CN110280299B - Flake-shaped g-C3N4Nanosheet and preparation method thereof - Google Patents
Flake-shaped g-C3N4Nanosheet and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000002135 nanosheet Substances 0.000 claims abstract description 35
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001626 barium chloride Inorganic materials 0.000 claims description 2
- 239000002055 nanoplate Substances 0.000 claims 6
- 230000001699 photocatalysis Effects 0.000 abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001257 hydrogen Substances 0.000 abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 16
- 150000003839 salts Chemical class 0.000 abstract description 12
- 238000005215 recombination Methods 0.000 abstract description 6
- 230000006798 recombination Effects 0.000 abstract description 6
- 230000031700 light absorption Effects 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000007792 addition Methods 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- 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
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- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to the technical field of nano materials, photocatalysis and water cracking hydrogen evolution detection, in particular to a scale-shaped g-C3N4Nanosheets and method for preparing same, scaly g-C of the invention3N4g-C in nanosheets3N4The nano-sheet is a fine and regular flaky structure, and g-C3N4The nano-scale is 50-600 nm in size and g-C3N4The thickness of the nanosheet is 5-30 nm. Scale-like g-C of the present invention3N4The nano-sheet is prepared by mixing three salts and a nitrogen-containing organic raw material and then calcining. g-C of the invention3N4The nano-sheet has a unique flaky structure, has higher crystallinity, can effectively expand the light absorption range, reduce the recombination probability of photo-generated electron-hole pairs, improve the photocatalytic activity and the water-splitting hydrogen evolution performance, and can be effectively applied to the technical field of photocatalytic water-splitting hydrogen evolution.
Description
Technical Field
The invention relates to the technical field of nano materials and photocatalytic water decomposition detection, in particular to a scaly g-C3N4Nanosheets and a method for preparing the same.
Background
With the progress of industrialization and urbanization deepening, fossil energy on the earth gradually becomes exhausted, and meanwhile, serious environmental problems are caused, and irreversible damage is generated to ecological balance. Therefore, the production mode using non-renewable fossil energy as a raw material is gradually eliminated, and the search for an energy source with high efficiency, energy conservation and environmental protection as a substitute becomes a research focus of current researchers. Currently, the photocatalytic and photocatalytic water-splitting hydrogen evolution technology is favored by many researchers, g-C3N4The nano material has good development prospect in the aspects of photocatalysis and photocatalytic water splitting hydrogen evolution. This is because its unique layered structure, suitable band gap and non-toxicity make it an excellent photocatalyst. But g-C3N4Has the defects of serious agglomeration, low visible light absorption, high recombination probability of photo-generated electron-hole pairs and the like, and greatly limits the g-C3N4The catalyst is further applied to the aspects of photocatalysis and photocatalytic water cracking hydrogen evolution. How to reduce g-C3N4The agglomeration phenomenon of the catalyst, the enhancement of light absorption capacity, the reduction of the probability of photo-generated electron-hole recombination and the improvement of the photocatalytic performance are difficult problems. Heretofore, methods such as exfoliation, recombination with a narrow bandgap semiconductor, and modification with monoatomic nanoparticles have been employed. The method is a popular research direction at present, and most of the traditional preparation methods are one or two salts mixed with urea or dicyandiamide and then calcined to obtain the modified photocatalyst, but the morphology of the photocatalyst is not easy to regulate and control and is still in an amorphous state, and the improvement of the photocatalytic performance of the photocatalyst is limited. Therefore, there is a need for a more efficient method for preparing g-C with controllable morphology and excellent photocatalytic performance3N4A photocatalyst.
Disclosure of Invention
In view of the above problems, the object of the present invention is: providing a flaky g-C3N4Nanosheet and preparation method thereof, aiming at obtaining g-C with adjustable and controllable morphology3N4Nanosheets, enhanced light absorption and reduced photogenerated electronsProbability of hole recombination to increase g-C3N4The nano-sheet has photocatalytic performance under the irradiation of visible light, can widen the spectral response range, and can be effectively applied to the technical field of photocatalysis.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
flake-shaped g-C3N4Nanosheets, said g-C3N4The nano-sheet is a fine and regular flaky structure, and g-C3N4The nano-scale is 50-600 nm in size and g-C3N4The thickness of the nanosheet is 5-30 nm.
Flake-shaped g-C3N4The preparation method of the nanosheet specifically comprises the following steps:
(1) dissolving a nitrogen-containing organic raw material and mixed inorganic salt in distilled water, stirring for 1-10 hours, and evaporating to dryness;
(2) placing the mixture after evaporation into a box furnace, heating and preserving heat to prepare the g-C with the scale-like characteristic3N4Nanosheets.
Preferably, the nitrogen-containing organic raw material in the step (1) is one or a mixture of more of cyanamide, dicyandiamide and melamine.
Preferably, the mixed inorganic salt in step (1) is BaCl2A mixture of KCl and NaCl.
Preferably, BaCl is mixed with the inorganic salt in the step (1)2And the mass ratio of KCl to NaCl is 1:3: 2-5: 3: 2.
Preferably, the mass ratio of the nitrogen-containing organic raw material to the mixed inorganic salt in the step (1) is 1: 9-9: 1.
Preferably, the drying temperature in the step (1) is 60-90 ℃.
Preferably, the heating temperature in the step (2) is 560-620 ℃, and the heat preservation time is 1-4 h.
Compared with the prior art, the invention has the beneficial effects that:
compared with the preparation method of directly calcining one or two salts and other nitrogen-containing organic raw materials together, the preparation method of the invention obtains g-C3N4The nano-sheet has a unique flaky structure and higher crystallinity, and can effectively expand the light absorption range, reduce the recombination probability of photo-generated electron-hole pairs and improve the photocatalytic activity and the water cracking hydrogen evolution performance of the nano-sheet.
Drawings
FIG. 1 shows g-C obtained by directly calcining a nitrogen-containing organic raw material3N4And g-C prepared in examples 1, 2 and 33N4A nano-sheet photocatalytic hydrogen evolution performance contrast diagram.
From FIG. 1 it can be seen that g-C is calcined after mixing the three salts with the nitrogen-containing organic raw material3N4The photocatalytic hydrogen evolution performance of the nano-sheet is greatly improved.
FIG. 2 shows g-C obtained by directly calcining a nitrogen-containing organic raw material3N4And g-C prepared in example 13N4TEM appearance comparison of nanosheets, wherein (i) is g-C directly calcined by a nitrogen-containing organic raw material3N4Morphology, (ii) is the morphology of the sample of example 1.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention is further described with reference to the following examples, which are intended to be illustrative and illustrative only, and various modifications, additions and substitutions for the specific embodiments described herein may be made by those skilled in the art without departing from the spirit of the invention or exceeding the scope of the claims.
Example 1
Flake-shaped g-C3N4A method of making nanoplatelets comprising the steps of:
(1) mixing melamine with three salts at a mass ratio of 1:1 (wherein the three salts are BaCl)2KCl and NaCl are mixed according to the mass ratio of 5:3: 2), the mixture is poured into a beaker containing distilled water, and then stirring and drying are carried out (wherein the stirring time is 1-10 hours, preferably 5 hours, and the drying temperature is 60-90 ℃, preferably 80 ℃);
(2) placing the mixture after evaporation in a boxHeating to 565 ℃ in a furnace, and preserving heat for 4 hours to prepare the g-C with the scaly characteristic3N4Nanosheets.
Tests show that g-C prepared according to the steps3N4The hydrogen evolution rate of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 25616 mu mol.h-1·g-1About 34.5 times the photolytic hydroevolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Example 2
The preparation process of this example is the same as example 1, except that the heating temperature in step (2) is 580 ℃.
Sample obtained in this example, g-C3N4The nanosheets have uniform surface distribution, no amorphous agglomeration phenomenon and unique microscopic morphology, and are tested to prepare the g-C3N4The rate of hydrogen evolution of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 28036 mu mol.h-1·g-1About 37.8 times the photolytic hydrolysis hydrogen evolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Example 3
The preparation method of this example is the same as example 1, except that the heating temperature in step (2) is 600 ℃.
Sample obtained in this example, g-C3N4The nanosheets have uniform surface distribution, no amorphous agglomeration phenomenon and unique microscopic morphology, and are tested to prepare the g-C3N4The hydrogen evolution rate of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 25730 mu mol.h-1·g-1About 34.6 times the photolytic hydroevolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Example 4
The preparation method of this example is the same as example 1, except that the heating temperature in step (2) is 620 ℃ and the holding time is 1 h.
Sample obtained in this example, g-C3N4The nano-sheet surface is uniformly distributed without amorphous agglomerationThe g-C prepared according to the steps is tested and has unique micro-morphology3N4The hydrogen evolution rate of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 23044 mu mol.h-1·g-1About 31.0 times the photolytic hydroevolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Example 5
The preparation method of this example is the same as example 4, except that the heat preservation time in step (2) is 1.5 h.
Sample obtained in this example, g-C3N4The nanosheets have uniform surface distribution, no amorphous agglomeration phenomenon and unique microscopic morphology, and are tested to prepare the g-C3N4The hydrogen evolution rate of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 21211 mu mol.h-1·g-1About 28.5 times the photolytic hydroevolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Example 6
The preparation method of this example is the same as example 4, except that the temperature-keeping time in step (2) is 2 hours.
Sample obtained in this example, g-C3N4The nanosheets have uniform surface distribution, no amorphous agglomeration phenomenon and unique microscopic morphology, and are tested to prepare the g-C3N4The hydrogen evolution rate of the nano-sheet by photocatalytic hydrolysis under the irradiation of visible light is 9433 mu mol.h-1·g-1About 12.7 times the photolytic hydroevolution performance of the coarse powder calcined from the nitrogen-containing organic feedstock without the addition of the three salts.
Claims (6)
1. Flake-shaped g-C3N4A nanoplate characterized by: said g-C3N4The nano-sheet is a fine and regular flaky structure, and g-C3N4The nano-scale is 50-600 nm in size and g-C3N4The thickness of the nanosheet is 5-30 nm;
the scale-like g-C3N4Preparation of nanosheetsThe method specifically comprises the following steps:
(1) dissolving a nitrogen-containing organic raw material and mixed inorganic salt in distilled water, stirring for 1-10 hours, and evaporating to dryness, wherein the mixed inorganic salt is BaCl2A mixture of KCl and NaCl;
(2) placing the mixture after evaporation into a box furnace, heating and preserving heat to prepare the g-C with the scale-like characteristic3N4Nanosheets.
2. The flaky g-C of claim 13N4A nanoplate characterized by: the nitrogen-containing organic raw material in the step (1) is one or a mixture of more of cyanamide, dicyandiamide and melamine.
3. The flaky g-C of claim 13N4A nanoplate characterized by: mixing BaCl in inorganic salt in step (1)2And the mass ratio of KCl to NaCl is 1:3: 2-5: 3: 2.
4. The flaky g-C of claim 13N4A nanoplate characterized by: the mass ratio of the nitrogen-containing organic raw material to the mixed inorganic salt in the step (1) is 1: 9-9: 1.
5. The flaky g-C of claim 13N4A nanoplate characterized by: the evaporation temperature in the step (1) is 60-90 ℃.
6. The flaky g-C of claim 13N4A nanoplate characterized by: the heating temperature in the step (2) is 560-620 ℃, and the heat preservation time is 1-4 h.
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| CN113318765B (en) * | 2021-05-28 | 2023-09-22 | 江苏大学 | Preparation method and application of ultrathin high-crystallization carbon nitride photocatalyst |
| CN113559911B (en) * | 2021-07-30 | 2022-09-13 | 中国科学院生态环境研究中心 | Monoatomic catalyst, preparation method and application thereof |
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