CN116212926A - Preparation method and application of brown carbon nitride photocatalyst - Google Patents
Preparation method and application of brown carbon nitride photocatalyst Download PDFInfo
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- CN116212926A CN116212926A CN202310147159.5A CN202310147159A CN116212926A CN 116212926 A CN116212926 A CN 116212926A CN 202310147159 A CN202310147159 A CN 202310147159A CN 116212926 A CN116212926 A CN 116212926A
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 10
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 3
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- 238000004519 manufacturing process Methods 0.000 claims 4
- 238000006243 chemical reaction Methods 0.000 abstract description 6
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- 239000000203 mixture Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
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- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography 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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- 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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
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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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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Abstract
The invention discloses a preparation method and application of a brown carbon nitride photocatalyst, belonging to the technical field of preparation of photocatalytic materials, and comprising the following steps of: mixing glycollic acid and urea, placing the mixture into an oil bath pot for stirring to obtain a target solution, pouring the target solution into a crucible, transferring the crucible into a muffle furnace for heating, and cooling to room temperature to obtain brown carbon nitride; grinding the obtained brown carbon nitride into powder in a mortar, and sieving for a plurality of times to obtain a brown carbon nitride photocatalytic material; the brown carbon nitride photocatalyst prepared by the scheme has wider photoresponse range, the structure provides large surface area, more active sites are exposed, and CO is better absorbed 2 At the same time can effectively inhibit photo-generated carriersFor photocatalytic CO 2 The reduction shows excellent photocatalytic activity, the scheme is environment-friendly, the used raw materials are low-cost and easy-to-obtain products, the treatment time is short, the reaction is mild, the energy consumption is low, and the method has very high application prospect and use value.
Description
Technical Field
The invention relates to a preparation method and application of a brown carbon nitride photocatalyst, and belongs to the technical field of preparation of photocatalytic materials.
Background
The current society develops rapidly, and the energy demand is greatly improved. The energy source is mainly derived from the combustion of non-renewable fossil fuels, so that the energy crisis is highlighted. Fossil fuel combustion, on the other hand, releases large amounts of CO 2 And brings great threat to our environment. Accordingly, various countries are also working on developing new energy technologies in order to meet the increasing energy demands of humans and to reduce environmental pollution. Wherein CO is generated by utilizing inexhaustible solar energy 2 Conversion to fuel is one of the most promising technologies, thus photocatalytic CO 2 Reduction is increasingly attracting attention from researchers. The key point of the technical development is to adopt a reasonable and novel design concept, and from different angles, the composition, morphology, structure, specific surface area and the like of the catalytic material are regulated, so that the catalytic efficiency of the traditional photocatalyst is improved and improved on the aspect of inheriting the existing performance of the traditional photocatalyst, and the efficient catalysis and high-selectivity conversion are achieved. Carbon nitride (g-C) 3 N 4 ) As a photocatalyst with a certain visible light response in organic pollutant degradation and CO 2 The reduction and other aspects are widely studied and applied. But due to the limited active sites of the traditional carbon nitride catalyst, the catalyst is combined with CO 2 The affinity between the two is weaker, and the carrier mobility is low, so that the photocatalysis efficiency is influenced. Therefore, it is necessary to design a suitable energy band structure, a suitable electronic structure, and a large specific surface area and light absorption range to enhance CO absorption 2 Capability, selectivity, and catalytic efficiency.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method and application of a brown carbon nitride photocatalyst.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a method for preparing a brown carbon nitride photocatalyst, which comprises the following steps:
step (1): weighing glycolic acid and urea into a beaker, and placing the beaker into an oil bath pot for stirring to obtain a target solution;
step (2): pouring the target solution obtained in the step (1) into a crucible, transferring into a muffle furnace, heating and calcining, and naturally cooling to room temperature to obtain brown carbon nitride;
step (3): grinding the obtained brown carbon nitride into powder in a mortar, and sieving to obtain the brown carbon nitride photocatalytic material.
Preferably, in the step (1), the glycollic acid and urea are both chemically pure, and the mass of the glycollic acid is 0.03g-0.07g; the mass of the urea is 8g-10g.
Preferably, in the step (1), the mass of the glycolic acid is 0.03g, and the mass of the urea is 10g.
Preferably, in the step (1), the mass of the glycollic acid is 0.05g, and the mass of the urea is 10g.
Preferably, in the step (1), the mass of the glycolic acid is 0.07g, and the mass of the urea is 10g.
Preferably, in the step (1), the temperature of the oil bath is 80 ℃, and the stirring time is 5-10min.
Preferably, in the step (2), the temperature rising speed is 2-4 ℃/min, the calcining temperature is 600 ℃, and the calcining temperature holding time is 1h.
Preferably, the temperature rise rate is 3 ℃/min.
Preferably, in step (2), the number of sieves screened is 100 mesh.
Brown carbon nitride photocatalyst obtained by preparation method of brown carbon nitride photocatalyst is used for photocatalytic CO 2 Application in reduction.
The invention has the following beneficial effects: (1) The brown carbon nitride photocatalyst prepared by the invention has wider photoresponse range, the structure provides large surface area, more active sites are exposed, and CO is better absorbed 2 At the same time, can effectively inhibit the recombination of photon-generated carriers, and is used for photocatalysis of CO 2 Reduction shows excellent photocatalytic activity.
(2) The brown carbon nitride photocatalytic material prepared by the invention has good photocatalytic performance and photoelectric performance, and can efficiently reduce CO 2 The selectivity is high. In the preparation method provided by the invention, the raw materials are easy to obtain, the process is simple, the reaction is mild, the energy consumption is low, and the solvent raw materials can be recycled in industry, so that the whole synthesis process is green and environment-friendly, the product cost is effectively reduced, and the preparation method has a very high application prospect and use value.
Drawings
FIG. 1 is a TEM spectrum of GACN-2.
FIG. 2 is a block g-C 3 N 4 XRD patterns with GACN-1, GACN-2, GACN-3 brown carbon nitride materials.
FIG. 3 is a block g-C 3 N 4 And the EPR spectrum of GACN-2.
FIG. 4 is a block g-C 3 N 4 And a diffuse ultraviolet-visible reflectance spectrum of a brown carbon nitride material.
FIG. 5 is a GACN-2 photocatalytic CO 2 XRD contrast patterns before and after reduction.
Description of the embodiments
The invention is further illustrated by the following examples, which are not intended to be limiting.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
Mixing 0.03g of glycolic acid and 10g of urea into a beaker, placing the beaker into an oil bath pot at 80 ℃ and stirring for 5 min by using a glass rod, dissolving to obtain a target solution, pouring the target solution into a crucible, transferring the crucible into a muffle furnace, heating to 600 ℃ at a heating rate of 3 ℃/min, keeping the temperature for 1h, naturally cooling to room temperature to obtain brown carbon nitride, grinding the brown carbon nitride into powder by using a mortar, sieving the powder by using a 100-mesh screen for multiple times, and obtaining the brown carbon nitride photocatalytic material after the treatment is finished, namely GACN-1.
Example 2
Mixing 0.05g of glycolic acid and 10g of urea into a beaker, placing the beaker into an oil bath pot at 80 ℃ and stirring the mixture for 5 min by using a glass rod, obtaining a target solution after dissolution, pouring the target solution into a crucible, transferring the crucible into a muffle furnace, heating the crucible to 600 ℃ at a heating rate of 3 ℃/min, keeping the crucible for 1h, naturally cooling the crucible to room temperature to obtain brown carbon nitride, grinding the brown carbon nitride into powder by using a mortar, sieving the powder by using a 100-mesh screen for multiple times, and obtaining the brown carbon nitride photocatalytic material after the treatment is finished, namely GACN-2.
Example 3
Mixing 0.07g of glycolic acid and 10g of urea into a beaker, placing the beaker into an oil bath pot at 80 ℃ and stirring the mixture for 5 min by using a glass rod, obtaining a target solution after dissolution, pouring the target solution into a crucible, transferring the crucible into a muffle furnace, heating the crucible to 600 ℃ at a heating rate of 3 ℃/min, keeping the crucible for 1h, naturally cooling the crucible to room temperature to obtain brown carbon nitride, grinding the brown carbon nitride into powder by using a mortar, sieving the powder by using a 100-mesh screen for multiple times, and obtaining the brown carbon nitride photocatalytic material after the treatment is finished, namely GACN-3.
The morphology and size of the prepared GACN-2 were observed using a dual calibration Tecnai G2F 30S-Tain FEI transmission electron microscope with a cold field emitter. FIG. 1 is a transmission electron microscope image of GACN-2, which is clearly observed to be thin flocculent and have a plurality of small pore morphology.
Prepared for photocatalytic CO 2 The structural test of the reduced brown carbon nitride photocatalytic material was carried out on a ray diffractometer (XRD) type Bruker D8, germany (Cu-ka radiation, λ=1.5418 a, range 10 ° -80 °), scanning rate 7 ° min -1 . As shown in FIG. 2, the block g-C 3 N 4 There was no major structural difference from the treated GACN-2 brown carbon nitride material.
FIG. 3 is a block g-C 3 N 4 With the EPR profile of the treated brown carbon nitride material we can see that GACN-2 has a stronger oxygen defect signal than Bulk CN.
FIG. 4 is a block g-C 3 N 4 With the ultraviolet visible diffuse reflection spectrum of the treated brown carbon nitride material, we can see that the brown carbon nitride material is compared with the blocky g-C 3 N 4 Has better light absorption performance in the visible light region and the near infrared light region.
10mg of brown carbon nitride photocatalyst was weighed out and dissolved in the prepared solution (6 mL acetonitrile, 4 mL H) by 3 min ultrasound 2 O,2 mL TEOA), the reaction was carried out under irradiation at a temperature of 10℃under a 300W xenon lamp. Gas product analysis was performed using a gas chromatography system (GC 9720, ar carrier) manufactured by religion gold sources limited in beijing.
For photocatalytic CO prepared for investigation 2 Stability of reduced brown carbon nitride photocatalyst we compared the XRD patterns of the GACN-2 catalyst before and after the reaction, as shown in figure 5, without significant changes to the catalyst itself.
The foregoing has outlined and described the basic principles, features, and advantages of the present invention. However, the foregoing is merely specific examples of the present invention, and the technical features of the present invention are not limited thereto, and any other embodiments that are derived by those skilled in the art without departing from the technical solution of the present invention are included in the scope of the present invention.
Claims (10)
1. A method for preparing a brown carbon nitride photocatalyst, which is characterized by comprising the following steps:
step (1): weighing glycolic acid and urea into a beaker, and placing the beaker into an oil bath pot for stirring to obtain a target solution;
step (2): pouring the target solution obtained in the step (1) into a crucible, transferring into a muffle furnace, heating and calcining, and naturally cooling to room temperature to obtain brown carbon nitride;
step (3): grinding the obtained brown carbon nitride into powder in a mortar, and sieving to obtain the brown carbon nitride photocatalytic material.
2. The method for producing a brown carbon nitride photocatalyst according to claim 1, wherein in step (1), both glycolic acid and urea are chemically pure, and the mass of glycolic acid is 0.03g to 0.07g; the mass of the urea is 8g-10g.
3. The method for producing a brown carbon nitride photocatalyst according to claim 1, wherein in step (1), the mass of the glycolic acid is 0.03g and the mass of the urea is 10g.
4. The method for producing a brown carbon nitride photocatalyst according to claim 1, wherein in step (1), the mass of the glycolic acid is 0.05g and the mass of the urea is 10g.
5. The method for producing a brown carbon nitride photocatalyst according to claim 1, wherein in step (1), the mass of the glycolic acid is 0.07g and the mass of the urea is 10g.
6. The method for preparing a brown carbon nitride photocatalyst according to claim 1, wherein in the step (1), the temperature of the oil bath is 80 ℃ and the stirring time is 5-10min.
7. The method for preparing a brown carbon nitride photocatalyst according to claim 1, wherein in the step (2), the temperature rising rate is 2-4 ℃/min, the calcination temperature is 600 ℃, and the calcination temperature holding time is 1h.
8. The method for preparing a brown carbon nitride photocatalyst according to claim 7, wherein the temperature rising rate is 3 ℃/min.
9. The method for preparing a brown carbon nitride photocatalyst according to claim 1, wherein in the step (2), the number of the sieved mesh is 100.
10. The brown carbon nitride photocatalyst obtained by the method for preparing a brown carbon nitride photocatalyst according to any one of claims 1 to 9, wherein the brown carbon nitride photocatalyst is used for photocatalytic CO 2 Application in reduction.
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| CN116351451A (en) * | 2023-03-22 | 2023-06-30 | 扬州大学 | Preparation method and application of full-spectrum response carbon nitride photocatalyst |
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