CN110639585A - Copolymerization modified layered graphite phase carbon nitride photocatalyst and preparation method and application thereof - Google Patents
Copolymerization modified layered graphite phase carbon nitride photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000007334 copolymerization reaction Methods 0.000 title claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 16
- 239000010439 graphite Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 239000010453 quartz Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
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- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 238000003892 spreading Methods 0.000 claims description 7
- 230000007480 spreading Effects 0.000 claims description 7
- 239000004065 semiconductor Substances 0.000 claims description 6
- PCCVSPMFGIFTHU-UHFFFAOYSA-N tetracyanoquinodimethane Chemical compound N#CC(C#N)=C1C=CC(=C(C#N)C#N)C=C1 PCCVSPMFGIFTHU-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000003421 catalytic decomposition reaction Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
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- 230000007547 defect Effects 0.000 description 3
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- 238000011161 development Methods 0.000 description 2
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- 238000013508 migration Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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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
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Abstract
The invention discloses a preparation method and application of a copolymerization modified lamellar graphite phase carbon nitride photocatalyst, belonging to the technical field of material preparation and photocatalysis. The graphite-phase carbon nitride photocatalyst with a nano-layered structure prepared by copolymerization is prepared by taking melamine and TCNQ as precursors and carrying out high-temperature copolymerization. Compared with the traditional bulk-phase carbon nitride, the graphite-phase carbon nitride photocatalyst prepared by the invention has the advantages of enhanced visible light absorption and high-efficiency photocatalytic hydrogen production performance. The preparation method is simple in preparation process and high in catalysis efficiency, and has wide potential application prospect in the field of photocatalysis.
Description
Technical Field
The invention relates to a preparation method and application of a copolymerization modified lamellar graphite phase carbon nitride photocatalyst, belonging to the technical field of preparation of semiconductor nano materials and photocatalysis.
Background
Energy shortages and environmental issues have become two major issues currently facing human society. The development of sustainable, clean and pollution-free new energy has great significance for solving the two problems and realizing the sustainable development of human beings. Solar energy is widely recognized in the world today as the best alternative to fossil fuels as a sustainable, pollution-free, ubiquitous and energy-intensive source of energy. However, solar energy has no continuity and stability in space and time, so that it is currently difficult to directly utilize the solar energy on a large scale. The photocatalytic water splitting hydrogen production only needs one step to convert solar energy into hydrogen energy, is one of the best ways for solar energy conversion, and is one of the most attractive ways for producing hydrogen by using renewable energy sources. The key point is to prepare the efficient, stable and nontoxic visible light catalytic material.
Graphite phase carbon nitride is a typical polymer semiconductor with C, N sp atoms in its molecular structure2Hybridization results in the formation of highly delocalized pi-conjugated systems. The forbidden band width is about 2.7eV, and the absorption is strong in the visible light region. In addition, the material also has the advantages of simple preparation, low cost, high stability, no toxicity and the like, and is concerned by extensive researchers. However, graphite-phase carbon nitride has a relatively large band gap width and a narrow range of response to visible light; the defects of high recombination probability of photon-generated carriers and the like seriously restrict the wide application of the photo-generated carriers in the fields of photocatalysis and energy. At present, the modification of carbon nitride mainly comprises the following steps: morphology regulation, element doping, surface modification, semiconductor compounding, precious metal deposition, copolymerization modification and the like. Among them, the copolymerization modification is considered to be a better modification method due to the advantages of rich raw material sources, simple operation and the like.
The conjugated structure of the carbon nitride is regulated and controlled by a copolymerization means, the surface active sites are increased, the band gap width of a semiconductor is reduced, the separation and migration of photon-generated carriers are promoted, the utilization efficiency of sunlight is improved, and the photocatalytic hydrogen production performance is effectively improved. At present, 7,7,8, 8-Tetracyanoquinodimethane (TCNQ) is mostly used in the aspect of capacitors, and is rarely applied to the preparation of photocatalysts.
Disclosure of Invention
The invention aims to provide a copolymerization modified layered graphite phase carbon nitride photocatalyst with low preparation cost and simple process, and a preparation method and application thereof.
The invention is realized by adopting the following technical scheme:
a copolymerization modified lamellar graphite phase carbon nitride photocatalyst is prepared by taking melamine and 7,7,8, 8-Tetracyanoquinodimethane (TCNQ) as precursors through high-temperature copolymerization. The molecular structure of the photocatalyst contains-CN, and the photocatalyst is a polymer semiconductor.
The invention also provides a preparation method of the copolymerization modified lamellar graphite phase carbon nitride photocatalyst, which comprises the following steps:
1) and uniformly grinding the melamine and the TCNQ in a mortar to obtain mixed solid powder.
2) Uniformly spreading the mixed solid powder obtained in the step 1) in a quartz boat, placing the quartz boat in a tube furnace, heating the quartz boat to 500-550 ℃ at a certain heating rate in an air atmosphere, keeping the temperature for 2-6h, and cooling the quartz boat to room temperature to obtain the copolymerization modified layered graphite-phase carbon nitride photocatalyst.
Further, the mass ratio of melamine to TCNQ in step 1) is 100: 0.1-10. Further, the range is 100: the photocatalytic performance of the sample obtained is best between 0.1 and 0.5.
Further, the temperature rise rate in the step 2) is 2-10 ℃/min.
The invention also provides an application of the copolymerization modified lamellar graphite phase carbon nitride photocatalyst, and the copolymerization modified lamellar graphite phase carbon nitride photocatalyst can be used for preparing hydrogen by decomposing water under the catalysis of visible light.
The invention has the advantages that:
1) the invention introduces TCNQ to g-C by means of copolymerization for the first time3N4In the molecular structure of (A), reinforcing g-C3N4The conjugated structure reduces the band gap width and improves the separation and migration efficiency of the photon-generated carriers.
2) The copolymerization modified laminated graphite phase carbon nitride photocatalyst has the advantages of simple preparation method, good repeatability, high yield, stable structure of the prepared composite photocatalyst and excellent performance.
3) Copolymerization modified lamellar graphite phase carbon nitride photocatalyst (g-C)3N4TCNQ) has better performance of photolyzing water to produce hydrogen under sunlight than pure g-C3N4The hydrogen production effect is improved by several times.
Drawings
Fig. 1 is an XRD diffraction pattern of example 1/2 and comparative example 1.
Fig. 2 is SEM pictures of example 1/2 and comparative example 1.
FIG. 3 is a photograph of UV-vis of example 2 and comparative example 1.
FIG. 4 is a photo-catalytic hydrogen production performance picture of example 1/2 and comparative example 1.
Detailed Description
Example 1
(1) Adding 5g of melamine and 5mg of TCNQ into a ceramic mortar, and continuously and fully grinding to obtain mixed solid powder;
(2) uniformly spreading the mixed solid powder prepared in the step (1) in a quartz boat, placing the quartz boat in a tube furnace, heating to 520 ℃ at a heating rate of 5 ℃/min in the air atmosphere, keeping the temperature for 4 hours, and then cooling to room temperature along with the furnace to obtain the copolymerization modified laminar graphite-phase carbon nitride photocatalyst (g-C)3N4/TCNQ0.1％)。
Example 2
(1) Adding 5g of melamine and 10mg of TCNQ into a ceramic mortar, and continuously and fully grinding to obtain mixed solid powder;
(2) uniformly spreading the mixed solid powder prepared in the step (1) in a quartz boat, placing the quartz boat in a tube furnace, heating to 520 ℃ at a heating rate of 5 ℃/min in the air atmosphere, keeping the temperature for 4 hours, and then cooling to room temperature along with the furnace to obtain the copolymerization modified laminar graphite-phase carbon nitride photocatalyst (g-C)3N4/TCNQ0.2％)。
Example 3
(1) Adding 5g of melamine and 25mg of TCNQ into a ceramic mortar, and continuously and fully grinding to obtain mixed solid powder;
(2) will be described in step (1)Uniformly spreading the prepared mixed solid powder in a quartz boat, placing in a tube furnace, heating to 520 ℃ at a heating rate of 5 ℃/min in the air atmosphere, keeping for 4h, and cooling to room temperature along with the furnace to obtain the copolymerization modified laminar graphite-phase carbon nitride photocatalyst (g-C)3N4/TCNQ0.5％)。
Example 4
(1) Adding 5g of melamine and 500mg of TCNQ into a ceramic mortar, and continuously and fully grinding to obtain mixed solid powder;
(2) uniformly spreading the mixed solid powder prepared in the step (1) in a quartz boat, placing the quartz boat in a tube furnace, heating to 520 ℃ at a heating rate of 5 ℃/min in the air atmosphere, keeping the temperature for 4 hours, and then cooling to room temperature along with the furnace to obtain the copolymerization modified laminar graphite-phase carbon nitride photocatalyst (g-C)3N4/TCNQ10％)。
Comparative example 1
(1) Adding 5g of melamine into a ceramic mortar, and continuously and fully grinding to obtain uniform solid powder;
(2) spreading the uniform solid powder prepared in the step (1) in a quartz boat, placing the quartz boat in a tube furnace, heating to 520 ℃ at a heating rate of 5 ℃/min in the air atmosphere, keeping the temperature for 4h, and then cooling to room temperature along with the furnace to obtain pure g-C3N4A photocatalyst.
The obtained photocatalyst was tested, and the test results are shown in fig. 1 to 4. Fig. 1 is an XRD diffraction pattern of example 1/2 and comparative example 1. From the figure, it can be seen that two distinct diffraction peaks of graphite phase carbon nitride (100) and (002) appear at 13.1 and 27.4, indicating that the structure of graphite phase carbon nitride is not affected by the copolymerization modification.
Fig. 2 is SEM pictures of example 1/2 and comparative example 1. As can be seen from the figure, the graphite phase carbon nitride prepared by the method has the appearance characteristic of layered stacking; without the pure g-C prepared by the process of the invention3N4Photocatalysts tend to be blocky and do not have the morphological characteristics of layered stacking.
FIG. 3 is a photograph of UV-vis of example 2 and comparative example 1. It can be seen from the figure that the absorption of the sample after copolymerization modification in the visible light region is obviously enhanced.
FIG. 4 is a photo-catalytic hydrogen production performance picture of example 1/2 and comparative example 1. 10mg of catalyst and reagent (2 vol.% in 30mL triethanolamine solution, in situ photo-reduction of H2PtCl6I.e., 2 wt.% Pt) was conducted in the reactor. As can be seen from the figure, the hydrogen production efficiency of the photocatalyst prepared in example 1 under simulated sunlight (xenon lamp 300W, AM1.5G filter) reaches 262 mu mol/h/g, which is compared with the pure g-C of comparative example 13N4The (74. mu. mol/h/g) ratio was increased by 3.5 times, and the photocatalyst prepared in example 2 was increased by 5.7 times under the same experimental conditions. As the pi defect of the carbon nitride is derived from an N atom with high electronegativity, and a C atom with low electronegativity replaces the N atom, the pi conjugated structure can be regulated and controlled, so that the pi defect is reduced. Since TCNQ structurally contains a benzene ring, 6C atoms are contained. Therefore, the photocatalytic performance of the melamine can be effectively enhanced by adding TCNQ into the melamine.
Claims (6)
1. The layered graphite-phase carbon nitride photocatalyst modified by copolymerization is characterized in that the photocatalyst is formed by sintering melamine powder doped with 7,7,8, 8-tetracyanoquinodimethane, and the molecular structure of the photocatalyst contains-CN which is a polymer semiconductor.
2. A method for preparing a copolymerization-modified layered graphite-phase carbon nitride photocatalyst according to claim 1, characterized in that: the method comprises the following steps:
1) uniformly grinding melamine and 7,7,8, 8-tetracyanoquinodimethane in a mortar to obtain mixed solid powder;
2) uniformly spreading the mixed solid powder obtained in the step 1) in a quartz boat, placing the quartz boat in a tube furnace, heating the quartz boat to 500-550 ℃ in the air atmosphere, keeping the temperature for 2-6h, and cooling the quartz boat to room temperature to obtain the copolymerization modified layered graphite-phase carbon nitride photocatalyst.
3. The method for preparing a layered graphite-phase carbon nitride photocatalyst through copolymerization modification according to claim 2, wherein the mass ratio of melamine to 7,7,8, 8-tetracyanoquinodimethane in the step 1) is 100: 0.1-10.
4. The method for preparing a layered graphite-phase carbon nitride photocatalyst through copolymerization modification according to claim 2, wherein the mass ratio of melamine to 7,7,8, 8-tetracyanoquinodimethane in the step 1) is 100: 0.1-0.5.
5. The method for preparing the layered graphite-phase carbon nitride photocatalyst modified by copolymerization according to claim 2, wherein the temperature increase rate in the step 2) is 2 to 10 ℃/min.
6. The use of the copolymerization-modified layered graphite phase carbon nitride photocatalyst according to claim 1, wherein the copolymerization-modified layered graphite phase carbon nitride photocatalyst is used for producing hydrogen by visible light catalytic decomposition of water.
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| CN111495414A (en) * | 2020-06-03 | 2020-08-07 | 上海大学 | Phenol-doped g-C3N4Nanosheet and preparation method thereof |
| CN112973792A (en) * | 2021-02-03 | 2021-06-18 | 江苏大学 | Modified photocatalyst with large pi bond expanded by cross-linked bridging molecules and preparation method and application thereof |
| CN113600239A (en) * | 2021-08-09 | 2021-11-05 | 华侨大学 | Triptycene modified graphite-phase carbon nitride and preparation method and application thereof |
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| CN113600239A (en) * | 2021-08-09 | 2021-11-05 | 华侨大学 | Triptycene modified graphite-phase carbon nitride and preparation method and application thereof |
| CN113600239B (en) * | 2021-08-09 | 2023-04-11 | 华侨大学 | Triptycene modified graphite-phase carbon nitride and preparation method and application thereof |
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