CN114682285B - SnNb 2 O (6-x) N x Preparation method and application of nano composite material of metal single atom and nano composite material - Google Patents
SnNb 2 O (6-x) N x Preparation method and application of nano composite material of metal single atom and nano composite material Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 title abstract description 10
- 239000002184 metal Substances 0.000 title abstract description 10
- 239000002135 nanosheet Substances 0.000 claims abstract description 56
- 229910052718 tin Inorganic materials 0.000 claims abstract description 39
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 38
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004202 carbamide Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011941 photocatalyst Substances 0.000 claims abstract description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052797 bismuth Chemical group 0.000 claims abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical group [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 239000010949 copper Chemical group 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Chemical group 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 12
- 239000001301 oxygen Substances 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 238000006303 photolysis reaction Methods 0.000 abstract description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000004873 anchoring Methods 0.000 abstract description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical group [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 abstract 1
- 230000004298 light response Effects 0.000 abstract 1
- 229910052707 ruthenium Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- 238000001914 filtration Methods 0.000 description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 14
- 229940043267 rhodamine b Drugs 0.000 description 14
- 238000001132 ultrasonic dispersion Methods 0.000 description 14
- 239000002086 nanomaterial Substances 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 13
- 229910000510 noble metal Inorganic materials 0.000 description 11
- 238000011161 development Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- KZEVSDGEBAJOTK-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[5-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CC=1OC(=NN=1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O KZEVSDGEBAJOTK-UHFFFAOYSA-N 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- FHMDYDAXYDRBGZ-UHFFFAOYSA-N platinum tin Chemical compound [Sn].[Pt] FHMDYDAXYDRBGZ-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- -1 nitrogen-substituted tin Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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
-
- 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
- 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
-
- 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
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Toxicology (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses SnNb 2 O (6‑x) N x Preparation method and application of metal single-atom nanocomposite and SnNb 2 O 6‑x N x The preparation method of the (C) comprises the following steps: (1) Uniformly mixing urea and water, adding tin niobate nanosheets, and performing hydrothermal reaction after ultrasonic treatment; (2) Drying the product obtained by the hydrothermal reaction and then placing the product in NH 3 And N 2 Is heated and roasted under the mixed atmosphere to obtain SnNb 2 O 6‑x N x A nano-sheet. The invention obtains the SnNb by substituting nitrogen for tin niobate lattice oxygen to form vacancies 2 O 6‑x N x By SnNb 2 O 6‑x N x The vacancy anchoring metal atom in the catalyst can improve the stability of metal monoatoms, and the monoatoms M-SnNb with high catalytic activity and stability is prepared 2 O 6‑x N x Nanocomposite, M is platinum, palladium, copper, ruthenium or bismuth; the nano composite material prepared by the invention has visible light response, and can be used as a visible light photocatalyst to be applied to photocatalytic degradation of organic pollutants, photolysis of water to produce hydrogen and CO 2 Reduction and heterogeneous catalytic reactionsShould, etc.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to SnNb 2 O 6-x N x And a preparation method and application of the metal single-atom nano composite material.
Background
Since the 70 s of the 20 th century, with the rapid development of industrialized society, the increasingly serious environmental pollution and energy shortage become two major difficulties in human development. In order to achieve the goal of sustainable development of human society, development of new technologies that are environmentally friendly and search for alternative clean energy sources are currently the most urgent tasks. Semiconductor photocatalytic technology is one of the most promising technologies for achieving the two tasks described above. However, the core of this process is the development of new stable semiconductor photocatalytic materials.
Tin niobate (SnNb) 2 O 6 ) As a typical two-dimensional (2D) nanomaterial, its valance band is composed of Sn 5s and O2 p hybridized orbitals together, which makes its valance band top position tend to be more negative than niobate composed of pure O2 p, and this unique band gap structure enables it to successfully capture visible light, thus undergoing visible light catalytic reactions; but with a single tin niobate materialThe problems of serious photo-generated electron-hole recombination and weak light absorption capacity severely restrict the use of the photocatalyst as a photocatalyst.
Noble metal loading is an effective means of improving the photocatalytic performance of semiconductors, but such catalysts are expensive, have a scarce storage capacity, and severely limit the wide commercial application thereof. Obviously, reducing the use of a single noble metal, developing a simple, green process to prepare a highly efficient hydrogen evolution catalyst has become extremely important. The research and development of the single-atom catalyst can maximally improve the utilization rate of noble metals, and has great application prospect in the field of photocatalysis. However, the instability of the structure of the single-atom site of the metal, and the migration and agglomeration phenomena of the single-atom site are often accompanied in the preparation and catalytic reaction processes, so that the application and development of the material are severely limited.
Therefore, there is a need to construct a visible light catalyst with low cost, good stability and high catalytic activity for photocatalytic degradation of organic pollutants, photolysis of water to produce hydrogen and CO 2 Reduction, various heterogeneous catalytic reactions, and the like.
Disclosure of Invention
The invention aims to solve the technical problems of providing SnNb 2 O 6-x N x And the preparation method and application of the nano composite material with metal monoatoms, wherein nitrogen is used for substituting tin niobate lattice oxygen to form vacancies, then the vacancies are used for anchoring noble metal monoatoms, the stability of the noble metal monoatoms is improved, and the monoatoms M-SnNb with high catalytic activity are obtained 2 O 6-x N x A nanocomposite.
In order to solve the technical problems, the invention provides the following technical scheme:
the first aspect of the invention provides a SnNb 2 O 6-x N x Preparation method of nanosheets, 0<x<6, comprising the following steps:
(1) Uniformly mixing urea and water, adding tin niobate nanosheets, performing ultrasonic treatment, and performing hydrothermal reaction;
(2) Drying the product obtained by the hydrothermal reaction and then placing the product in NH 3 And N 2 Is heated and roasted under the mixed atmosphere to obtain SnNb 2 O 6-x N x A nano-sheet.
Further, in the step (1), the mass ratio of the urea to the tin niobate nano-sheet is 1:1-10.
Further, in the step (1), the time of the ultrasonic treatment is 0.5-1h.
Further, in the step (1), the temperature of the hydrothermal reaction is 80-220 ℃.
In the step (2), a product after the hydrothermal reaction is dried by adopting a suction filtration drying mode.
Further, in step (2), the NH 3 And N 2 NH in a mixed atmosphere of (2) 3 And N 2 The volume ratio of (2) is 1:0.5-2.
Further, in step (2), the NH 3 And N 2 NH in a mixed atmosphere of (2) 3 And N 2 Preferably 1:0.5 by volume.
Further, in the step (2), the temperature of the heating and roasting is 200-500 ℃, and the time of the heating and roasting is 2-4 hours.
Carrying out hydrothermal reaction on a tin niobate nanosheet, urea and an aqueous solution, carrying out preliminary substitution on oxygen in the tin niobate by nitrogen in the urea, and then placing a product after preliminary substitution of the nitrogen in NH 3 And N 2 Roasting at high temperature in the mixed atmosphere of (2) to obtain SnNb with oxygen vacancies by further substituting nitrogen for lattice oxygen 2 O 6-x N x A nano-sheet. If only hydrothermal reaction is adopted or tin niobate nano-sheets are directly placed in NH 3 And N 2 Is baked at high temperature in the mixed atmosphere of (a) and the tin niobate nano sheet has little oxygen replaced by nitrogen, so that SnNb with a large amount of oxygen vacancies is difficult to obtain 2 O 6-x N x A nano-sheet.
In a second aspect, the invention provides SnNb prepared by the preparation method in the first aspect 2 O 6-x N x Nanoplatelets, 0<x<6。
In a third aspect, the invention provides a monoatomic M-SnNb 2 O 6-x N x A method for preparing a nanocomposite; the preparation method specifically comprises the following steps: the invention is toSnNb of the second aspect 2 O 6-x N x Adding the nano-sheet into the M source precursor solution, heating and stirring to react to obtain single-atom M-SnNb 2 O 6-x N x A nanocomposite.
Further, M is platinum, palladium, silver, copper or bismuth.
Further, the M source precursor solution is chloroplatinic acid, chloropalladic acid, silver nitrate, copper sulfate or bismuth nitrate solution.
Further, the concentration of the M source precursor solution is 2-10mol/L.
Further, the monoatomic M-SnNb 2 O 6-x N x SnNb in nanocomposite 2 O 6-x N x The mass ratio of the metal M is 1:2-10.
Further, the constant-temperature water bath is adopted for heating, so that the materials are heated uniformly.
Further, the temperature of the heating and stirring reaction is 60-80 ℃ and the time is 2-24h.
Further, the temperature of the heating and stirring reaction is preferably 70 ℃ for 2-10h.
Further, the preparation method also comprises the steps of heating, stirring, solid-liquid separation after reaction, water washing and alcohol washing of the separated solid.
According to a fourth aspect of the present invention, there is provided a monoatomic M-SnNb prepared by the preparation method of the third aspect 2 O 6-x N x A nanocomposite.
A fifth aspect of the invention provides a monoatomic M-SnNb as described in the fourth aspect 2 O 6-x N x The application of the nanocomposite in the aspect of visible light photocatalyst.
Further, the visible light photocatalyst can be used for photocatalytic degradation of organic pollutants, photolysis of water to produce hydrogen and CO 2 Reduction and various heterogeneous catalytic reactions.
The invention has the beneficial effects that:
1. the invention utilizes Sn, nb and O ions in the tin niobate to be easy to modulateOr replaced by other ions, and the nitrogen-substituted tin niobate lattice oxygen is formed into SnNb with vacancies by the hydrothermal and atmosphere roasting method 2 O 6-x N x Nanoplatelets, compared to tin niobate nanoplatelets, snNb 2 O 6-x N x Has better photocatalysis performance under the excitation of visible light.
2. The invention utilizes SnNb 2 O 6-x N x The vacancies formed by substituting lattice oxygen with nitrogen in the nano-sheet anchors the noble metal monoatoms, so that the noble metal monoatoms are uniformly distributed in the composite material, and meanwhile, the stability of the noble metal monoatoms in the composite material is improved, so that the noble metal monoatoms are not easy to form clusters to form particles, and the utilization rate of the noble metal is further improved.
3. The invention is realized by adopting SnNb 2 O 6-x N x Dipping in a metal precursor solution to react and prepare the monoatomic M-SnNb 2 O 6-x N x The preparation method is simple to operate, mild in condition, high in reaction rate and low in cost, and is suitable for quantitative production; the prepared monoatomic M-SnNb 2 O 6-x N x The nano composite material has high catalytic activity and good stability, and the full utilization of noble metal in the composite material greatly reduces the catalytic cost.
Drawings
FIG. 1 shows SnNb prepared according to the present invention 2 O 6-x N x Scanning Electron Microscope (SEM) image (a) and X-ray spectroscopy (EDS) image (b);
FIG. 2 is a Pt-SnNb alloy obtained in example 6 2 O 6-x N x SEM images of nanocomposite;
FIG. 3 is a Pt-SnNb alloy obtained in example 6 2 O 6-x N x A High Resolution Transmission Electron Microscope (HRTEM) image of the nanocomposite;
FIG. 4 is a schematic diagram of Pt-SnNb 2 O 6-x N x Nanocomposite, pt-SnNb 2 O 6 Nanocomposite and SnNb 2 O 6 The photocatalytic degradation performance of (2) is compared with that of the other(s);
FIG. 5 is a schematic diagram of Pt-SnNb 2 O 6-x N x Nanocomposite, pt-SnNb 2 O 6 Nanocomposite and SnNb 2 O 6 Is a comparison of the photocatalytic degradation rate.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Example 1: preparation of tin niobate nano material
(1) Weigh 2.24g KOH and disperse in 40mL deionized water and weigh 0.5. 0.5gNb again 2 O 5 Adding into the above solution and stirring for 30min. The mixture was then transferred to a teflon kettle and reacted at 200℃for 3h to give a clear solution, which was then treated with HCl (concentration 2 mol. L -1 ) The solution was adjusted to neutral pH of the above transparent solution to obtain a suspension.
(2) Weigh 0.42g SnCl 2 ·2H 2 O is added to the suspension and the suspension is stirred at 500 r.min -1 Is stirred for 30min. HCl (2 mol.L) -1 ) The pH value of the solution is regulated to 1-3. Then transferred to a teflon reactor and reacted at 200℃for 12h. And (3) after the isothermal temperature is reduced to the room temperature, carrying out suction filtration and washing on the solution in the teflon kettle, and drying the collected yellow powder for 12 hours to obtain the product tin niobate nano material.
Example 2: snNb (tin-zinc) alloy 2 O 6-x N x Preparation of nanomaterials
0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h.Subsequently, the mixture was transferred to a 100mL hydrothermal kettle and reacted hydrothermally at 100℃for 12h. After filtration and drying, at NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 1:2), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nanomaterial.
Example 3: snNb (tin-zinc) alloy 2 O 6-x N x Preparation of nanomaterials
0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle and hydrothermal was performed at 180℃for 12h. After filtration and drying, at NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 1:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nanomaterial.
Example 4: snNb (tin-zinc) alloy 2 O 6-x N x Preparation of nanomaterials
0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle and hydrothermal was performed at 220℃for 12h. After filtration and drying, at NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nanomaterial.
For SnNb prepared in this example 2 O 6-x N x And carrying out analysis and characterization of a scanning electron microscope and an X-ray energy spectrum, wherein the characterization result is shown in figure 1:
FIG. 1a is SnNb 2 O 6-x N x SEM image of nanomaterial, as can be seen from the image, snNb prepared in this example 2 O 6-x N x The nano material presents a fiber and sheet-shaped interweaved morphology, the X-ray energy spectrum analysis result of the nano material is shown as a figure 1b and comprises an element N, O, sn, nb, wherein the mass ratio of oxygen element is 14.31%, the mass ratio of nitrogen element is 5.90%, and the oxygen element is in a tin niobate nano sheetFrom the fact that the mass ratio of the tin oxide to the tin niobate crystal lattice is approximately 24%, oxygen in the tin niobate crystal lattice is replaced by nitrogen, and SnNb is obtained 2 O 6-x N x A nanomaterial.
Example 5: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 2 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Example 6: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 4 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
For Pt-SnNb prepared in this example 2 O 6-x N x Nanocomposite processingThe scanning electron microscope and the high-resolution transmission electron microscope are characterized, and the characterization results are respectively shown in fig. 2 and 3:
FIG. 2 is an SEM image of a sample showing Pt-SnNb 2 O 6-x N x The nano composite material is flake-shaped, and the composite material prepared by the method has smooth surface and no obvious particles; FIG. 3 is a schematic diagram of Pt-SnNb 2 O 6-x N x The HRTEM pattern of the nanocomposite material was observed as distinct lattice fringes, and no lattice fringes of platinum were found, indicating that platinum did not form clusters in the nanocomposite material.
Example 7: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 6 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Example 8: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 8 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Example 9: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.05g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 10 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Example 10: pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.1g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 4 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Examples11：Pt-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.15g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding H into nano-sheet 2 PtCl 6 ·6H 2 O(2 mg·mL -1 ) Stirring at 70deg.C for 4 hr, filtering, and drying to obtain single-atom Pt-SnNb product 2 O 6-x N x A nanocomposite.
Example 12: pd-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.15g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding the nano-sheet into a chloropalladite solution, stirring for 4 hours at 70 ℃, filtering and drying to obtain a product monoatomic Pd-SnNb 2 O 6-x N x A nanocomposite.
Example 13: ag-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.15g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding the nanosheets into silver nitrate solution, stirring for 4 hours at 70 ℃, filtering and drying to obtain the product monoatomic Ag-SnNb 2 O 6-x N x A nanocomposite.
Example 14: cu-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.15g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermally heated at 180℃for 12h, then to NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) SnNb prepared in the step (1) 2 O 6-x N x Adding the nanosheets into a copper nitrate solution, stirring for 4 hours at 70 ℃, filtering and drying to obtain a product of monoatomic Cu-SnNb 2 O 6-x N x A nanocomposite.
Example 15: bi-SnNb 2 O 6-x N x Preparation of nanocomposite materials
(1) 0.15g of urea was weighed and added to 50mL of H 2 To O, 0.5g of the tin niobate nanosheets prepared in example 1 was then added for ultrasonic dispersion for 0.5h. Subsequently, the mixture was transferred to a 100mL hydrothermal kettle, hydrothermal at 180deg.C for 12h, at NH 3 And N 2 Is a mixed atmosphere (NH) 3 And N 2 In a volume ratio of 2:1), roasting for 2 hours at 400 ℃ to obtain yellow SnNb 2 O 6-x N x A nano-sheet.
(2) Preparing SnNb in the step (1) 2 O 6-x N x Adding the nano-sheet into bismuth nitrate solution, stirring for 4 hours at 70 ℃, filtering and drying to obtain the product monoatomic Bi-SnNb 2 O 6-x N x A nanocomposite.
Comparative example: pt-SnNb 2 O 6 Preparation of nanocomposite materials
0.5g of the tin niobate nanosheets prepared in example 1 was weighed and added to 50mL H 2 O, then add a certain amount of H 2 PtCl 6 ·6H 2 O(2mg·mL -1 ) Stirring at 70deg.C for 4 hr, filtering, and drying to obtain final product Pt-SnNb 2 O 6 A nanocomposite.
Photocatalytic Performance study
For the tin niobate nano-sheet prepared in example 1, the single-atom Pt-SnNb prepared in example 6 2 O 6-x N x Nanocomposite and Pt-SnNb prepared in comparative example 2 O 6 The nano composite material is subjected to photocatalysis performance research, rhodamine B (RhB) is taken as a target pollutant, and the photocatalysis degradation effect of different materials on RhB under the irradiation of a 350W xenon lamp (with an optical filter more than or equal to 420 nm); the specific operation is as follows:
(1) Each of the samples prepared in the above examples or comparative examples was taken as a photocatalyst, and mixed with 50mL of RhB solution (10 mol. L -1 ) Adding the mixture into a photocatalysis reaction bottle, and carrying out dark reaction for 0.5h under the condition of no illumination so as to ensure that adsorption-desorption balance is achieved between the photocatalyst and pollutants;
(2) And (3) placing the photocatalytic reaction bottle under a xenon lamp for irradiation, introducing circulating water to maintain the reaction system at 25 ℃, respectively taking 4mL of suspension when the light is irradiated for 0, 30min, 60min, 90min, 120min and 150min, centrifuging to remove the catalyst, measuring the absorbance of the RhB in 554 nm of each system by an ultraviolet spectrophotometer, determining the concentration of the RhB in each system, and further calculating the photocatalytic degradation efficiency of different catalysts.
The test results are shown in FIG. 4, C 0 For the initial concentration of RhB in the reaction system, C is the concentration of RhB in the reaction system during the test, C/C 0 The smaller the value of (C) is, the better the degradation effect of the corresponding photocatalyst on RhB is under the corresponding time, and the graph shows that under the same action time, the monoatomic Pt-SnNb 2 O 6-x N x Nanocomposite materialThe photocatalytic degradation effect on RhB is far better than that of tin niobate and platinum-tin niobate nano composite material, and after 2.5 hours of photocatalytic decomposition, single-atom Pt-SnNb is adopted 2 O 6-x N x The concentration of RhB in the system with the nano composite material as the catalyst is reduced to about 0.3 of the initial concentration, while the concentration of RhB in the system with the platinum-tin niobate nano composite material as the catalyst is still more than 70 percent of the initial concentration; FIG. 5 shows photocatalytic degradation rates of RhB under the same conditions by different catalysts, and shows that the single-atom Pt-SnNb 2 O 6-x N x The photocatalytic degradation rate of the nanocomposite to RhB is higher than that of tin niobate and platinum-tin niobate nanocomposite. As can be seen from the above-mentioned photocatalytic test results, the monoatomic Pt-SnNb prepared by the present invention 2 O 6-x N x The nanocomposite material has excellent visible light photocatalytic effect, and the photocatalytic degradation rate does not change obviously with the extension of the catalytic time, so that the nanocomposite material has good stability.
The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (4)
1. Monoatomic M-SnNb 2 O 6-x N x A method for preparing a nanocomposite material, characterized by comprising the steps of 2 O 6-x N x Adding the nano-sheet into the M source precursor solution, heating and stirring to react to obtain single-atom M-SnNb 2 O 6-x N x A nanocomposite; wherein M is platinum, palladium, silver, copper or bismuth, 0<x<6, preparing a base material; the M source precursor solution is chloroplatinic acid, chloropalladac acid, silver nitrate, copper sulfate or bismuth nitrate solution; the temperature of the heating and stirring reaction is 60-80 ℃ and the time is 2-10 h;
the SnNb 2 O 6-x N x The preparation of the nano-sheet comprises the following steps:
(1) Uniformly mixing urea and water, adding tin niobate nanosheets, performing ultrasonic treatment, and performing hydrothermal reaction; the mass ratio of the urea to the tin niobate nanosheets is 1:1-10;
(2) Drying the product obtained by the hydrothermal reaction and then placing the product in NH 3 And N 2 Is heated and roasted under the mixed atmosphere to obtain SnNb 2 O 6-x N x A nanosheet; the NH is 3 And N 2 NH in a mixed atmosphere of (2) 3 And N 2 The volume ratio of (2) is 1:0.5-2; the temperature of the heating and roasting is 200-500 ℃, and the time of the heating and roasting is 2-4h.
2. A single atom M-SnNb as claimed in claim 1 2 O 6-x N x The preparation method of the nanocomposite is characterized in that in the step (1), the temperature of the hydrothermal reaction is 80-220 ℃.
3. Monoatomic M-SnNb 2 O 6-x N x Nanocomposite material, characterized in that it is prepared by the preparation method according to claim 1 or 2.
4. A monoatomic M-SnNb as in claim 3 2 O 6-x N x The application of the nanocomposite in the aspect of visible light photocatalyst.
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