CN111232939B - Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) - Google Patents
Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) Download PDFInfo
- Publication number
- CN111232939B CN111232939B CN202010051384.5A CN202010051384A CN111232939B CN 111232939 B CN111232939 B CN 111232939B CN 202010051384 A CN202010051384 A CN 202010051384A CN 111232939 B CN111232939 B CN 111232939B
- Authority
- CN
- China
- Prior art keywords
- calcining
- temperature
- modified
- stripping
- reaction precursor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims abstract description 11
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 238000003892 spreading Methods 0.000 claims abstract description 7
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 6
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 18
- 239000002135 nanosheet Substances 0.000 claims description 16
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical group NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- POJWUDADGALRAB-PVQJCKRUSA-N Allantoin Natural products NC(=O)N[C@@H]1NC(=O)NC1=O POJWUDADGALRAB-PVQJCKRUSA-N 0.000 claims description 6
- 229960000458 allantoin Drugs 0.000 claims description 6
- 239000002062 molecular scaffold Substances 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 28
- 238000012719 thermal polymerization Methods 0.000 abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 26
- 229910052739 hydrogen Inorganic materials 0.000 description 26
- 239000001257 hydrogen Substances 0.000 description 26
- 238000004519 manufacturing process Methods 0.000 description 23
- 238000001816 cooling Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-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
- 230000005540 biological transmission Effects 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- 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
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
Abstract
The invention discloses a method for preparing g-C which is easier to peel by embedding a three-dimensional molecule 3 N 4 The method comprises the steps of preparing modified g-C by a high-temperature thermal polymerization method by taking an organic compound with a triazine ring structure or an organic compound capable of generating the triazine ring structure through a polycondensation reaction as a reaction precursor and a comonomer with a three-dimensional structure 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the After the reaction, modified g-C 3 N 4 Spreading on ceramic plate, and performing thermal oxidation stripping. The preparation method is simple, low-cost raw materials and simple equipment conditions are adopted, human interference factors are few in the preparation process, expensive equipment is not needed in the preparation process, and chemical reagents are not needed to be added; preparation of modified g-C which is easier to peel 3 N 4 Photocatalytic activity and pure g-C 3 N 4 Can be improved by 8 times compared with the prior art.
Description
Technical Field
The invention belongs to the technical field of photocatalysis materials, and particularly relates to a method for preparing g-C which is easier to peel by embedding a three-dimensional molecule 3 N 4 Is a method of (2).
Background
With the continued development of the economic society, excessive consumption of fossil fuels has raised global energy crisis and environmental pollution. The hydrogen energy is renewable, pollution-free and high in energy density, so that the hydrogen energy becomes a new energy source with great utilization value. Photocatalytic water splitting is one of the most promising methods for converting solar energy into storable hydrogen energy.
g-C 3 N 4 Is a visible light responsive polymer semiconductor, has a band gap of 2.7eV, and has many excellent performances such as good chemical and thermodynamic stability, low price, simple preparation and the like. g-C 3 N 4 The introduction of the field of photocatalysis has attracted a great public interest, although g-C 3 N 4 The initial activity of (2) is not obvious, but it opens a new door for the investigation of organic photocatalysis. Over the past few decades scientists have studied many improvements in g-C 3 N 4 A method for producing hydrogen by photocatalytic pyrolysis, such as: stripping, designing nanostructures, doping elements, constructing heterojunctions, etc., thermal oxidative stripping is one of the common and effective means. However, due to g-C 3 N 4 The tight stack between layers, which is very difficult to peel, still presents many bottlenecks to be resolved, such as interface defects, reduced light absorption, and low yields<6%) and the like. If there is a weakening g-C 3 N 4 Stacking method, g-C 3 N 4 The peeling of (c) is facilitated, so that defects caused by the peeling can be overcome in anticipation.
Molecular copolymerization has been demonstrated to regulate g-C 3 N 4 Efficient methods of electron and band structure. In general, the molecularly copolymerized monomers are mostly planar two-dimensional molecules for the extension of g-C 3 N 4 And accelerates in-plane electron-hole separation. However, the molecules with three-dimensional structure are in g-C 3 N 4 Is seriously neglected in the molecular copolymerization of (2) because the steric molecules may act as scaffolds between layers to weaken g-C 3 N 4 Is laminated. These problems have prompted us to further search for simpler, efficient, low cost, and practical methods of preparation.
Disclosure of Invention
The purpose of the invention is to solve the problem of g-C 3 N 4 The problems of low photocatalytic activity and difficult stripping are solved, and the problems existing in the prior art are solved, so that the g-C which is easier to strip is prepared by embedding the three-dimensional molecules 3 N 4 Is a method of (2).
The technical scheme adopted by the invention is as follows: doping a three-dimensional molecular support into g-C by a high-temperature thermal polymerization method 3 N 4 In the molecular plane of (2), modifying g-C by thermal oxidation stripping method 3 N 4 Stripping to obtain a modified g-C with better catalytic performance and easier stripping 3 N 4 。
Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Comprises the following steps:
(1) Uniformly mixing a reaction precursor and a molecular bracket with a three-dimensional structure, and calcining at a high temperature to synthesize the block modified g-C 3 N 4 ；
The reaction precursor is an organic compound with a triazine ring structure or an organic compound capable of generating the triazine ring structure through polycondensation reaction;
(2) Modifying g-C with the block obtained in step (1) 3 N 4 Taking the modified g-C as a raw material, and performing thermal oxidation stripping to obtain the modified g-C 3 N 4 A nano-sheet.
Further, the high-temperature calcination synthesis temperature in the step (1) is 520-550 ℃, and the reaction time is 1-4 hours; the temperature of the thermal oxidation stripping in the step (2) is 520-550 ℃, and the stripping time is 1-3 hours.
Further, the reaction precursor in the step (1) is melamine or dicyandiamide.
Further, the molecular scaffold with a three-dimensional structure is allantoin.
Further, the mass ratio of the molecular scaffold with the three-dimensional structure to the reaction precursor is 0.02-0.3:10.
Further, the specific process of the step (1) is as follows: the reaction precursor and the molecular bracket with the three-dimensional structure are uniformly mixed and placed in a high-temperature resistant container, the high-temperature resistant container with the reaction precursor and the molecular bracket with the three-dimensional structure uniformly mixed is placed in a calcining device, the calcining device is arranged to be heated to 520-550 ℃ from room temperature, and the calcining is carried out for 4 hours under the condition of 520-550 ℃.
Further, the temperature rising rate of the calcining equipment in the step (1) is controlled to be 25 ℃/min.
Further, the specific process of the step (2) is as follows: modifying the block body to g-C 3 N 4 Grinding into powder in a mortar, spreading the powder on a ceramic sheet, placing the ceramic sheet with the powder in a calcining device, setting the calcining device to rise from room temperature to 520-550 ℃, and calcining for 3 hours at 520-550 ℃.
Further, the temperature rising rate of the calcining equipment in the step (2) from room temperature to 520-550 ℃ is 2 ℃/min.
The beneficial effects of the invention are as follows:
(1) The preparation method is simple, has few human interference factors in the preparation process, does not need expensive equipment in the preparation process, and does not need to add chemical reagents;
(2) Can better promote g-C through the embedding of the stereo molecule 3 N 4 Is modified g-C after peeling 3 N 4 With pure g-C after stripping 3 N 4 Compared with the method, the photocatalytic hydrogen production performance is improved by several times.
(3) After thermal oxidation stripping, modifying g-C 3 N 4 The photocatalytic hydrogen production of the nano-sheet can reach pure g-C 3 N 4 8 times of (3);
(4) Modified g-C prepared by the invention 3 N 4 Has a thinner layer number and a multi-fold morphology.
Drawings
FIG. 1 is pure g-C 3 N 4 A transmission electron microscope image;
FIG. 2 is a modified g-C 3 N 4 Is a transmission electron microscope image;
FIG. 3 is pure g-C 3 N 4 And modifying g-C 3 N 4 The photo-catalytic hydrogen production amount after 3 hours of unpeeled and thermal oxidation stripping is shown in the schematic diagram.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
Weighing 5g of melamine and 0.15g of allantoin, uniformly mixing and grinding, loading into a 100ml crucible, covering a crucible cover, and placing the crucible into a muffle furnace; setting a muffle furnace to raise the temperature from room temperature to 550 ℃, reacting for 4 hours, and naturally cooling to room temperature after calcining to obtain modified g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Grinding the calcined sample into powder in an agate mortar, weighing 0.1g of powder, and spreading the powder on a ceramic plate with the diameter of 10 cm; calcining in muffle furnace at 550deg.C for 2 hr at heating rate of 2deg.C/min, naturally cooling to room temperature after calcining, and collecting to obtain modified g-C 3 N 4 A nanosheet;
the results of the photocatalytic hydrogen production test show that the modified g-C prepared in example 1 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is modified g-C which is not stripped 3 N 4 Is 3.6 times that of the stripped pure g-C prepared by the traditional thermal polymerization method 3 N 4 The photocatalytic hydrogen production performance of (C) is only that of pure g-C which is not stripped 3 N 4 1.7 times of (2); block g-C prepared by traditional thermal polymerization method 3 N 4 Comparative, modified g-C prepared in example 1 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is improved by 7 times.
Example 2
Weighing 5g of melamine and 0.025g of allantoin, uniformly mixing and grinding, loading into a 100ml crucible, covering the crucible with a crucible cover, and placing the crucible into a muffle furnace; setting a muffle furnace to raise the temperature from room temperature to 520 ℃, reacting for 4 hours, and naturally cooling to room temperature after calcining to obtain modified g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Grinding the calcined sample into powder in an agate mortar, weighing 0.1g of powder, and spreading the powder on a ceramic plate with the diameter of 10 cm; calcining in muffle furnace at 550deg.C for 1 hr at heating rate of 2deg.C/min, naturally cooling to room temperature after calcining, and collecting to obtain modified g-C 3 N 4 A nanosheet;
photocatalytic hydrogen production test junctionThe results show that modified g-C prepared in example 2 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is modified g-C which is not stripped 3 N 4 Is 2.2 times that of the stripped pure g-C prepared by the traditional thermal polymerization method 3 N 4 The photocatalytic hydrogen production performance of (C) is pure g-C without stripping 3 N 4 1.2 times of (2); block g-C prepared by traditional thermal polymerization method 3 N 4 Comparative, modified g-C prepared in example 2 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is improved by 2 times.
Example 3
Weighing 10g of dicyandiamide and 0.15g of allantoin, uniformly mixing and grinding, loading into a 100ml crucible, covering a crucible cover, and placing the crucible into a muffle furnace; setting a muffle furnace to raise the temperature from room temperature to 550 ℃, controlling the reaction time to be 4 hours, controlling the heating rate to 25 ℃/min, and naturally cooling to room temperature after calcining to obtain the modified g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Thermal oxidation stripping: grinding the calcined sample into powder in an agate mortar, weighing 0.1g of powder, and spreading the powder on a ceramic plate with the diameter of 10 cm; calcining in muffle furnace at 550deg.C for 3 hr at heating rate of 2deg.C/min, naturally cooling to room temperature after calcining, and collecting to obtain modified g-C 3 N 4 A nanosheet;
the results of the photocatalytic hydrogen production test show that the modified g-C prepared in example 3 3 N 4 The photocatalytic hydrogen production performance of the nano sheet is non-stripping modified g-C 3 N 4 4.2 times that of the stripped pure g-C prepared by the traditional thermal polymerization method 3 N 4 The photocatalytic hydrogen production performance of (C) is that of pure g-C which is not stripped 3 N 4 2.2 times of (2); block g-C prepared by traditional thermal polymerization method 3 N 4 Comparative, modified g-C prepared in example 3 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is improved by 8 times.
Example 4
Weighing 10g of dicyandiamide and 0.02g of allantoin, uniformly mixing and grinding, putting into a 100ml crucible, covering a crucible cover, and placing the crucible into a muffle furnace; setting a muffle furnace, raising the temperature from room temperature to 520 ℃, reacting for 4 hours, and naturally cooling to room temperature after calcining to obtain modified g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Grinding the calcined sample into powder in an agate mortar, weighing 0.1g of powder, and spreading the powder on a ceramic plate with the diameter of 10 cm; calcining in muffle furnace at 550deg.C for 4 hr at heating rate of 2deg.C/min, naturally cooling to room temperature after calcining, and collecting to obtain modified g-C 3 N 4 A nanosheet;
the results of the photocatalytic hydrogen production test show that the modified g-C prepared in example 4 3 N 4 The photocatalytic hydrogen production performance of the nano sheet is non-stripping modified g-C 3 N 4 3 times that of the stripped pure g-C prepared by the traditional thermal polymerization method 3 N 4 The photocatalytic hydrogen production performance of (C) is that of pure g-C which is not stripped 3 N 4 1.6 times of (2); block g-C prepared by traditional thermal polymerization method 3 N 4 Comparative, modified g-C prepared in example 4 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is improved by 5 times.
When the thermal oxidation stripping is performed for more than 4 hours, the obtained modified g-C 3 N 4 The nanoplatelet yield is too low.
In summary, pure g-C prepared by the thermal polymerization process 3 N 4 And modifying g-C 3 N 4 Compared with the prior art, the molecular scaffold embedding can better promote the modified g-C after thermal oxidation stripping 3 N 4 The photocatalytic hydrogen production performance of the nano-sheet is obviously improved.
As shown in FIGS. 1 and 2, modified g-C 3 N 4 With pure g-C 3 N 4 Compared with the appearance with thinner layer number and multiple folds. From FIG. 3, it can be seen that the modified g-C 3 N 4 And pure g-C 3 N 4 In contrast, modified g-C, whether thermally oxidized or not 3 N 4 The photocatalytic hydrogen production amount of the catalyst is obviously higher than that of pure g-C 3 N 4 Hydrogen production amount of (2).
In this solution, the high temperature resistant container is a ceramic crucible, the calcination device is a muffle furnace, the mortar is an agate mortar, the above is merely an example and illustration of the inventive concept, and those skilled in the art can make various modifications or supplements to or replace the described specific embodiments in a similar way, so long as they do not deviate from the inventive concept or exceed the scope defined in the claims.
Claims (3)
1. Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is characterized by comprising the following steps:
(1) Uniformly mixing a reaction precursor and a molecular bracket with a three-dimensional structure, and calcining at a high temperature to synthesize the block modified g-C 3 N 4 ；
The reaction precursor is an organic compound with a triazine ring structure or an organic compound capable of generating the triazine ring structure through polycondensation reaction;
(2) Modifying g-C with the block obtained in step (1) 3 N 4 Taking the modified g-C as a raw material, and performing thermal oxidation stripping to obtain the modified g-C 3 N 4 A nanosheet;
the molecular scaffold with the three-dimensional structure is allantoin; the mass ratio of the molecular scaffold with the three-dimensional structure to the reaction precursor is-0.02-0.3:10;
the specific process of the step (1) is as follows: uniformly mixing a reaction precursor and a molecular bracket with a three-dimensional structure, placing the mixture in a high-temperature resistant container, placing the high-temperature resistant container with the uniformly mixed reaction precursor and the molecular bracket with the three-dimensional structure in a calcining device, setting the calcining device to rise to 520-550 ℃ from room temperature, and calcining for 4 hours under the condition of 520-550 ℃; the temperature rising rate of the calcining equipment in the step (1) is controlled to be 25 ℃/min;
the specific process of the step (2) is as follows: modifying the block body to g-C 3 N 4 Grinding into powder in a mortar, spreading the powder on a ceramic sheet, placing the ceramic sheet with the powder in a calcining device, setting the calcining device to raise the temperature from room temperature to 520-550 ℃, and calcining for 3 hours at 520-550 ℃; the temperature rising rate of the calcining equipment in the step (2) from room temperature to 520-550 ℃ is 2 ℃/min.
2. Such as weightThe method for preparing more easily-strippable g-C by embedding a three-dimensional molecule according to claim 1 3 N 4 The method is characterized in that the high-temperature calcination synthesis temperature in the step (1) is 520-550 ℃ and the reaction time is 1-4 hours; the temperature of the thermal oxidation stripping in the step (2) is 520-550 ℃, and the stripping time is 1-3 hours.
3. The method of claim 1, wherein the method comprises preparing more easily peelable g-C 3 N 4 Is characterized in that the reaction precursor in step (1) is melamine or dicyandiamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010051384.5A CN111232939B (en) | 2020-01-17 | 2020-01-17 | Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010051384.5A CN111232939B (en) | 2020-01-17 | 2020-01-17 | Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111232939A CN111232939A (en) | 2020-06-05 |
| CN111232939B true CN111232939B (en) | 2023-06-09 |
Family
ID=70868255
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010051384.5A Active CN111232939B (en) | 2020-01-17 | 2020-01-17 | Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111232939B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232458A (en) * | 2013-04-25 | 2013-08-07 | 大连理工大学 | Method for preparing graphite phase carbon nitride material with monatomic layer structure |
| CN108355698A (en) * | 2018-02-13 | 2018-08-03 | 西安理工大学 | A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder |
| CN109046420A (en) * | 2018-07-09 | 2018-12-21 | 江苏大学 | A kind of preparation method of nitride porous carbon photochemical catalyst |
-
2020
- 2020-01-17 CN CN202010051384.5A patent/CN111232939B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232458A (en) * | 2013-04-25 | 2013-08-07 | 大连理工大学 | Method for preparing graphite phase carbon nitride material with monatomic layer structure |
| CN108355698A (en) * | 2018-02-13 | 2018-08-03 | 西安理工大学 | A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder |
| CN109046420A (en) * | 2018-07-09 | 2018-12-21 | 江苏大学 | A kind of preparation method of nitride porous carbon photochemical catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111232939A (en) | 2020-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107098323B (en) | A kind of g-C3N4Nanometer sheet and the preparation method and application thereof | |
| CN112169819A (en) | g-C3N4 (101)-(001)-TiO2Preparation method and application of composite material | |
| CN102886270B (en) | SiC is nanocrystalline/Graphene hetero-junctions and preparation method and application | |
| CN111545235A (en) | 2D/2Dg-C3N4CoAl-LDH hydrogen-production heterojunction material and preparation method and application thereof | |
| CN107983387B (en) | Preparation method and application of carbon nitride/bismuth selenate composite material | |
| CN110624550B (en) | In-situ carbon-coated copper-nickel alloy nanoparticle photocatalyst and preparation method and application thereof | |
| CN111085236A (en) | Preparation method of flexible recyclable photocatalytic film of carbon cloth loaded boron-doped graphite-phase carbon nitride | |
| CN115007194A (en) | Preparation method and application of amorphous boron-doped carbon nitride | |
| CN111841583B (en) | Preparation method of indium selenide/titanium dioxide nanosheet composite material | |
| CN108927197B (en) | g-C with high catalytic performance3N4Preparation method and use of | |
| CN113000061B (en) | Preparation method of banded graphite carbon nitride nanosheets | |
| CN113058601B (en) | Preparation method and application of ternary composite catalyst for photocatalytic hydrogen production by water splitting | |
| CN111298824B (en) | Graphite-like carbon nitride-based photocatalytic composite material and preparation method and application thereof | |
| CN112479248B (en) | Preparation method of strontium titanate with adjustable strontium vacancy and application of strontium titanate in field of photocatalytic hydrogen production | |
| CN111232939B (en) | Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2) | |
| CN113385210A (en) | Photocatalytic hydrogen production catalyst and preparation method and application thereof | |
| CN112962114A (en) | Photocatalytic full-hydrolysis/fuel cell integrated system and preparation method | |
| CN111644185A (en) | Bi stripping by cell crusher3O4Method for Cl and in photocatalytic reduction of CO2Application of aspects | |
| CN115181265B (en) | Methylene modified covalent triazine framework material and preparation method and application thereof | |
| CN111097475A (en) | Hydrogen peroxide modified graphite phase carbon nitride nanosheet and preparation method thereof | |
| CN111330617B (en) | Bismuth metal loaded tungsten nitride photocatalyst and preparation method and application thereof | |
| CN110124650B (en) | graphene/TiO2Compound, preparation method and method for catalyzing water decomposition to produce hydrogen by using compound as catalyst | |
| CN112058289A (en) | Strontium titanate/strontium carbonate heterojunction photocatalyst and preparation method and application thereof | |
| CN113697783B (en) | Porous g-C 3 N 4 Preparation method and application of nano-sheet | |
| CN113751050B (en) | Graphite-phase carbon nitride/graphene composite photocatalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |