CN111330611A - Graphene-modified prismatic carbon nitride, and preparation method and application thereof - Google Patents
Graphene-modified prismatic carbon nitride, and preparation method and application thereof Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 13
- 229920000877 Melamine resin Polymers 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000013032 photocatalytic reaction Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement 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
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- 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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- 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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- 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 graphene-modified prismatic carbon nitride, a preparation method and application thereof. The material consists of graphene and prismatic carbon nitride, and the graphene and the prismatic carbon nitride are compounded through the action of a covalent bond. The graphene-modified prismatic carbon nitride prepared by the method increases the specific surface area, and exposes more active sites; the absorption and utilization rate of visible light are improved; the separation and migration of photon-generated carriers are facilitated, and the catalytic activity of the visible light hydrogen production is greatly improved.
Description
Technical Field
The invention relates to a preparation method and application of graphene-modified prismatic carbon nitride, and belongs to the field of application of nano materials.
Background
Energy crisis andenvironmental pollution is two major problems in today's society. Solar energy has the advantages of cleanness, large reserves, low cost and the like, and how to effectively convert the solar energy into chemical energy becomes a hot spot which is concerned by scientists. With the rise of semiconductor photocatalytic materials, more and more efficient catalysts are likely to be applied. Graphite phase carbon nitride (g-C)3N4) As a novel visible light response photocatalysis material, the material has many advantages, such as high chemical stability, high thermal stability, safety, no toxicity, abundant raw materials, low price, easy obtainment and the like. However, ordinary g-C3N4Still have some problems to be improved, such as less specific surface area, low utilization ratio of visible light, high recombination rate of photo-generated electrons and holes, and the like, so that the application of photocatalysis is obviously restricted. In recent years, scientists have focused on how to increase g-C3N4Visible light catalytic activity and achieves breakthrough development. Zhang et al, by hydrothermal treatment of melamine, form a supramolecular precursor by self-assembly of intermolecular hydrogen bonds, and then obtain porous thin-layer carbon nitride [ J.W. Zhang, S. Gong, N. Mahood, L. Pan, X. Zhang, J.J. Zou, Oxygen-bonded nanoporous carbon nitride salt water-based rare halogenated carbohydrate supra molecular carbohydrate for photocatalytic hydrogen evolution, Applied Catalysis B: Environmental, 221 (2018) 9-16.]. Quan et al ultrasonically bonded graphite oxide to g-C3N4The composite effectively improves the catalytic activity of degrading organic dye under Visible Light [ Gaozu Liao, Shuo Chen, XieQuan, HongtaoYu and Huimin Zhuao. Graphene Oxide Modi fi ed g-C3N4 Hybrid with enhanced photo catalytic performance unit Visible Light Irradiation J. Mater. chem. 2012, 22, 2721. 2726. the organic dye has good catalytic activity.]. However, the currently reported composites of graphite oxide or graphene and carbon nitride materials are all simple layer-by-layer stacking, and a preparation method of graphene-modified prismatic carbon nitride obtained by wrapping prismatic carbon nitride with single-layer graphene and performing covalent bond action between the prismatic carbon nitride and the single-layer graphene and application of the graphene-modified prismatic carbon nitride in photocatalytic hydrogen production are not reported.
Disclosure of Invention
The invention aims to provide graphene-modified prismatic carbon nitride, a preparation method and application thereof.
The technical solution for realizing the invention is as follows: a graphene-modified prismatic carbon nitride and a preparation method thereof comprise the following steps:
firstly, carrying out hydrothermal treatment on melamine to obtain a supramolecular precursor;
secondly, mixing the supermolecule precursor with the graphite oxide solution uniformly dispersed by ultrasonic, and oscillating uniformly on a shaking table;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
and fourthly, roasting the solid obtained in the third step at 550 +/-10 ℃ for 4-6 hours to obtain the graphene-modified prismatic carbon nitride.
Furthermore, in the first step, the hydrothermal treatment temperature is 180 +/-20 ℃, and the hydrothermal treatment time is 24-48 h.
Furthermore, in the second step, the mass ratio of the supermolecule precursor to the graphite oxide is 96-99.5: 0.5-4.
The number of graphene layers in the graphene-modified prismatic carbon nitride is 1, and the graphene and the prismatic carbon nitride are compounded through a covalent bond effect and are used as a catalyst to be applied to photocatalytic hydrogen production.
Compared with the prior art, the invention has the advantages that: (1) the graphene-modified prismatic carbon nitride prepared by the method increases the specific surface area and has more active sites; (2) the graphene-modified prismatic carbon nitride prepared by the method improves the absorption and utilization rate of visible light; (3) the structure of the graphene-modified prismatic carbon nitride prepared by the invention is beneficial to separation and migration of photon-generated carriers, so that the activity of photocatalytic hydrogen production is improved.
Drawings
Fig. 1 is an XRD diffractogram of graphene-modified prismatic carbon nitride prepared in comparative example of the present invention and examples 1, 2, 3, and 4.
Figure 2 is a fourier spectrum of the graphene-modified prismatic carbon nitride prepared according to comparative example of the present invention and examples 1, 2, 3, 4.
Fig. 3 is a scanning electron microscope image of carbon field emission at 900 times (a), 2700 times (b), 7000 times (c) and a scanning electron microscope image of field emission at 2000 times (d) of the supramolecular precursor prepared in example 2 of the present invention.
Fig. 4 is a nitrogen adsorption desorption isotherm of graphene-modified prismatic carbon nitride prepared according to comparative example of the present invention and example 2.
Fig. 5 is a graph of photocatalytic hydrogen production performance of graphene-modified prismatic carbon nitride prepared according to comparative example of the present invention and examples 1, 2, 3, and 4.
Detailed description of the invention
The preparation method of the graphene-modified prismatic carbon nitride comprises the following steps:
firstly, dissolving melamine and then carrying out hydrothermal treatment for 48 hours to obtain a supramolecular precursor;
secondly, mixing the supermolecule precursor with the graphite oxide solution uniformly dispersed by ultrasonic, and oscillating for 4-8 h on a shaking table at the frequency of 5000-;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
fourthly, roasting the solid obtained in the third step for 4 hours at the temperature of 550 +/-10 ℃ to obtain the graphene-modified prismatic carbon nitride;
and fifthly, weighing 20mg of graphene-modified prismatic carbon nitride into a photocatalytic reaction tank, adding 90 mL of deionized water, 10 mL of triethanolamine and 3 wt.% of Pt, and producing hydrogen under visible light.
The graphene-modified prismatic carbon nitride prepared by the method increases the specific surface area, exposes more active sites, improves the absorption and utilization rate of visible light, and is beneficial to the separation and migration of photon-generated carriers, thereby greatly improving the catalytic activity of hydrogen production by visible light.
Example 1 was carried out:
firstly, dissolving 2 g of melamine in 80 mL of deionized water, heating and stirring at 80 ℃ to dissolve the melamine, pouring the melamine into a 200 mL reaction kettle while the melamine is hot, carrying out a hydrothermal reaction for 48 hours at 180 ℃, and washing and drying the obtained solid to obtain a supramolecular precursor;
secondly, ultrasonically dispersing 5 mg of graphite oxide in 50 mL of deionized water, adding 1g of supramolecular precursor, and oscillating for 4-8 h on a shaking table at the frequency of 5000-6000 r/min;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
fourthly, roasting the freeze-dried solid at 550 +/-10 ℃ for 4 hours to prepare graphene-modified prismatic carbon nitride rGO-pCN (0.5%);
and fifthly, weighing 20mg of graphene-modified prismatic carbon nitride into a photocatalytic reaction tank, adding 90 mL of deionized water, 10 mL of triethanolamine and 3 wt.% of Pt, and producing hydrogen under visible light.
As shown in FIG. 5, the hydrogen is produced under visible light, and the yield reaches 202.5 mu mol h-1。
Example 2 was carried out:
firstly, dissolving 2 g of melamine in 80 mL of deionized water, heating and stirring 80 g of water for dissolving, pouring the solution into a 200 mL reaction kettle while the solution is hot, carrying out hydrothermal reaction for 48 hours at 180 ℃, washing and drying the obtained solid to obtain a supramolecular precursor;
secondly, ultrasonically dispersing 10 mg of graphite oxide in 50 mL of deionized water, adding 1g of supramolecular precursor, and oscillating for 4-8 h on a shaking table at the frequency of 5000-6000 r/min;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
fourthly, roasting the freeze-dried solid at 550 +/-10 ℃ for 4 hours to prepare the graphene-modified prismatic carbon nitride rGO-pCN (1%);
and fifthly, weighing 20mg of graphene-modified prismatic carbon nitride into a photocatalytic reaction tank, adding 90 mL of deionized water, 10 mL of triethanolamine and 3 wt.% of Pt, and producing hydrogen under visible light.
The prepared material is graphene-modified prismatic carbon nitride characterized by a field emission scanning electron microscope, an XRD diffraction spectrum, a Fourier transform infrared spectrum and a nitrogen adsorption/desorption curve, wherein the graphene is of a single-layer structure, wraps the surface of the carbon nitride through covalent bond, and has a large specific surface area, as shown in figures 1-4.
The performance test of photocatalytic hydrogen production is carried out by taking the prepared rGO-pCN (1%) as a visible light catalyst, and the result is shown in figure 5 and is compared with g-C prepared by traditional melamine3N4Compared with the rGO-pCN (1 percent), the rGO-pCN has better performance of hydrogen production by visible light catalysis, and the yield reaches 281.5 mu mol h-1。
Example 3 of implementation:
firstly, dissolving 2 g of melamine in 80 mL of deionized water, heating and stirring 80 g of water for dissolving, pouring the solution into a 200 mL reaction kettle while the solution is hot, carrying out hydrothermal reaction for 48 hours at 180 ℃, washing and drying the obtained solid to obtain a supramolecular precursor;
secondly, ultrasonically dispersing 20mg of graphite oxide in 50 mL of deionized water, adding 1g of supramolecular precursor, and oscillating for 4-8 h on a shaking table at the frequency of 5000-6000 r/min;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
fourthly, roasting the freeze-dried solid at 550 +/-10 ℃ for 4 hours to prepare graphene-modified prismatic carbon nitride rGO-pCN (2%);
and fifthly, weighing 20mg of graphene-modified prismatic carbon nitride into a photocatalytic reaction tank, adding 90 mL of deionized water, 10 mL of triethanolamine and 3 wt.% of Pt, and producing hydrogen under visible light.
As shown in FIG. 5, the hydrogen is produced under visible light, and the yield reaches 233.7 mu mol h-1。
Example 4 of implementation:
firstly, dissolving 2 g of melamine in 80 mL of deionized water, heating and stirring 80 g of water for dissolving, pouring the solution into a 200 mL reaction kettle while the solution is hot, carrying out hydrothermal reaction for 48 hours at 180 ℃, washing and drying the obtained solid to obtain a supramolecular precursor;
secondly, ultrasonically dispersing 40 mg of graphite oxide in 50 mL of deionized water, adding 1g of supramolecular precursor, and oscillating for 4-8 h on a shaking table at the frequency of 5000-6000 r/min;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
fourthly, roasting the freeze-dried solid at 550 +/-10 ℃ for 4 hours to prepare graphene-modified prismatic carbon nitride rGO-pCN (4%);
and fifthly, weighing 20mg of graphene-modified prismatic carbon nitride into a photocatalytic reaction tank, adding 90 mL of deionized water, 10 mL of triethanolamine and 3 wt.% of Pt, and producing hydrogen under visible light.
As shown in FIG. 5, the hydrogen is produced under visible light, and the yield reaches 170.8 mu mol h-1。
Comparative example:
2 g of melamine is roasted for 4 h at 550 +/-10 ℃ to obtain g-C3N4。
As shown in FIG. 5, hydrogen was produced in a yield of 38.6. mu. mol h under visible light-1。
Claims (6)
1. A preparation method of graphene-modified prismatic carbon nitride is characterized by comprising the following steps:
firstly, carrying out hydrothermal treatment on melamine to obtain a supramolecular precursor;
secondly, mixing the supermolecule precursor with the graphite oxide solution uniformly dispersed by ultrasonic, and oscillating uniformly on a shaking table;
thirdly, filtering and washing the precipitate obtained in the second step, and freeze-drying the obtained solid;
and fourthly, roasting the solid obtained in the third step at 550 +/-10 ℃ for 4-6 hours to obtain the graphene-modified prismatic carbon nitride.
2. The method according to claim 1, wherein in the first step, the hydrothermal treatment temperature is 180 ± 20 ℃ and the hydrothermal treatment time is 24-48 h.
3. The method according to claim 1, wherein in the second step, the mass ratio of the supramolecular precursor to the graphite oxide is 96-99.5: 0.5-4.
4. Graphene-modified prismatic carbon nitride prepared according to the method of any one of claims 1 to 3.
5. The graphene-modified prismatic carbon nitride according to claim 4, wherein the number of graphene layers in the graphene-modified prismatic carbon nitride is 1, and graphene and the prismatic carbon nitride are complexed by covalent bonding.
6. Use of graphene-modified prismatic carbon nitride prepared according to any one of claims 1 to 3 as a catalyst in photocatalytic hydrogen production.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103985875A (en) * | 2014-05-21 | 2014-08-13 | 南京理工大学 | Application of graphene-carbon nitride composite material |
| CN104437589A (en) * | 2014-11-07 | 2015-03-25 | 江苏大学 | Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof |
| CN108126729A (en) * | 2018-01-10 | 2018-06-08 | 南京工程学院 | One type graphene carbonitride base composite photocatalyst and preparation method thereof |
| CN108786892A (en) * | 2018-06-26 | 2018-11-13 | 江苏师范大学 | A kind of graphite oxide phase single layer C3N4Composite film material and its preparation method and application |
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- 2018-12-19 CN CN201811555592.8A patent/CN111330611A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103985875A (en) * | 2014-05-21 | 2014-08-13 | 南京理工大学 | Application of graphene-carbon nitride composite material |
| CN104437589A (en) * | 2014-11-07 | 2015-03-25 | 江苏大学 | Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof |
| CN108126729A (en) * | 2018-01-10 | 2018-06-08 | 南京工程学院 | One type graphene carbonitride base composite photocatalyst and preparation method thereof |
| CN108786892A (en) * | 2018-06-26 | 2018-11-13 | 江苏师范大学 | A kind of graphite oxide phase single layer C3N4Composite film material and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| CHAO ZHOU ET AL.: "Template-free large-scale synthesis of g-C3N4 microtubes for enhanced visible light-driven photocatalytic H2 production", 《NANO RESEARCH》 * |
| YUANZHI HONG ET AL.: "Rational synthesis of ultrathin graphitic carbon nitride nanosheets for efficient photocatalytic hydrogen evolution", 《CARBON》 * |
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