CN110420656B - Gas-phase acidified g-C3N4 nanosheet and preparation method thereof - Google Patents
Gas-phase acidified g-C3N4 nanosheet and preparation method thereof Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000003929 acidic solution Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 24
- 239000001257 hydrogen Substances 0.000 abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 24
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000002064 nanoplatelet Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 19
- 238000005054 agglomeration Methods 0.000 description 11
- 230000002776 aggregation Effects 0.000 description 11
- 238000006303 photolysis reaction Methods 0.000 description 10
- 230000015843 photosynthesis, light reaction Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000005336 cracking Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 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
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- 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
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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
- C01B3/042—Decomposition of water
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- 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
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- 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
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Abstract
The invention relates to the technical field of nano materials and photocatalytic hydrogen evolution, in particular to gas-phase acidified g-C3N4A method of making nanoplatelets comprising the steps of: the nitrogenous organic raw material is calcined at high temperature to obtain g-C3N4Coarse powder; g to C3N4Placing the coarse powder in a tubular furnace, passing nitrogen through the acidic solution at a fixed flow rate, introducing the nitrogen into the tubular furnace, heating and preserving heat for a certain time to prepare g-C3N4Nanosheets. g-C of the invention3N4The nanosheets are g-C pairs utilizing the strong oxidizing property of volatile acids3N4The coarse powder is obtained by high-temperature gas phase stripping. g-C prepared in comparison with other methods3N4Nanosheets, g-C obtained in a high temperature acidic atmosphere3N4The nano-sheet has smaller size, the specific surface area is increased, and the g-C can be improved3N4The nano-sheet has photocatalytic performance under the irradiation of visible light, and can be effectively applied to the technical field of photocatalytic hydrogen evolution.
Description
Technical Field
The invention relates to the field of nano materials and photocatalytic hydrogen evolution, in particular to gas-phase acidified g-C3N4Nanosheets and a method for preparing the same.
Background
With the continuous and deep urbanization development of the world, the industrialization degree is higher and higher, the dependence on the traditional fossil energy is also higher and higher, and the energy crisis therewith becomes a serious problem which all human beings must face. Therefore, there is a need for a green, environmentally friendly, sustainable solution to the energy shortage problem. This is almost achieved by means of photocatalytic techniquesInexhaustible solar energy is converted into hydrogen energy, and photocatalytic water cracking draws great attention of many researchers. Wherein g-C3N4The nano material has good development prospect in the aspects of photocatalysis and photocatalytic water cracking. Relative to other photocatalysts studied, graphite carbide (g-C)3N4) Due to the appropriate band gap, no toxicity, adjustable electronic structure and high chemical stability, the catalyst becomes a new star of semiconductor catalysts. However, g-C3N4The agglomeration phenomenon of coarse powder is serious and the coarse powder presents a block shape with the size of a few micrometers, so that the active sites of the reaction are fewer, and the photocatalytic process is not facilitated. For g-C3N4The coarse powder is effectively stripped and etched to obtain g-C with smaller size and larger specific surface area3N4The nano-sheet further improves the photocatalytic performance of the nano-sheet, and the g-C with thinner sheet layer and smaller size is obtained by adopting ultrasonic stripping, liquid phase stripping and thermal oxidation stripping3N4Nanoplatelets are the most common approach. But using ultrasonic stripping to obtain g-C3N4The yield of the nano-sheets is not high, which is not beneficial to the mass synthesis and preparation of samples. The solvent may remain in the catalyst during the liquid phase stripping process, thereby affecting the photocatalytic performance thereof. Although the thermal oxidation stripping method is convenient, the stripping effect still cannot reach a perfect state. These more common stripping methods have some more or less drawbacks. Therefore, a more efficient stripping method is needed to produce g-C with smaller size and larger specific surface area3N4Nanosheets.
Disclosure of Invention
In view of the above problems, the object of the present invention is: providing a gas phase acidified g-C3N4Nanosheet and method for preparing same, aimed at obtaining finely dispersed g-C3N4The nano-sheet reduces the agglomeration phenomenon so that the nano-sheet has more active sites on the catalytic surface to improve the g-C3N4The nano sheet has photocatalytic performance under the irradiation of visible light, and can be effectively applied to the technical fields of photocatalysis and photoelectrochemistry detection.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
gas phase acidified g-C3N4A method of making nanoplatelets comprising the steps of:
(1) the nitrogenous organic raw material is calcined at high temperature to obtain g-C3N4Coarse powder;
(2) g to C3N4Placing the coarse powder in a tubular furnace, passing nitrogen through the acidic solution at a fixed flow rate, introducing the nitrogen into the tubular furnace, heating and preserving heat for a certain time to prepare g-C3N4Nanosheets.
Preferably, the calcining temperature in the step (1) is 500-550 ℃, and the heat preservation time is 2-4 h.
Preferably, the nitrogen-containing organic raw material in the step (1) is one or a mixture of urea, melamine, cyanamide and dicyandiamide.
Preferably, the flow rate of the nitrogen passing through the acidic solution in the step (2) is 0.1-1L/min.
Preferably, the acidic solution in step (2) is one or a mixture of nitric acid and hydrochloric acid.
Preferably, the concentration of the acidic solution in the step (2) is 1-5 mol/L.
Preferably, the calcining temperature in the step (2) is 450-550 ℃, and the heat preservation time is 2-8 h.
A gas phase acidified g-C prepared by the above process3N4Nanosheets, g-C3N4The surface of the nano sheet has a corrugated shape and a high specific surface area.
Compared with the prior art, the invention has the beneficial effects that:
gas phase acidified g-C of the invention3N4Compared with the traditional ultrasonic stripping, liquid phase stripping and thermal oxidation stripping preparation methods, the preparation method of the nanosheet has the advantage that the obtained g-C3N4The nano-sheets are not easy to agglomerate, have larger specific surface area, can provide more effective reaction active sites, are beneficial to the catalytic reaction, and improve the photocatalytic activity and the hydrogen desorption efficiency of water cracking.
g-C of the invention3N4The nanosheets are g-C pairs utilizing the strong oxidizing property of volatile acids3N4The coarse powder is obtained by high-temperature gas phase stripping. Gas phase acidified g-C produced by the invention3N4The nano-sheet has more active sites on the catalytic surface to improve g-C3N4The nano sheet has photocatalytic performance under the irradiation of visible light, and can be effectively applied to the technical fields of photocatalysis and photoelectrochemistry detection.
Drawings
FIG. 1 shows g-C obtained by high-temperature calcination3N4Coarse powder and g-C prepared in examples 1, 2 and 33N4And (4) comparing the performance of hydrogen evolution by photolysis of the nanosheet.
FIG. 2 shows the g-C obtained by direct calcination of a nitrogen-containing organic raw material3N4And g-C prepared in example 33N4Comparing the TEM appearance. (i) Direct calcination of the nitrogen-containing organic feedstock, (ii) morphology of the sample of example 3.
Detailed Description
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
A preparation method of gas-phase acidified g-C3N4 nanosheets comprises the following steps:
(1) taking melamine as a raw material, heating the melamine to 550 ℃, and preserving heat for 4 hours to prepare g-C3N4 coarse powder;
(2) placing g-C3N4 coarse powder in the middle of a tubular furnace, firstly passing nitrogen through a nitric acid solution with the concentration of 1 mol/L, then introducing the nitrogen into the tubular furnace, heating to 500 ℃, and then preserving heat for 2 hours to obtain gas-phase acidified g-C3N4 nanosheets.
Tests show that the hydrogen evolution rate of g-C3N4 nanosheets prepared according to the above steps by photolysis of water under visible light irradiation is 3817 mu mol.h < -1 >. g < -1 >, which is 7.2 times of the hydrogen evolution rate of g-C3N4 coarse powder which is not subjected to gas phase acidification.
Example 2
The preparation method of this example is the same as example 1, except that the temperature-keeping time in step (2) is 3 hours.
The phase-acidified sample obtained in this example, g-C3N4The nanosheet becomes thinner and thinner, no obvious agglomeration phenomenon exists, the specific surface area is increased, and the test shows that the photolysis water hydrogen evolution rate of the sample is 5360 mu mol.h under the irradiation of visible light-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 10.2 times.
Example 3
The preparation method of this example is the same as example 1, except that the temperature-keeping time in step (2) is 5 hours.
The phase-acidified sample obtained in this example, g-C3N4The nano-sheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and is tested to have the rate of hydrogen evolution by water photolysis of 7666 mu mol.h under the irradiation of visible light-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 14.5 times.
Example 4
This example was prepared as in example 3, except that the temperature was heated to 550 ℃ in step (2).
The phase-acidified sample obtained in this example, g-C3N4The nano-sheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and is tested to have the hydrogen evolution rate of 6844 mu mol.h by photolysis water under the irradiation of visible light-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 12.9 times.
Example 5
The preparation method of this example is the same as example 1, except that the concentration of the nitric acid solution in step (3) is changed to 2 mol/L.
The phase-acidified sample obtained in this example, g-C3N4The nano-sheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and has a photolysis water hydrogen evolution rate of 6530 mu mol per hour under the irradiation of visible light through tests-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 12.3 times.
Example 6
The preparation method of this example is the same as example 4, except that the concentration of the nitric acid solution in the step (2) is changed to 5 mol/L.
The phase-acidified sample obtained in this example, g-C3N4The nano-sheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and is tested to have the hydrogen evolution rate of 5119 mu mol per hour by photolysis of water under the irradiation of visible light-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder was 9.7 times.
Example 7
The preparation method of this example is the same as example 5, except that the acid solution in step (1) is changed to hydrochloric acid solution.
The phase-acidified sample obtained in this example, g-C3N4The nano-sheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and is tested to have the hydrogen evolution rate of 7253 mu mol.h by photolysis under the irradiation of visible light-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 9.9 times.
Example 8
The preparation method of this example is the same as example 1, except that in step (1), the ratio of urea to melamine by mass is 1: 1 is mixed as raw material.
The phase-acidified sample obtained in this example, g-C3N4The nanosheet becomes thinner and thinner, has no obvious agglomeration phenomenon, has increased specific surface area, and has a hydrogen evolution rate of 5653 mu mol per hour by photolysis under the irradiation of visible light through tests-1·g-1Is g-C without gas phase acidification3N4The hydrogen evolution rate of the coarse powder is 10.7 times.
FIG. 1 shows the procedure of example 1Step (1) high temperature calcination to obtain g-C3N4Coarse powder and g-C prepared in examples 1, 2 and 33N4And (4) comparing the performance of hydrogen evolution by photolysis of the nanosheet.
From the figure it can be seen that g-C is acidified via the gas phase3N4The hydrogen evolution performance of the nano-sheet in photocatalytic water cracking is greatly improved.
FIG. 2 shows the g-C obtained by direct calcination of a nitrogen-containing organic raw material3N4And g-C prepared in example 33N4Comparing the TEM appearance. (i) Direct calcination of the nitrogen-containing organic feedstock, (ii) morphology of the sample of example 3.
It is evident from the figure that g-C obtained by direct calcination of the nitrogenous organic starting material3N4The agglomeration phenomenon was severe, g-C prepared in example 33N4The corrugated coating is free from obvious agglomeration, and has small particle size and large specific surface area.
Claims (5)
1. Gas phase acidified g-C3N4The preparation method of the nanosheet is characterized by comprising the following steps:
(1) the nitrogenous organic raw material is calcined at high temperature to obtain g-C3N4Coarse powder;
(2) g to C3N4Placing the coarse powder in a tubular furnace, passing nitrogen through the acidic solution at a fixed flow rate, introducing the nitrogen into the tubular furnace, heating and preserving heat for a certain time to prepare g-C3N4The flow rate of nitrogen passing through the acid solution is 0.1-1L/min, the acid solution is one or a mixture of nitric acid and hydrochloric acid, and the concentration of the acid solution is 1-5 mol/L.
2. Gas phase acidified g-C according to claim 13N4The preparation method of the nanosheet is characterized in that in the step (1), the calcining temperature is 500-550 ℃, and the heat preservation time is 2-4 h.
3. Gas phase acidified g-C as claimed in claim 13N4The preparation method of the nanosheet is characterized in that the nitrogenous organic raw material in the step (1) is one or a mixture of urea, melamine, cyanamide and dicyandiamide.
4. Gas phase acidified g-C according to claim 13N4The preparation method of the nanosheet is characterized in that the calcining temperature in the step (2) is 450-550 ℃, and the heat preservation time is 2-8 h.
5. A gas phase acidified g-C obtainable by the process of any one of claims 1 to 43N4Nanosheets characterized by g-C3N4The surface of the nano sheet has a corrugated shape and a high specific surface area.
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| CN106732739A (en) * | 2017-02-20 | 2017-05-31 | 合肥工业大学 | A kind of g C3N4The preparation method of nanometer sheet |
| CN108380230A (en) * | 2018-01-24 | 2018-08-10 | 江苏大学 | The preparation method and application of ultra-thin graphite phase carbon nitride |
| CN109395758A (en) * | 2018-11-12 | 2019-03-01 | 江苏大学 | A kind of dimensional thinlayer CdS/g-C3N4The Preparation method and use of composite photo-catalyst |
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| CN106732739A (en) * | 2017-02-20 | 2017-05-31 | 合肥工业大学 | A kind of g C3N4The preparation method of nanometer sheet |
| CN108380230A (en) * | 2018-01-24 | 2018-08-10 | 江苏大学 | The preparation method and application of ultra-thin graphite phase carbon nitride |
| CN109395758A (en) * | 2018-11-12 | 2019-03-01 | 江苏大学 | A kind of dimensional thinlayer CdS/g-C3N4The Preparation method and use of composite photo-catalyst |
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| Title |
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| Enhanced photocatalytic performances of ultrafine g-C3N4 nanosheets obtained by gaseous stripping with wet nitrogen;Chengkong Fan;《Applied Surface Science》;20170818;第427卷;第731页第2段，第2节，图2 * |
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