CN115518666A - Preparation method and application of ammonium formate modified coral-shaped wide-spectral-response carbon-nitrogen polymer photocatalyst - Google Patents
Preparation method and application of ammonium formate modified coral-shaped wide-spectral-response carbon-nitrogen polymer photocatalyst Download PDFInfo
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- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229920000642 polymer Polymers 0.000 title claims abstract description 28
- 230000004044 response Effects 0.000 title claims abstract description 28
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 239000002861 polymer material Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 230000001699 photocatalysis Effects 0.000 claims abstract description 16
- 230000003595 spectral effect Effects 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims description 22
- 238000006722 reduction reaction Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 238000007146 photocatalysis Methods 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 230000009467 reduction Effects 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 230000031700 light absorption Effects 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 230000005684 electric field Effects 0.000 abstract description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 36
- 229910002092 carbon dioxide Inorganic materials 0.000 description 18
- 239000001569 carbon dioxide Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052755 nonmetal Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- CGYGETOMCSJHJU-UHFFFAOYSA-N 2-chloronaphthalene Chemical compound C1=CC=CC2=CC(Cl)=CC=C21 CGYGETOMCSJHJU-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B01J35/39—
-
- 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
- B01D53/74—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
Abstract
The invention belongs to the technical field of preparation of photocatalytic materials, and discloses a preparation method of an ammonium formate modified coralliform wide spectral response carbon nitrogen polymer photocatalyst and photocatalytic CO 2 The use of reduction. According to the invention, ammonium formate and urea are mixed by a stirring and grinding method and transferred to a crucible, and then a tin foil paper is used for sealing and covering a cover to ensure the sealing property. And (3) placing the crucible in a muffle furnace, and calcining for a period of time to obtain the oxygen-doped orange carbon nitrogen polymer material. The carbon-nitrogen polymer photocatalyst prepared by the method realizes the widening of the photoresponse range and improves the light absorption capacity of the material. On the other hand, oxygen is completedThe nitrogen position doping of the elements not only accurately regulates and controls the energy band position, but also constructs a strong built-in electric field and provides strong pushing power for the efficient transmission of electrons.
Description
Technical Field
The invention relates to a preparation method and application of an ammonium formate modified coral-shaped wide spectral response carbon-nitrogen polymer photocatalyst, belonging to the technical field of preparation of photocatalytic materials.
Background
Consumption of fossil fuels leads to atmospheric carbon dioxide (CO) 2 ) The increase in concentration has a serious influence on the environment. Use of semiconductor photocatalysis technology to remove excess CO from environment 2 The reduction preparation of high value-added carbon-based chemicals is one of the effective strategies. However, CO 2 The high bond energy of the C = O bond in the molecule makes it thermodynamically stable, requiring a very high activation energy to break it. In this context, natural solar energy is used as an energy source to drive CO 2 Producing fuels has attracted the interest of a large number of researchers. The key of the technology lies in the design and development of high-efficiency catalysts.
In the past decades, semiconductor photocatalysts have attracted extensive attention because of their excellent performance, and have broad application prospects in environmental pollution control and the effective conversion of sunlight into renewable energy. However, most of the reported metal semiconductor materials are only active in the ultraviolet region, which accounts for about 5% of the solar spectrum, and many studies are being conducted to find a photocatalyst capable of extending the absorption wavelength of the photocatalyst in order to improve the utilization rate of solar energy. The non-metal semiconductor is low in cost and environment-friendly, and can expand light absorption to a visible light region so as to improve photocatalytic CO 2 Performance of reduction. At present, the carbon-nitrogen polymer is limited in photocatalysis of CO to a certain extent due to the defects of low-efficiency solar energy utilization, easy recombination of photogenerated electrons and holes, weak light absorption and the like 2 And (4) practical application of reduction.
Therefore, the carbon-nitrogen polymer modified by the modified carbon-nitrogen polymer has wide spectral response to improve the photocatalytic CO 2 The reduction performance is generally modified by noble metal deposition, defect engineering,Doping elements, constructing a heterojunction and the like. While non-metal doping in element doping is considered to be one of the most effective strategies for improving the band gap of the carbon-nitrogen polymer. However, the problems of difficult directional doping, unclear doping mechanism, complex doping method and the like still exist in the prior nonmetal doping. The invention provides a simple one-step doping strategy, oxygen is successfully doped at a nitrogen site, the positions of a conduction band and a valence band are adjusted to inhibit the recombination of photogenerated electrons and holes, and the morphology of a carbon-nitrogen polymer is changed to realize photocatalysis of CO 2 The reduction occurs to provide more reaction sites, and simultaneously, the photoresponse range of the carbon-nitrogen polymer is expanded to promote light absorption.
Disclosure of Invention
The invention aims to provide a preparation method of an ammonium formate modified coral-shaped wide spectral response carbon-nitrogen polymer photocatalyst. The method successfully dopes non-metallic oxygen into nitrogen sites of the carbon-nitrogen polymer by a simple one-step high-temperature calcination technology. For photocatalytic CO 2 The reduction reaction process has the defects of few reactive active sites, easy recombination of photogenerated electrons and holes, low utilization rate of visible light and the like, the energy band structure is adjusted by introducing non-metallic element oxygen, a built-in electric field is constructed to adjust the carrier transmission behavior, the light absorption is expanded, and meanwhile, the coralliform carbon nitrogen polymer is successfully constructed, so that the density of the active sites and the CO are effectively improved 2 The adsorption capacity is finally improved to catalyze CO 2 Activity of reduction.
The specific technical scheme of the invention is as follows:
a preparation method of an ammonium formate modified coral-shaped wide spectral response carbon nitrogen polymer photocatalyst comprises the following steps:
(1) Putting urea and ammonium formate in proportion into an agate mortar, stirring and grinding for a certain time to uniformly mix the urea and the ammonium formate;
(2) Transferring the mixture to a ceramic crucible, and drying the ceramic crucible in a vacuum drying oven at a certain temperature for a period of time;
(3) Wrapping and sealing a crucible containing a dried sample by using tinfoil paper, covering a ceramic cover, putting the crucible into a muffle furnace, heating to a certain temperature at a certain heating rate, calcining for a certain time, cooling to room temperature, and grinding for a certain time to obtain an orange oxygen-doped carbon nitrogen polymer material (O-PCN), namely an ammonium formate-modified coral-shaped wide-spectrum response carbon nitrogen polymer photocatalyst.
Further, in the step (1), the mass ratio of urea to ammonium formate is 9-11g:0.05-0.5g.
Further, in the step (1), the grinding time is 5-15min.
Further, in the step (2), the temperature of the vacuum drying oven is 30-50 ℃, and the drying time is 30-60min.
Further, in the step (3), the temperature rise rate of the muffle furnace is 2-5 ℃/min, the calcining temperature is 500-600 ℃, and the calcining time is 50-80min.
Further, in the step (3), the grinding time is 10-15min.
By contrast, without the addition of ammonium formate, the product is a carbon nitrogen polymer material PCN.
The coral-shaped wide-spectral-response carbon-nitrogen polymer photocatalyst modified by ammonium formate prepared by the invention is used for photocatalysis of CO 2 Use of a reduction reaction.
The invention has the following advantages:
1. by adding ammonium formate, the doping of oxygen element is realized, thereby changing the appearance of carbon-nitrogen polymer, and constructing coralliform structure into photocatalytic CO 2 The reduction reaction occurs to provide more reaction sites;
2. through the polymerization reaction of ammonium formate and a urea intermediate, an orange carbon nitrogen polymer with wide spectral response is successfully synthesized, the energy band structure is adjusted, and the light capture capacity is enhanced;
3. the addition of ammonium formate realizes the formation of C-O bonds, narrows the band gap and maintains the non-metallic property of the carbon-nitrogen polymer.
Drawings
FIG. 1 is an XRD pattern of an ammonium formate-modified coral-like broad spectral response carbon nitrogen polymer material prepared in accordance with the present invention;
FIG. 2 is an SEM image of an ammonium formate modified coral-like broad spectral response carbon nitrogen polymer material prepared by the present invention;
FIG. 3 shows the preparation of the inventionCoral-shaped wide-spectral-response carbon-nitrogen polymer material with added ammonium formate and photocatalytic CO of monomer PCN 2 Reduction activity diagram.
FIG. 4 is a DRS diagram of a coral-like broad spectral response carbon nitrogen polymer material prepared by the present invention;
FIG. 5 shows a coral-shaped wide-spectral-response carbon-nitrogen polymer material prepared by the method 13 A CNMR map.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
Comparative example 1:
weighing 9g of urea, placing the urea in an agate mortar, stirring and grinding for 5min to uniformly mix the urea and the agate mortar, transferring the mixture to a ceramic crucible, placing the ceramic crucible into a vacuum drying oven, drying the ceramic crucible at 30 ℃ for 30min, wrapping the crucible with a dried sample with tinfoil paper, sealing the crucible, covering a ceramic cover, placing the crucible into a muffle furnace, heating to 500 ℃ at the heating rate of 2 ℃/min, calcining for 50min, cooling to room temperature, and grinding for 10min to obtain a white carbon nitrogen polymer material (PCN).
Example 1:
the structuring and broad spectral response of the coralline carbonitride polymer was achieved by adding ammonium formate and varying the milling and drying times compared to comparative example 1.
Weighing 9g of urea, adding 0.1g of ammonium formate, placing the urea and the ammonium formate into an agate mortar, stirring and grinding for 10min to uniformly mix the urea and the ammonium formate, transferring the mixture to a ceramic crucible, placing the ceramic crucible into a vacuum drying oven, drying the ceramic crucible at 30 ℃ for 50min, wrapping the crucible with dried samples with tinfoil paper, sealing the crucible, covering a ceramic cover, placing the crucible into a muffle furnace, heating the crucible to 500 ℃ at the heating rate of 2 ℃/min, calcining the crucible for 50min, cooling the crucible to room temperature, and grinding for 10min to obtain an orange coral-shaped carbon-nitrogen polymer material (0.1O-PCN)
Example 1 has better photocatalytic CO than comparative example 1 2 The reduction performance is mainly caused by the fact that nonmetal oxygen is introduced into the ammonium formate, the energy band position is regulated and controlled, and light absorption is expanded. As shown in fig. 3.
Example 2:
compared with the example 1, the structuring and the wide spectral response of the coral-shaped carbon-nitrogen polymer are realized by increasing the mass of ammonium formate and changing the temperature rise rate and the calcination time.
Weighing 9g of urea, adding 0.25g of ammonium formate, placing the urea and the ammonium formate into an agate mortar, stirring and grinding for 5min to uniformly mix the urea and the ammonium formate, transferring the mixture to a ceramic crucible, placing the ceramic crucible into a vacuum drying oven, drying the ceramic crucible at 30 ℃ for 30min, wrapping the crucible with a dried sample by using tinfoil paper, sealing the crucible, covering a ceramic cover, placing the crucible into a muffle furnace, heating the crucible to 500 ℃ at the heating rate of 5 ℃/min, calcining the crucible for 80min, cooling the crucible to room temperature, and grinding for 10min to obtain an orange coral-shaped carbon-nitrogen polymer material (0.25O-PCN)
Example 2 has better photocatalytic CO than example 1 2 The reduction performance is mainly due to the fact that the increase of the mass of ammonium formate realizes the increase of the oxygen doping amount. As shown in fig. 3.
The 0.25O-PCN prepared in the example was compared with the PCN of the comparative example in terms of the relevant properties;
FIG. 1 is an XRD pattern of the coral-shaped wide-spectral-response carbonitride polymer material modified by ammonium formate prepared in this example, and XRD diffraction peaks of O-PCN correspond to characteristic peaks of a monomer material PCN, which proves the successful synthesis of the coral-shaped orange carbonitride polymer material with wide spectral response;
FIG. 2 is an SEM image of an ammonium formate-modified coral-shaped broad spectral response carbon nitrogen polymer material prepared in this example, demonstrating that the morphology of O-PCN is coral-shaped;
FIG. 4 is a DRS diagram of the coral-shaped wide-spectral-response carbon-nitrogen polymer material prepared by the method, and it is obvious that the optical response range of the coral-shaped wide-spectral-response carbon-nitrogen polymer material modified by ammonium formate is obviously widened compared with that of a monomer material PCN, and the optical absorption is obviously enhanced in the range of 400-600 nm;
FIG. 5 shows a coral-shaped wide-spectral-response carbon-nitrogen polymer material prepared by the invention 13 CNMR picture, two shoulder peaks appeared on coral-like carbon-nitrogen polymer to prove the formation of C-O-C bond, and the absorption peak of N = C-N with coral-like carbon-nitrogen polymer near 156.5ppm is shifted to low energy region, which indicates that successful doping of oxygen results in electron densityAnd (4) increasing.
Example 3:
compared with example 1, the build-up and broad spectral response of the coral-like carbon nitrogen polymer was achieved by increasing the mass of urea and ammonium formate and the grinding time after cooling.
Weighing 11g of urea, adding 0.4g of ammonium formate, placing the urea and the ammonium formate into an agate mortar, stirring and grinding the urea and the ammonium formate for 5min to uniformly mix the urea and the ammonium formate, transferring the mixture into a ceramic crucible, placing the ceramic crucible into a vacuum drying oven, drying the ceramic crucible at 30 ℃ for 30min, wrapping the crucible with a dried sample by using tin foil paper, sealing the crucible, covering a ceramic cover, placing the crucible into a muffle furnace, heating the crucible to 500 ℃ at the heating rate of 5 ℃/min, calcining the crucible for 80min, cooling the crucible to room temperature, and grinding the crucible for 15min to obtain an orange coral-shaped carbon-nitrogen polymer material (0.4O-PCN)
Example 3 had poorer photocatalytic CO than example 2 2 The reduction performance is mainly caused by the fact that the carrier transmission is hindered due to the fact that ammonium formate is added too much, and the catalyst body is damaged. The material in example 2 is the best ratio material, as shown in figure 3.
Claims (7)
1. A preparation method of an ammonium formate modified coral-shaped wide spectral response carbon nitrogen polymer photocatalyst is characterized by comprising the following steps:
(1) Proportionally placing urea and ammonium formate in an agate mortar, stirring and grinding for a certain time to uniformly mix the urea and the ammonium formate;
(2) Transferring the mixture to a ceramic crucible, and drying the ceramic crucible in a vacuum drying oven at a certain temperature for a period of time;
(3) And (2) wrapping and sealing the crucible containing the dried sample by using tin foil paper, covering a ceramic cover, putting the crucible into a muffle furnace, heating to a certain temperature at a certain heating rate in an ammonia gas atmosphere, calcining for a certain time, cooling to room temperature, and grinding for a certain time to obtain an orange carbon nitrogen polymer material O-PCN, namely the coral-shaped wide-spectrum response carbon nitrogen polymer photocatalyst modified by ammonium formate.
2. The process according to claim 1, wherein in step (1), the mass ratio between urea and ammonium formate is between 9 and 11g:0.05-0.5g.
3. The method according to claim 1, wherein in the step (1), the milling time is 5 to 15min.
4. The method according to claim 1, wherein in the step (2), the temperature of the vacuum drying oven is 30 to 50 ℃ and the drying time is 30 to 60min.
5. The method according to claim 1, wherein in the step (3), the muffle furnace is heated at a rate of 2-5 ℃/min, the calcination temperature is 500-600 ℃, and the calcination time is 50-80min.
6. The method according to claim 1, wherein in the step (3), the grinding time is 10 to 15min.
7. The ammonium formate modified coral-shaped wide-spectral-response carbon-nitrogen polymer photocatalyst prepared by the preparation method of any one of claims 1 to 6 is used for photocatalysis of CO 2 Use of a reduction reaction.
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