CN117019193B - Piezoelectric auxiliary photocatalyst and preparation method and application thereof - Google Patents
Piezoelectric auxiliary photocatalyst and preparation method and application thereof Download PDFInfo
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- CN117019193B CN117019193B CN202310846048.3A CN202310846048A CN117019193B CN 117019193 B CN117019193 B CN 117019193B CN 202310846048 A CN202310846048 A CN 202310846048A CN 117019193 B CN117019193 B CN 117019193B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002135 nanosheet Substances 0.000 claims abstract description 75
- 239000002356 single layer Substances 0.000 claims abstract description 51
- 229920003023 plastic Polymers 0.000 claims abstract description 32
- 239000004033 plastic Substances 0.000 claims abstract description 32
- 230000001699 photocatalysis Effects 0.000 claims abstract description 30
- 238000002407 reforming Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000000707 layer-by-layer assembly Methods 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- 239000002244 precipitate Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 239000002064 nanoplatelet Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 229920000098 polyolefin Polymers 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000005286 illumination Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
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- 238000002604 ultrasonography Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000969 carrier Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 40
- 239000000243 solution Substances 0.000 description 26
- 239000004800 polyvinyl chloride Substances 0.000 description 19
- 229920000915 polyvinyl chloride Polymers 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 16
- 239000007864 aqueous solution Substances 0.000 description 16
- 239000004698 Polyethylene Substances 0.000 description 15
- 239000004743 Polypropylene Substances 0.000 description 15
- 229920000573 polyethylene Polymers 0.000 description 15
- 229920001155 polypropylene Polymers 0.000 description 15
- 235000019441 ethanol Nutrition 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 11
- 239000002131 composite material Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
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- 230000000630 rising effect Effects 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- UCOSJYDCOFLFHL-UHFFFAOYSA-N 2-acetylpropanedioic acid Chemical compound CC(=O)C(C(O)=O)C(O)=O UCOSJYDCOFLFHL-UHFFFAOYSA-N 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry 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
- 230000036541 health Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000013502 plastic waste Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
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Classifications
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
- C07C49/04—Saturated compounds containing keto groups bound to acyclic carbon atoms
- C07C49/17—Saturated compounds containing keto groups bound to acyclic carbon atoms containing hydroxy groups
-
- 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
Abstract
The invention discloses a piezoelectric auxiliary photocatalyst, a preparation method and application thereof, wherein the piezoelectric auxiliary photocatalyst comprises the following components: the chemical connection is constructed between the ultrathin BiVO 4 nano-sheet and the ultrathin single-layer g-C 3N4 nano-sheet loaded with Pt, and between the ultrathin BiVO 4 nano-sheet and the ultrathin single-layer g-C 3N4 nano-sheet. The piezoelectric auxiliary photocatalyst is prepared by an electrostatic self-assembly method, wherein a stable chemical connection is formed between an ultrathin BiVO 4 nano sheet with a (010) crystal face selectively exposed and an ultrathin single-layer g-C 3N4 nano sheet, an S-shaped heterojunction is formed, separation and transfer of photo-generated electron hole pairs are promoted, the service life of photo-generated carriers is prolonged, and the hydrogen production activity of photo-catalytic plastic reforming is improved.
Description
Technical Field
The invention belongs to the technical field of degradation of environmental waste plastics, and particularly relates to a piezoelectric auxiliary photocatalyst, and a preparation method and application thereof.
Background
Polyolefin, such as polyvinyl chloride (PVC), polyethylene (PE) and polypropylene (PP), has high chemical stability and low cost, and occupies the highest proportion in plastic production, accounting for more than 50 percent of the total amount of plastic garbage. By 2050, the amount of plastic waste accumulated in the natural environment has increased to 12 hundred million metric tons. Unfortunately, about 80% of the waste plastic is dumped directly into landfills, and the highly chemically inert nature of the plastic exacerbates the problem. "white pollution" constitutes a serious threat to the environment, and its potential impact on human health through biological enrichment is a serious concern.
Compared with the traditional technologies such as mechanical recovery or incineration, the technology of plastic photocatalytic reforming driven by solar energy can convert waste plastics into chemical products with high added value and green hydrogen at normal temperature and normal pressure, and has the advantages of high efficiency, no environmental pollution and the like. However, the photo-catalytic performance is poor due to the defects of easy recombination of photo-generated charges, low service life of photo-generated carriers and the like of the photocatalyst, which limits the application of the catalyst in the aspect of plastic photo-reforming.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a piezoelectric auxiliary photocatalyst, which has stable catalytic performance.
The invention also aims to provide a preparation method of the piezoelectric auxiliary photocatalyst, which is an electrostatic self-assembly method and has the advantages of simple operation, low cost, large-scale preparation, no pollution and the like.
Another object of the present invention is to provide the use of the above-mentioned piezoelectrically assisted photocatalyst for the photocatalytic plastic reforming production of hydrogen.
The aim of the invention is achieved by the following technical scheme.
A piezoelectric assisted photocatalyst, comprising: chemical connection is constructed between an ultrathin BiVO 4 (BVO) nanosheet and an ultrathin monolayer g-C 3N4 (CN) nanosheet loaded with Pt, an ultrathin BiVO 4 (BVO) nanosheet and an ultrathin monolayer g-C 3N4 (CN) nanosheet.
In the technical scheme, chemical connection is constructed between the ultrathin BiVO 4 (BVO) nanosheets and the ultrathin monolayer g-C 3N4 (CN) nanosheets through electrostatic self assembly.
In the technical scheme, the thickness of the ultrathin single-layer g-C 3N4 (CN) nanosheet loaded with Pt is 1-2 nm, and the thickness of the ultrathin BiVO 4 (BVO) nanosheet is 5-6 nm.
The preparation method of the piezoelectric auxiliary photocatalyst comprises the following steps: dispersing an ultrathin single-layer g-C 3N4 (CN) nanosheet and an ultrathin BiVO 4 (BVO) nanosheet into water to obtain a second mixed solution, carrying out ultrasonic treatment on the second mixed solution under the illumination condition for at least 1h, dropwise adding a Pt source (carrying Pt monoatoms by adopting an impregnation adsorption method) into the second mixed solution in the ultrasonic treatment process under the illumination condition, stirring to obtain a second precipitate, cleaning and drying the obtained second precipitate to obtain the piezoelectric auxiliary photocatalyst, wherein the ratio of the ultrathin single-layer g-C 3N4 (CN) nanosheet to the ultrathin BiVO 4 (BVO) nanosheet is 1 (1-5) in parts by weight, and Pt in the Pt source is 0.3-1 wt% of the ultrathin single-layer g-C 3N4 (CN) nanosheet.
In the technical scheme, the concentration of the ultrathin single-layer g-C 3N4 (CN) nanosheets in the second mixed solution is 0.05-0.1 mg/mL.
In the above technical scheme, the ultrathin BiVO 4 (BVO) nanosheets are selectively exposed for (010) crystal faces.
In the above technical solution, the Pt source is a Pt salt solution.
In the above technical solution, the Pt salt solution is an aqueous H 2PtCl6·6H2 O solution.
In the technical scheme, the concentration of H 2PtCl6·6H2 O in the H 2PtCl6·6H2 O aqueous solution is 1-1.5 mg mL -1.
In the technical scheme, the cleaning agent is a mixture of water and ethanol, and the ratio of the water to the ethanol in the cleaning agent is 7 (1-3) in parts by volume.
In the technical scheme, the stirring temperature is 60-80 ℃, and the stirring time is 1-3 h.
In the technical scheme, the drying temperature is 60-80 ℃.
In the above technical scheme, the time of the ultrasonic treatment is 1-5 hours, preferably 2-4 hours.
In the technical scheme, the method for preparing the ultrathin single-layer g-C 3N4 (CN) nanosheets comprises the following steps: calcining urea powder for 1-4 h at 500-580 ℃ with limited oxygen to obtain a first product, oxidizing and etching the first product for 1-4 h at 500-555 ℃ to obtain a second product, dispersing the second product into water and carrying out ultrasonic treatment for 1-3 h, and drying to obtain the ultrathin single-layer g-C 3N4 (CN) nanosheets.
In the technical scheme, the drying temperature is 60-80 ℃, and the drying time is 8-12 h.
In the technical scheme, 0.2-0.5 part by weight of the second product is dispersed into 50-100 parts by volume of water and is subjected to ultrasonic treatment for 1-3 hours, wherein the unit of the parts by volume is mL, and the unit of the parts by weight is g.
Preferably, the temperature of the oxygen limiting calcination is 545-555 ℃, and the time of the oxygen limiting calcination is 1.5-2.5 h.
Preferably, the temperature of the oxidation etching is 515-525 ℃, and the time of the oxidation etching is 2.5-3.5 h.
Preferably, in the method for preparing the ultrathin single-layer g-C 3N4 (CN) nanosheets, the ultrasonic time is 1.5-2.5 h.
Preferably, the temperature rising rates of oxygen limited calcination and oxidation etching are each 4 to 6 ℃/min.
In the above technical scheme, the method for preparing the ultrathin BiVO 4 (BVO) nanosheets comprises the following steps: dissolving 0.1 to 0.5 part by mass (preferably 0.2 to 0.25 part by mass) of Bi (NO 3)3·5H2 O) in 2 to 8 parts by volume (preferably 4 to 6 parts by volume) of HNO 3 aqueous solution, adding 0.1 to 0.3 part by mass (preferably 0.12 to 0.15 part by mass) of sodium dodecyl benzene sulfonate (C 18H29NaO3 S, SDBS), and fully dissolving to obtain a first solution; dissolving 0.1-0.5 part by weight (preferably 0.25-0.35 part by weight) of NH 4VO3 in 1-8 parts by weight (preferably 4-6 parts by weight) of NaOH aqueous solution, adding 0.1-0.3 part by weight (preferably 0.12-0.15 part by weight) of sodium dodecyl benzene sulfonate (C 18H29NaO3 S, SDBS), fully dissolving to obtain a second solution, mixing the first solution and the second solution, stirring to obtain a first mixed solution, adjusting the first mixed solution to be neutral, carrying out hydrothermal reaction on the first mixed solution adjusted to be neutral at 100-250 ℃ for 1-5 hours, naturally cooling to room temperature after the reaction is finished to obtain a first precipitate, washing and drying the obtained first precipitate to obtain an ultrathin BiVO 4 (BVO) nanosheet, wherein the ratio of Bi (NO 3)3·5H2 O) in the first solution to NH 4VO3 in the second solution is (0.1-0.5) in parts by weight:
(0.1-0.5), wherein the volume fraction is in mL, and the mass fraction is in g.
In the above technical scheme, the concentration of HNO 3 in the HNO 3 aqueous solution is 2.0-5.0M, preferably 3.5-4M.
In the technical scheme, naOH aqueous solution is adopted for adjusting to be neutral.
In the above technical scheme, the concentration of NaOH in the NaOH aqueous solution is 1-4M, preferably 1.5-2.5M.
In the technical scheme, the drying temperature is 60-80 ℃.
In the technical scheme, the temperature of the hydrothermal reaction is 190-210 ℃, and the time of the hydrothermal reaction is 3-5 h.
In the technical scheme, the cleaning adopts a mixture of water and ethanol, and the ratio of the water to the ethanol is 7 (1-3) in parts by volume.
The application of the piezoelectric auxiliary photocatalyst in hydrogen production by reforming photocatalytic plastic.
In the above technical scheme, the plastic is polyolefin, and the polyolefin is PVC, PP or PE.
In the technical scheme, the piezoelectric auxiliary photocatalyst, the plastic and the water are mixed, and an ultrasonic field is applied and irradiated under the environment of 5-15 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. The piezoelectric auxiliary photocatalyst is prepared by an electrostatic self-assembly method, wherein a stable chemical connection is formed between an ultrathin BiVO 4 (BVO) nano sheet with a (010) crystal face selectively exposed and an ultrathin single-layer g-C 3N4 (CN) nano sheet, an S-shaped heterojunction is formed, separation and transfer of photo-generated electron hole pairs are promoted, the service life of photo-generated carriers is prolonged, and the reforming hydrogen production activity of photocatalytic plastics is improved;
2. Stretching or compressing an ultra-thin single-layer g-C 3N4 (CN) nanosheet dipole of an ultrasonic field under mechanical vibration to generate piezoelectric potential, and loading Pt single-atom sites to further improve the polarized dipole moment of the ultra-thin single-layer g-C 3N4 (CN) nanosheet to generate stronger piezoelectric potential, wherein the piezoelectric field drives photo-generated carriers to directionally migrate, so that the separation efficiency and the transmission distance of photo-generated charges are obviously improved;
3. The piezoelectric auxiliary photocatalyst can realize plastic photocatalytic reforming and separate out hydrogen, is an ideal, efficient and stable photocatalyst for producing hydrogen by photocatalytic plastic reforming, and has obviously improved plastic reforming performance due to Pt single atoms;
4. The plastic is an energy source raw material rich in carbon and hydrogen, and chemical products with high added value can be obtained by utilizing a piezoelectric auxiliary photocatalyst photocatalysis plastic reforming method. PVC, PP and PE are selectively photo-reformed into dicarboxylacetone (glycerone), which shows that the technology has the advantages of low cost, low carbon, environmental protection and industrialization potential.
Drawings
FIG. 1 is an X-ray diffraction pattern of an ultrathin single-layer g-C 3N4 nano-sheet in example 1, an ultrathin BiVO 4 nano-sheet in example 1, a CN/BVO composite photocatalyst prepared in example 1 and a piezoelectric auxiliary photocatalyst prepared in example 2 of the invention;
FIG. 2 is a transmission electron microscope image of the piezoelectric auxiliary photocatalyst in example 2, wherein a is a transmission electron microscope image at a lower resolution, and b is a transmission electron microscope image at a higher resolution;
FIG. 3 is a high angle annular dark field image-scanning transmission electron microscope of the piezoelectric assisted photocatalyst of example 2, wherein a is a high angle annular dark field image-scanning transmission electron microscope of ultrathin BiVO 4 (BVO) nanoplatelets in the piezoelectric assisted photocatalyst, and b is a high angle annular dark field image-scanning transmission electron microscope of ultrathin single-layer g-C 3N4 (CN) nanoplatelets in the piezoelectric assisted photocatalyst;
FIG. 4 is a scanning Atomic Force Microscope (AFM) image of the piezoelectric assisted photocatalyst prepared in example 2;
FIG. 5 is a piezoelectric atomic force microscope (PFM) diagram of the piezoelectric assisted photocatalyst prepared in example 2;
FIG. 6 is a graph showing the displacement-voltage curve and the phase of the piezoelectric auxiliary photocatalyst prepared in example 2;
FIG. 7 is an X-ray photoelectron spectrum of the piezoelectric auxiliary photocatalyst obtained in example 2, wherein a to f are high-resolution X-ray photoelectron spectra of C element, N element, pt element, V element, bi element, and O element, respectively;
FIG. 8 shows the photocatalytic PVC reforming activity of the CN/BVO composite photocatalyst prepared in example 1 and the piezoelectric auxiliary photocatalyst prepared in example 2 under the condition of applying an ultrasonic field;
FIG. 9 is the Apparent Quantum Efficiency (AQE) of photocatalytic PVC reforming for the piezoelectrically assisted photocatalyst of example 2;
FIG. 10 is a graph showing the comparison of the photo-reforming rates of PE and PP with respect to the piezoelectric auxiliary photocatalyst prepared in example 2;
FIG. 11 is a gas chromatograph-mass spectrum of the products of photocatalytic PVC, PE and PP reforming with the piezoelectrically assisted photocatalyst of example 2;
Fig. 12 is Sang Jitu of low carbon products of photocatalytic PVC, PE and PP reforming for the piezoelectrically assisted photocatalyst of example 2.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
The method for preparing the ultrathin single-layer g-C 3N4 (CN) adopts a thermal polycondensation method.
In the following examples, oxygen limited calcination: this was accomplished in static air by covering the porcelain boat containing the sample with tinfoil.
The raw materials and home information involved in the following examples are as follows: urea (Shanghai Ala chemical Co., ltd.), absolute ethyl alcohol (Shanghai Ala chemical Co., ltd.), bismuth nitrate pentahydrate (Shanghai Tay chemical Co., ltd.), nitric acid (Tianjin Bo chemical Co., ltd.), sodium dodecylbenzenesulfonate (Shanghai Ala chemical Co., ltd.), ammonium vanadate (Kai Mart chemical Co., ltd.), sodium hydroxide (Tianjin Bo chemical Co., ltd.), hexachloroplatinic acid (Shanghai Ala chemical Co., ltd.), PVC plastics (Jie Cheng plasticizing Co., powder), PP plastics (Jie Cheng plasticizing Co., powder), PE plastics (Jie Cheng plasticizing Co., powder).
The instruments and their model information involved in the following examples are as follows: magnetic stirrer (PT 1000-A, kamammot technologies Co., ltd.), tube furnace (GY 200, tianjin Solomon biotechnology Co., ltd.), high pressure reactor (S50, tianjin Solomon biotechnology Co., ltd.), oven (TR 620, bellgley technologies Co., ltd.), xenon lamp (CEL-PF 300, beijing medium teaching gold source Co., ltd.), ultrasonic generator (SB-3200 DT, shanghai Taitan technologies Co., ltd.), high resolution transmission electron microscope (HR-TEM, JEOL JEM-2100F, japanese electronics Co., ltd.), HAADF-STEM spherical aberration correction transmission electron microscope (JEM-ARM 200F NEOARM, japanese electronics Co., ltd.), an X-ray diffractometer (Rigaku D/Max2200PC, japanese Co., ltd.), an X-ray photoelectron spectrometer (Thermal ESCALAB 250, simer 'S Feishmanic technology Co., ltd.), an atomic force microscope (division Icon, bruce Co., ltd.), a photocatalytic activity evaluation system (CEL-PAEM-D8, beijing' S Ind.), a GC-MS gas chromatograph/four-pole electrostatic field orbital hydrazine combination high resolution mass spectrum (HP 6890-Plus, agilent technology Co., ltd.).
Example 1
The preparation method of the CN/BVO composite photocatalyst is an electrostatic self-assembly method, and comprises the following steps: and dispersing the ultrathin single-layer g-C 3N4 (CN) nanosheets and the ultrathin BiVO 4 (BVO) nanosheets with the (010) crystal faces selectively exposed into water to obtain a second mixed solution, wherein the concentration of the ultrathin single-layer g-C 3N4 (CN) nanosheets in the second mixed solution is 0.05mg/mL. And (3) carrying out ultrasonic treatment on the second mixed solution for 3 hours under the irradiation of a 300W xenon lamp, stirring for 2 hours at 70 ℃ to obtain a second precipitate, washing the obtained second precipitate for 5 times by using a mixed solution of water and ethanol (the volume ratio of water to ethanol is 7:3), drying for 12 hours in an oven at 80 ℃, and grinding to obtain the CN/BVO composite photocatalyst, wherein the ratio of the ultrathin single-layer g-C 3N4 (CN) nanosheets to the ultrathin BiVO 4 (BVO) nanosheets selectively exposed by (010) crystal faces is 1:1 in parts by weight.
The method for preparing the ultrathin single-layer g-C 3N4 (CN) nanosheets is a thermal condensation method (see document ：Hu C,Chen F,Wang Y,et al.Exceptional cocatalyst-free photo-enhanced piezocatalytic hydrogen evolution of carbon nitride nanosheets from strong in-plane polarization[J].Advanced Materials,2021,33(24):2101751.),, which comprises the steps of placing urea powder in an alumina crucible, performing oxygen limiting calcination at 550 ℃ for 2 hours to obtain a first product, performing oxidative etching (air condition) on the first product at 520 ℃ for 3 hours to obtain a second product, dispersing 0.2g of the second product into 50mL of water, performing ultrasonic treatment for 3 hours, and drying at 60 ℃ for 12 hours to obtain the ultrathin single-layer g-C 3N4 (CN) nanosheets, wherein the temperature rising speed of the oxygen limiting calcination and the oxidative etching is 5 ℃/min.
The method for preparing the ultrathin BiVO 4 (BVO) nanosheets with selectively exposed (010) crystal faces is a hydrothermal method (see literature ：Chen T,Chen W,Zhang Z,et al.Preferential photo-carrier exchange in(010)facet of BiVO4 with decorated CdS nanoparticles[J].Applied Physics Letters,2021,119(25).),, which comprises the steps of dissolving 0.21 part by mass of Bi (NO 3)3·5H2 O) in 5 parts by volume of HNO 3 aqueous solution, adding 0.13 part by mass of sodium dodecyl benzene sulfonate (C 18H29NaO3 S, SDBS) into the solution, fully dissolving to obtain a first solution, dissolving 0.29 part by mass of NH 4VO3 into 5 parts by volume of NaOH aqueous solution, adding 0.13 part by mass of sodium dodecyl benzene sulfonate (C 18H29NaO3 S, SDBS) into the solution, fully dissolving to obtain a second solution, slowly mixing the first solution and the second solution, stirring to obtain a first mixed solution, transferring the first mixed solution which is adjusted to be neutral into a Teflon lining autoclave (the filling ratio is 60-90%), carrying out hydrothermal reaction for 4h at 200 ℃, naturally cooling to room temperature after the reaction is finished, obtaining a first precipitate (the solution with the concentration of HNO) of 60-90%, and the ethanol solution (the concentration of the first precipitate being equal to 57M, namely, 50M, 37 g of ethanol (water solution, 60:37) is obtained by volume of ethanol (water solution, 60:37) of the aqueous solution, and the second precipitate (aqueous solution of ethanol solution with the concentration of water solution being equal to 57 g, and 60M, and 60% of ethanol (water solution of the aqueous solution of the second precipitate being obtained by volume, and 50) being washed by volume of water solution being prepared by 35, and the aqueous solution being washed by volume of the aqueous solution being washed by 35, and the solution being prepared by 35 (containing the solution).
Example 2
A piezoelectric assisted photocatalyst, comprising: the ultrathin BiVO 4 (BVO) nanosheets and the ultrathin single-layer g-C 3N4 (CN) nanosheets loaded with Pt form stable chemical connection through electrostatic self assembly between the ultrathin BiVO 4 (BVO) nanosheets and the ultrathin single-layer g-C 3N4 (CN) nanosheets, wherein the thickness of the ultrathin single-layer g-C 3N4 (CN) nanosheets loaded with Pt is 1.5nm, and the thickness of the ultrathin BiVO 4 (BVO) nanosheets with selective exposure of (010) crystal faces is 5.7nm.
The preparation method of the piezoelectric auxiliary photocatalyst is an electrostatic self-assembly method and comprises the following steps: dispersing ultrathin single-layer g-C 3N4 (CN) nanosheets and ultrathin BiVO 4 (BVO) nanosheets with selectively exposed (010) crystal faces into water to obtain a second mixed solution, wherein the concentration of the ultrathin single-layer g-C 3N4 (CN) nanosheets in the second mixed solution is 0.05mg/mL, carrying out ultrasonic treatment on the second mixed solution for 3H under the irradiation condition of a 300W xenon lamp, dropwise adding an H 2PtCl6·6H2 O aqueous solution with the concentration of 1.48mg of H 2PtCl6·6H2 O being -1 into the second mixed solution in the process of ultrasonic treatment under the irradiation condition of the xenon lamp, stirring for 2H at 70 ℃ to obtain a second precipitate, washing the obtained second precipitate for 5 times through a mixed solution of water and ethanol (the volume ratio of water to ethanol is 7:3), and drying for 12H in an oven at 80 ℃ and grinding to obtain the piezoelectric auxiliary photocatalyst, wherein the ratio of the ultrathin single-layer g-C 3N4 (CN) nanosheets to the ultrathin single-layer (BVO) nanosheets with selectively exposed (010) crystal faces is 1.48mg of H 2PtCl6·6H2 O aqueous solution in 35wt% of 1 to 35wt% of BVO (35) aqueous solution in the mixed solution.
The method for preparing the ultrathin single-layer g-C 3N4 (CN) nanosheets is the same as that of the ultrathin single-layer g-C 3N4 (CN) nanosheets in example 1.
The method of preparing (010) crystal plane selectively exposed ultrathin BiVO 4 (BVO) nanoplatelets is the same as the method of preparing (010) crystal plane selectively exposed ultrathin BiVO 4 (BVO) nanoplatelets in example 1.
Product analysis and performance determination:
Topography schematic and phase analysis:
The X-ray diffraction patterns of the ultra-thin single-layer g-C 3N4 nano-sheet (CN in fig. 1), the ultra-thin BiVO 4 nano-sheet (BVO in fig. 1) in example 1, the CN/BVO composite photocatalyst (CN/BVO in fig. 1) prepared in example 1, and the piezoelectric auxiliary photocatalyst (Pt SA/CN/BVO in fig. 1) prepared in example 2 are shown in fig. 1, and the TEM pattern of the piezoelectric auxiliary photocatalyst prepared in example 2 is shown in fig. 2, and it can be seen that the ultra-thin single-layer g-C 3N4 (CN) nano-sheet and the ultra-thin BiVO 4 (BVO) nano-sheet with the (010) crystal face selectively exposed are successfully combined and a two-dimensional stacked photocatalytic system is formed.
The high-angle annular dark field image-scanning transmission electron microscope image of the piezoelectric auxiliary photocatalyst prepared in example 2 is shown in fig. 3, and it can be seen that Pt single-atom sites are successfully loaded on an ultrathin single-layer g-C 3N4 (CN) nanosheet.
As shown in a scanning Atomic Force Microscope (AFM) of the piezoelectric auxiliary photocatalyst prepared in example 2 in FIG. 4, it can be seen that the thicknesses of the ultrathin monolayer g-C 3N4 (CN) nanosheets and the ultrathin BiVO 4 (BVO) nanosheets with selectively exposed (010) crystal faces after Pt single atoms are supported are 1.5nm and 5.7nm, respectively.
As shown in FIG. 5, the piezoelectric atomic force microscope (PFM) of the piezoelectric auxiliary photocatalyst prepared in example 2 shows that the ultrathin single-layer g-C 3N4 (CN) nanosheets have a strong in-plane polarization effect.
The displacement-voltage curve and the phase curve of the piezoelectric auxiliary photocatalyst prepared in example 2 are shown in fig. 6, and it can be seen that the ultrathin monolayer g-C 3N4 (CN) nanosheets have good piezoelectric response after Pt monoatomic sites are loaded.
The X-ray photoelectron spectrum of the piezoelectric auxiliary photocatalyst prepared in example 2 is shown in fig. 7, and it can be seen that stable chemical connection is constructed between an ultrathin single-layer g-C 3N4 (CN) nanosheet and an ultrathin BiVO 4 (BVO) nanosheet with a (010) crystal face selectively exposed through electrostatic self-assembly.
Example 3
The application of the piezoelectric auxiliary photocatalyst in hydrogen production by photocatalysis of PVC reforming.
The photocatalytic reforming method comprises the following steps: 20mg of the piezoelectrically assisted photocatalyst obtained in example 2 were admixed with 300mg of PVC in 100mL of water, and the whole system was kept at 10 ℃. A300W xenon lamp (simulated sunlight) was irradiated for 8 hours, and simultaneously an ultrasonic wave of 40kHZ was applied with an ultrasonic generating device (SB-3200 DT). And analyzing and collecting the generated gas by adopting gas chromatography (CEL-PAEM-D8), filtering the residual solid after the reaction, drying at 60 ℃ for 12 hours, weighing by using a precision balance, and calculating the weight loss of the plastic, thus obtaining the PVC light reforming activity of the piezoelectric auxiliary photocatalyst when light irradiation and an ultrasonic field are simultaneously applied.
Example 4
The CN/BVO composite photocatalyst is applied to hydrogen production by photocatalysis of PVC reforming. The procedure was essentially the same as in example 3, "application of the piezoelectrically assisted photocatalyst in photocatalytic PVC reforming to hydrogen", with the only difference that "piezoelectrically assisted photocatalyst of example 2" in example 3 was replaced by "CN/BVO composite photocatalyst of example 1".
The experimental results of example 3 (Pt SA/CN/BVO in fig. 8) and example 4 (CN/BVO in fig. 8) are shown in fig. 8, where the piezo-assisted photocatalyst has the highest plastic reforming rate, the plastic mass loss (Weight loss in fig. 8) can reach 18.39mg·h -1, and the synchronous hydrogen production rate can reach 8.08mmol·g -1·h-1, indicating that loading Pt single atoms can significantly improve the performance of the catalyst due to the enhanced piezoelectric field promoting rapid separation and migration of photogenerated carriers.
Example 5
Measurement of apparent light quantum efficiency (AQE): the experimental procedure is identical to example 3, except that: the apparent light quantum efficiency of the piezoelectric auxiliary photocatalyst reaches the highest at 365nm and can reach 1.37% when light with different wavelengths (365 nm, 420nm, 475nm, 530nm and 585 nm) is used for irradiation, as shown in fig. 9, which further shows the excellent plastic light reforming activity of the piezoelectric auxiliary photocatalyst.
Example 6
The application of the piezoelectric auxiliary photocatalyst in the photocatalytic PE reforming hydrogen production is provided. The procedure was essentially the same as in example 3, "application of the piezo-assisted photocatalyst in photocatalytic PVC reforming to hydrogen, except that" PVC "in example 3 was replaced with" PE ".
Example 7
The application of the piezoelectric auxiliary photocatalyst in hydrogen production by photocatalytic PP reforming. The procedure is essentially the same as in example 3, "application of the piezo-assisted photocatalyst in photocatalytic PVC reforming to hydrogen", except that "PVC" in example 3 is replaced with "PP".
The reforming activities of example 6 (photocatalytic PE) and example 7 (photocatalytic PP) are shown in fig. 10, and the piezoelectric auxiliary photocatalyst shows excellent catalytic activity in the application of both photocatalytic PE and photocatalytic PP, wherein the mass loss of PE can reach 16.72mg·h -1, the synchronous hydrogen generation rate can reach 7.50mmol·g -1·h-1, the mass loss of PP can reach 14.54mg·h -1, and the synchronous hydrogen generation rate can reach 6.21mmol·g -1·h-1, which indicates that Pt single atom loading can significantly improve the catalytic activity of the catalyst, and the plastic photo-reforming strategy based on piezoelectric field assistance has better universality.
Analysis method of plastic light reformate: the photocatalytic plastic reformate for example 3, example 6 and example 7 was analyzed using an HP 6890-Plus gas chromatograph mounted on a 5973 type mass selective detector (agilent, usa), using a fused silica capillary column (CP-SIL 8cb,30cm x 0.25 mm), with the carrier gas being helium, the GC oven was held at 80 ℃ for 10 minutes, warmed to 270 ℃ at a 50 ℃/min ramp rate, and held at 270 ℃ for 3 minutes. The transmission line temperature was 280 ℃, the MS ion source temperature was 230 ℃, and the electron impact ionization was maintained at 70eV. 2 μl of the solution after the extraction reaction (from example 3, example 5 and example 6, respectively) was injected into a gas chromatograph injector (injector temperature was set to 250 ℃), and as a result, about 20 peaks appeared in the gas chromatograph mass spectrogram, corresponding to products after photo-reforming of PP, PVC and PE, respectively, were shown in fig. 11, and for detailed understanding of the composition of the products, a list of possible low carbon products (C6 <) was obtained by using a NIST database for product screening, and as shown in fig. 12 and table 1, sang Jitu of photo-catalytic reformed products and corresponding low carbon product summary tables were obtained, among which glycerones were relatively high in the reformed products, indicating that PVC, PP and PE were selectively photo-reformed into glycerones, and the selectivity was up to 91%.
TABLE 1
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (12)
1. The application of the piezoelectric auxiliary photocatalyst in hydrogen production by reforming of photocatalytic plastic is characterized in that the preparation method of the piezoelectric auxiliary photocatalyst comprises the following steps: dispersing an ultrathin single-layer g-C 3N4 nano sheet and an ultrathin BiVO 4 nano sheet into water to obtain a second mixed solution, carrying out ultrasonic treatment on the second mixed solution for at least 1h under the illumination condition, dropwise adding a Pt source into the second mixed solution in the ultrasonic treatment process under the illumination condition, stirring to obtain a second precipitate, and washing and drying the obtained second precipitate to obtain the piezoelectric auxiliary photocatalyst, wherein the ratio of the ultrathin single-layer g-C 3N4 nano sheet to the ultrathin BiVO 4 nano sheet is 1 (1-5) in parts by weight, and Pt in the Pt source is 0.3-1 wt% of the ultrathin single-layer g-C 3N4 nano sheet.
2. The use according to claim 1, wherein the ultra-thin BiVO 4 nanoplatelets are (010) crystal plane selective exposed.
3. The use according to claim 1, wherein the method for preparing ultra-thin single-layer g-C 3N4 nanoplatelets comprises: calcining urea powder for 1-4 h at 500-580 ℃ with limited oxygen to obtain a first product, oxidizing and etching the first product for 1-4 h at 500-555 ℃ to obtain a second product, dispersing the second product into water and carrying out ultrasonic treatment for 1-3 h, and drying to obtain the ultrathin single-layer g-C 3N4 nano sheet.
4. The use according to claim 1, wherein the piezo-assisted photocatalyst comprises: the chemical connection is constructed between the ultrathin BiVO 4 nano-sheet and the ultrathin single-layer g-C 3N4 nano-sheet loaded with Pt, and between the ultrathin BiVO 4 nano-sheet and the ultrathin single-layer g-C 3N4 nano-sheet.
5. The use according to claim 4, wherein chemical bonding is established between the ultra-thin BiVO 4 nanoplatelets and the ultra-thin monolayer g-C 3N4 nanoplatelets by electrostatic self-assembly.
6. The use according to claim 4, wherein the thickness of the Pt-loaded ultra-thin monolayer g-C 3N4 nanoplatelets is 1-2 nm.
7. The use according to claim 4, wherein the ultra-thin BiVO 4 nanoplatelets have a thickness of 5-6 nm.
8. The use according to claim 1, wherein the concentration of the ultrathin monolayer g-C 3N4 nanoplatelets in the second mixed solution is 0.05-0.1 mg/mL.
9. The use according to claim 1, wherein the Pt source is a Pt salt solution.
10. Use according to claim 8, wherein the plastic is a polyolefin.
11. Use according to claim 10, characterized in that the polyolefin is PVC, PP or PE.
12. Use according to claim 1, characterized in that the piezo-electric auxiliary photocatalyst, plastic and water are mixed, an ultrasound field is applied and illuminated in an environment of 5-15 ℃.
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