CN115608402B - Crystalline phase carbon nitride photocatalyst with ordered-distorted interface - Google Patents
Crystalline phase carbon nitride photocatalyst with ordered-distorted interface Download PDFInfo
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- CN115608402B CN115608402B CN202211337344.2A CN202211337344A CN115608402B CN 115608402 B CN115608402 B CN 115608402B CN 202211337344 A CN202211337344 A CN 202211337344A CN 115608402 B CN115608402 B CN 115608402B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 54
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 47
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 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
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- OWYWGLHRNBIFJP-UHFFFAOYSA-N Ipazine Chemical compound CCN(CC)C1=NC(Cl)=NC(NC(C)C)=N1 OWYWGLHRNBIFJP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000031700 light absorption Effects 0.000 abstract description 5
- 239000002243 precursor Substances 0.000 abstract description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000002256 photodeposition Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 1
- 229940116357 potassium thiocyanate Drugs 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 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
Classifications
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a crystalline phase carbon nitride photocatalyst with an ordered-twisted interface, and a preparation method and application thereof, and belongs to the technical field of photocatalytic material preparation. The method is characterized in that cyanuric chloride and sodium thiocyanate are used as precursors, and a carbon nitride photocatalyst with a heptazine ordered-twist interface is synthesized in a high-temperature molten salt environment. The invention has simple process and low cost, meets the actual production requirement, and the prepared photocatalyst has good light absorption performance and hydrogen production activity at a long wavelength, and has higher application potential under the condition that platinum is used as a promoter and triethanolamine is used as a sacrificial agent, wherein the photocatalytic hydrogen production activity is obviously superior to that of single crystal phase carbon nitride.
Description
Technical Field
The invention belongs to the technical field of preparation of photocatalytic materials, and particularly relates to a crystalline phase carbon nitride photocatalyst with an ordered-twisted interface, and a preparation method and application thereof.
Background
The energy and environmental problems associated with the massive use of fossil energy in human society have become increasingly prominent. On the one hand, the reserves of these fossil energy sources such as oil and gas are limited, on the other hand, the exploitation and extraction of fossil energy sources causes serious environmental pollution, and the large-scale use of fossil energy sources also causes an increase in carbon emissions. Therefore, the development and utilization of clean sustainable new energy is a future trend of human society. Hydrogen is taken as a novel energy source, and is regarded as an ideal alternative energy source due to the advantages of high energy density, cleanness, environmental protection and the like. However, hydrogen is mainly produced by cracking fossil fuel and electrolyzing water at present, and the production procedures of the methods are complex and the cost is high. The photocatalysis hydrogen production technology for converting solar energy into hydrogen energy has the advantages of simple process, economy, environmental protection and the like, and is considered as one of ideal ways for preparing hydrogen energy in the future. The core of this technology is the development of efficient photocatalysts.
Currently, most of the widely used photocatalysts are metal-inorganic semiconductor photocatalysts. Although such photocatalysts exhibit good photocatalytic performance, the presence of metals or even noble metals in the structure results in high costs and complex synthesis steps, which limit large-scale use. In recent years, organic polymer photocatalysts, particularly graphite phase carbon nitride materials, have attracted considerable interest to researchers due to their advantages of simple synthesis, economy, environmental protection, and the like. However, despite their great development in photolysis of water, reduction of carbon dioxide, organic photosynthesis, etc., they still only use short wavelength visible light (less than 450 nm). Therefore, the development of a carbon nitride photocatalyst which is easy to prepare, economical and environment-friendly and has long-wavelength visible light absorption has extremely important significance.
Disclosure of Invention
The invention aims to provide a crystalline phase carbon nitride photocatalyst with an ordered-twisted interface, a preparation method and application thereof, and the prepared carbon nitride photocatalyst has good long-wavelength sunlight utilization rate and can realize efficient photocatalytic decomposition of water to produce hydrogen.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a crystalline phase carbon nitride photocatalyst with an ordered-twisted interface is synthesized in a high-temperature condition by taking cyanuric chloride and sodium thiocyanate as precursors and sodium chloride as a co-molten salt and lithium chloride as an additional salt, and has a heptazine ordered-twisted interface, a micro-morphology of a nano rod and an optical absorption wavelength of 300-700 nm. The ordered structure and the twisted structure in the photocatalyst form a good contact interface, so that the light absorption performance of the material is improved, the separation of photo-generated charges is promoted, and the efficient long-wavelength visible light can be realized for preparing hydrogen by driving water decomposition.
The preparation method of the crystalline phase carbon nitride photocatalyst with the ordered-distorted interface comprises the following steps:
(1) Uniformly grinding and mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a glove box with inert gas protection according to the mass ratio of 185:243:327;
(2) And (3) calcining the mixture obtained in the step (1) at 500-650 ℃ for 4 hours in a nitrogen atmosphere to obtain the crystalline phase carbon nitride photocatalyst.
The crystalline phase carbon nitride photocatalyst with the ordered-twisted interface can be used for preparing hydrogen by catalyzing and decomposing water under long-wavelength visible light, and particularly, when the crystalline phase carbon nitride photocatalyst is used, platinum is used as a cocatalyst, triethanolamine is used as a sacrificial agent, and the hydrogen is generated by photolysis under the illumination condition of 450-700nm of wavelength.
The invention has the remarkable advantages that:
(1) The invention firstly utilizes the precursor cyanuric chloride and sodium thiocyanate to polymerize to form a distorted carbon nitride structure, and in the polymerization process, the precursor cyanuric chloride and sodium thiocyanate can react to form sodium chloride, and the sodium chloride and lithium chloride can form a eutectic salt system with higher eutectic point, and the distorted structure can be converted into an ordered structure by combining with the regulation and control of calcination temperature, so that an ordered-distorted interface is finally formed.
(2) The photocatalyst synthesized by the invention contains ordered and distorted carbon nitride structures, and good contact between the ordered and distorted carbon nitride structures not only improves the light absorption performance of the material, but also promotes the separation of photo-generated charges, thereby realizing efficient long-wavelength visible light driving water decomposition to prepare hydrogen.
(3) The whole preparation process is simple and easy to control, has low energy consumption and cost, meets the actual production requirement, and is beneficial to large-scale popularization.
Drawings
FIG. 1 is a powder X-ray diffraction chart of the carbon nitride photocatalyst obtained in examples 1 to 4.
Fig. 2 is a fourier transform infrared spectrum of the carbon nitride photocatalyst obtained in example 3.
FIG. 3 is a high resolution transmission electron microscope image of the carbon nitride photocatalyst obtained in example 3.
FIG. 4 is a graph showing the diffuse reflectance of ultraviolet-visible light of the carbon nitride photocatalyst obtained in example 3.
FIG. 5 is a graph showing steady-state fluorescence spectra of carbon nitride photocatalysts obtained in examples 1 to 4 and comparative examples.
FIG. 6 is a graph showing the comparative activities of photocatalytic-decomposed water to hydrogen for the carbon nitride photocatalysts obtained in examples 1 to 4 and comparative examples.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
(1) Grinding and uniformly mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a mass ratio of 185:243:327 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 500 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the crystalline phase carbon nitride photocatalyst.
Example 2
(1) Grinding and uniformly mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a mass ratio of 185:243:327 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 550 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the crystalline phase carbon nitride photocatalyst.
Example 3
(1) Grinding and uniformly mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a mass ratio of 185:243:327 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 600 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the crystalline phase carbon nitride photocatalyst.
Example 4
(1) Grinding and uniformly mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a mass ratio of 185:243:327 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 650 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the crystalline phase carbon nitride photocatalyst.
Comparative example
(1) Grinding and uniformly mixing cyanuric chloride, potassium thiocyanate and lithium chloride in a mass ratio of 185:292:183 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 550 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the carbon nitride photocatalyst with an unoptimized structure.
FIG. 1 is a powder X-ray diffraction chart of the carbon nitride photocatalyst obtained in examples 1 to 4. As can be seen from the figure, the carbon nitride photocatalyst prepared in example 1 has a distorted structure, while the carbon nitride photocatalysts prepared in examples 2, 3 and 4 have both heptazine ordered and distorted carbon nitride structures, wherein diffraction peaks at 8 ° and 14 ° are attributed to heptazine-based crystalline phase carbon nitride, and a broad peak at 27 ° is attributed to distorted heptazine-based matrix phase carbon nitride. The method of the invention can form a distorted carbon nitride structure firstly, and then regulate and control the conversion of the distorted structure to an ordered structure by using the calcination temperature to form an ordered-distorted interface. However, the structure of the photocatalyst prepared in example 4 is different from that of examples 2 and 3, which means that too high a calcination temperature will result in a change in the catalyst structure.
Fig. 2 is a fourier infrared spectrum of the carbon nitride photocatalyst obtained in example 3. From the figure, it can be found that the prepared carbon nitride photocatalyst is a heptazine carbon nitride photocatalyst. Wherein, is greater than 3000 cm -1 The absorbance peak of wavenumber represents amino or hydroxyl groups in the sample structure, at 2170 cm -1 The absorption peak of wave number represents cyano group in the structure, and the remaining absorption peakThe characteristic infrared absorption peak of the heptazinyl carbon nitride material is mainly.
FIG. 3 is a high resolution transmission electron microscope image of the carbon nitride photocatalyst obtained in example 3. The figure further shows that ordered-twisted structures are present in the photocatalyst and that the two structures form a good contact.
FIG. 4 is a graph showing the diffuse reflectance of ultraviolet-visible light of the carbon nitride photocatalyst obtained in example 3. It can be seen from the figure that the photocatalyst has good long wavelength visible light absorption. Wherein the absorption edge at 450nm represents an ordered (crystalline phase) structure, and the absorption at 450-700nm is attributed to a twisted structure.
FIG. 5 is a graph showing steady-state fluorescence spectra of the carbon nitride photocatalysts obtained in examples 1-4 and comparative examples. As can be seen from the figures, the carbon nitride photocatalysts prepared in examples 2 and 3 exhibited lower steady-state fluorescence intensities than those of example 1 (twisted structure) and comparative example, which demonstrated that the order-twisted interface effectively improved the photocarrier separation efficiency of the photocatalysts. Whereas the photocatalyst prepared in example 4 had a higher steady state fluorescence intensity, which may be caused by a structural change due to an excessively high calcination temperature.
The hydrogen-generating activity was that 50 mg of a photocatalyst was used and 100 ml of an aqueous solution containing 10% by volume of triethanolamine, 3% by mass of Pt (H) 2 PtCl 6 Pt in situ photo-deposition) as a cocatalyst, in a reactor with a 300 watt xenon lamp (using a 450nm cut-off piece to control the incident light wavelength to be greater than 450 nm) at the top.
FIG. 6 is a graph showing the activities of photocatalytic decomposition of water into hydrogen for the carbon nitride photocatalysts obtained in examples 1 to 4 and comparative examples. From the figures, it can be seen that the photocatalysts prepared in examples 2 and 3 have higher long wavelength visible light hydrogen production activity. The hydrogen production rate of the photocatalyst prepared in the embodiment 3 reaches 80 mu mol/h, which is higher than that of the photocatalysts prepared in other embodiments and comparative examples.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. A preparation method of a crystalline phase carbon nitride photocatalyst with an ordered-distorted interface is characterized by comprising the following steps: the method comprises the following steps:
(1) Grinding and uniformly mixing cyanuric chloride, sodium thiocyanate and lithium chloride in a mass ratio of 185:243:327 in a glove box with inert gas protection;
(2) Calcining the mixture obtained in the step (1) for 4 hours at 600 ℃ in nitrogen atmosphere, cooling, washing with water to remove molten salt, and drying to obtain the crystalline phase carbon nitride photocatalyst.
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| CN104399509A (en) * | 2014-12-08 | 2015-03-11 | 福州大学 | Hydrogen-free precursor synthesized carbon nitride photocatalyst |
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| CN110124719A (en) * | 2019-05-21 | 2019-08-16 | 电子科技大学 | A kind of preparation method and application of highly crystalline carbonitride catalysis material |
| CN114289063A (en) * | 2022-01-18 | 2022-04-08 | 东北大学 | Carbon quantum dot and high-crystallinity polyheptazine imide compound and preparation method thereof |
| CN114377711A (en) * | 2021-12-16 | 2022-04-22 | 中国科学院金属研究所 | Simple preparation method and application of high-crystallinity graphite carbon nitride |
| CN114920219A (en) * | 2022-05-31 | 2022-08-19 | 西安交通大学 | Preparation method and application of spherical crystalline carbon nitride with heptazine ring structure |
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2022
- 2022-10-28 CN CN202211337344.2A patent/CN115608402B/en active Active
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