitride photocatalyst prepared by taking pine as a control agent, which is prepared by calcining yellow graphite carbon nitride (g-C) 3 N 4 ) Spreading the powder in a covered crucible, placing foam nickel at a position slightly below the crucible, placing pine blocks with different masses on the foam nickel, and performing secondary calcination on the whole to obtain the g-C rich defect 3 N 4 (Cv-g-C 3 N 4 ). In different stages of temperature rise, the pine releases different gases to penetrate through the porous foamed nickel, thereby realizing g-C of the bottom of the crucible 3 N 4 Effective modification of (1). The light gray color Cv-g-C obtained 3 N 4 Exhibits smaller micro-morphology size, higher specific surface area to expose more catalytic active sites, and Cv-g-C as the usage amount of pine wood increases 3 N 4 The medium carbon nitrogen defects are gradually increased, and the repeated arrangement in the crystal surface and the stacking size of the molecular layer are gradually reduced. Finally, the photocatalytic hydrogen production performance of the photocatalyst is higher than that of pure g-C 3 N 4 About 20 times higher. Compared with the disclosed 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 invention has the beneficial effects that: the method only realizes secondary calcination in a simple crucible, uses cheap and economic pine as a control material of calcination atmosphere, and wood is supported by porous foam nickel, so that g-C is avoided 3 N 4 The wood generates different gases at different stages in the process of heating and decomposing, and can effectively and uniformly treat g-C 3 N 4 The modification is carried out. Through secondary calcinationPost, cv-g-C 3 N 4 The yield is about 95 percent, and the Cv-g-C is effectively inhibited in the semi-closed environment 3 N 4 Thermal decomposition of (3). The photocatalyst shows smaller size appearance and larger specific surface area, the size is gradually reduced and the carbon-nitrogen defect is increased along with the increase of the dosage of wood, compared with g-C 3 N 4 Shows higher photocatalytic hydrogen production performance.
Drawings
FIG. 1 shows preparation of Cv-g-C according to example two of the present invention 3 N 4 Schematic representation of a photocatalyst.
FIG. 2 is g-C prepared according to example two of the present invention 3 N 4 And Cv-g-C 3 N 4 Scanning Electron Microscope (SEM) pictures of the photocatalyst.
In the figure: 1.g-C 3 N 4 The nitrogen adsorption-desorption curve of (a); cv-g-C 3 N 4 Nitrogen adsorption-desorption curve of photocatalyst; 3.g-C 3 N 4 XPS C1s spectra curve of (a); cv-g-C 3 N 4 XPS C1s spectra curve of photocatalyst; 5.g-C 3 N 4 The hydrogen production performance curve of (1); cv-g-C 3 N 4 The hydrogen production performance curve of (2).
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the first embodiment is as follows:
(1) 10g of melamine powder are placed in a crucible with a cover and put in a muffle furnaceHeating to 580 deg.C at a heating rate of 5 deg.C/min, maintaining the temperature for 2h, cooling to room temperature, grinding the yellow block into powder, and recording as g-C 3 N 4 。
(2) 1g of g-C in step one 3 N 4 The powder was placed in the bottom of a 100ml crucible and the nickel foam was cut into a circular shape and clamped just 1cm below the top of the crucible.
(3) Cutting dried pine wood pieces into small wood blocks with the weight of 5mg per block for later use, uniformly placing the small wood blocks with the total weight of 25mg on the foamed nickel, covering a crucible, then integrally placing the whole body in a muffle furnace again, heating to 580 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours at the temperature, and cooling to room temperature to obtain light gray powder at the bottom, namely carbon defect g-C 3 N 4 (Cv-g-C 3 N 4 )。
Example two:
(1) 10g of melamine powder are placed in a covered crucible, heated to 550 ℃ in a muffle furnace at a heating rate of 3.5 ℃/min and kept at the temperature for 3h, after cooling to room temperature, the yellow blocks are ground into powder, recorded as g-C 3 N 4 。
(2) Taking 1.5g of g-C in the step one 3 N 4 The powder was placed in the bottom of a 100ml crucible and the nickel foam was cut into a circular shape and clamped just 1cm below the top of the crucible.
(3) Cutting dried pine pieces into small wood blocks with the weight of 5mg each for standby, then uniformly placing the small wood blocks with the total mass of 50mg on foamed nickel, covering a crucible, then integrally placing the crucible in a muffle furnace again, heating to 550 ℃ at the heating rate of 3.5 ℃/min, preserving heat for 3 hours at the temperature, 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 )。
Example three:
(1) 10g of melamine powder are placed in a covered crucible, heated to 520 ℃ in a muffle furnace at a heating rate of 2 ℃/min and kept at the temperature for 4h, after cooling to room temperature, the yellow block is ground into powder, recorded as g-C 3 N 4 。
(2) Taking 2g of g-C in step one 3 N 4 The powder was placed in the bottom of a 100ml crucible and the nickel foam was cut into a circular shape and clamped just 1cm below the top of the crucible.
(3) Cutting dried pine pieces into small wood blocks of 5mg each for later use, then uniformly placing the small wood blocks with the total mass of 100mg on the foamed nickel, covering a crucible, then integrally placing the whole body in a muffle furnace again, raising the temperature to 520 ℃ at the temperature raising rate of 2 ℃/min, preserving the heat for 4h at the temperature, and after cooling to the room temperature, obtaining powder with light gray bottom, namely carbon defect g-C 3 N 4 (Cv-g-C 3 N 4 )。
The embodiment figures show that the photocatalyst shows smaller size and appearance and larger specific surface area, the size is gradually reduced and the carbon and nitrogen defects are increased along with the increase of the wood consumption, compared with g-C 3 N 4 Shows higher photocatalytic hydrogen production performance.
FIG. 1 shows preparation of Cv-g-C according to example two of the present invention 3 N 4 Schematic representation of a photocatalyst. It can be seen that the method is simple, takes up little space, and utilizes economical pine to assist the secondary calcination for the preparation of Cv-g-C 3 N 4 A photocatalyst. During the calcination process, various mixed gases are uniformly distributed in the crucible, the porous foamed nickel can enable the gases to reach the position of the catalyst below the crucible from the upper part of the crucible, and due to the small pore size of the foamed nickel, the pine solids which are not completely calcined cannot fall into the lower part of the crucible from the upper part of the foamed nickel, and cannot pollute the Cv-g-C below the crucible 3 N 4 。
FIG. 2 is g-C prepared according to example two of the present invention 3 N 4 And Cv-g-C 3 N 4 SEM pictures of the photocatalyst. It can be seen from the figure that g-C 3 N 4 Is a large block stacked in disorder, and is generated due to the mixed gas in Cv-g-C 3 N 4 The internal effect, which shows a smaller particle morphology, and such morphology becomes smaller as the amount of wood used increases.
Claims (5)
1. A high-yield defect-rich graphite carbon nitride photocatalyst prepared by taking pine as a control agent is characterized by comprising the following steps:
step 1: putting 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 a yellow block into powder of g-C 3 N 4 ；
Step 2: g to C 3 N 4 Placing the powder at the bottom of the crucible, cutting the foamed nickel into a circular shape, and clamping the circular shape at the position below the top of the crucible; the diameter of the circular foam nickel is matched with that of the crucible;
and step 3: placing the dried pine wood pieces on foamed nickel, covering the crucible, placing the whole crucible in a muffle furnace, and heating to 520E to E at a heating rate of 2-5 ℃/min580 ℃ and keeping the temperature for 2 to 4 hours, and after cooling to the room temperature, the powder with light gray bottom is rich in defects g-C 3 N 4 (Cv-g-C 3 N 4 ) I.e., defect-rich graphitic carbon nitride photocatalysts.
2. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by using pine as a control agent according to claim 1, is characterized in that: the circular 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 using pine as a control agent according to claim 1, is characterized in that: the dried pine pieces were 5mg of small wood pieces per piece.
4. The method for preparing the defect-rich graphite carbon nitride photocatalyst with high yield by using pine as a control agent according to claim 1, 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 using pine as a control agent according to claim 1, is characterized in that: the introduced carbon and nitrogen defects are positively correlated with the added mass of the pine wood chips.
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| CN115010101A (en) * | 2022-07-18 | 2022-09-06 | 河南大学 | Preparation method and application of carbon nitride nanosheet with wide spectral response and high crystallinity |
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