CN111790380B - Preparation method of fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles - Google Patents
Preparation method of fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles Download PDFInfo
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- CN111790380B CN111790380B CN202010770579.5A CN202010770579A CN111790380B CN 111790380 B CN111790380 B CN 111790380B CN 202010770579 A CN202010770579 A CN 202010770579A CN 111790380 B CN111790380 B CN 111790380B
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 53
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 5
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000027756 respiratory electron transport chain Effects 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 description 13
- 229910017745 AgNP Inorganic materials 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- 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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
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- 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
- B01J35/396—Distribution of the active metal ingredient
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical Kinetics & Catalysis (AREA)
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- Combustion & Propulsion (AREA)
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Abstract
A preparation method of a fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles comprises the following steps: dissolving silver nitrate in a mixed solution of deionized water and methanol to form a solution a; dissolving benzimidazole in a mixed solution of deionized water and methanol to form a solution b; and dissolving melamine and polyvinylpyrrolidone in the mixed solution of deionized water and methanol to form a solution d. And pouring the solution b into the solution a to form a solution c, and pouring the solution d into the solution c to form a solution e. Heating and stirring the solution e, centrifugally separating and collecting a product, and washing to obtain an Ag precursor; and calcining the precursor of Ag at high temperature for a period of time to obtain a fan-shaped structure assembled by the carbon-coated silver nanoparticles. The method of the invention takes the silver-based complex as a precursor, constructs the photocatalyst with a fan-shaped structure assembled by carbon-coated silver nano particles through in-situ calcination, and improves the electron transfer capacity and the photocatalytic activity of the silver nano particles.
Description
Technical Field
The invention relates to a photocatalyst, in particular to a preparation method of a fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles.
Background
Silver (Ag) Nanoparticles (NPs) are relatively inexpensive compared to other noble metal NPs such as platinum (Pt) and gold (Au), etc., and the agnps have high conductivity, large specific surface area, plasmon properties, etc., and thus have attracted considerable attention. The surface plasmon resonance technology of AgNP is widely applied to the aspects of sensors, biological equipment, data storage, spectrum technology, catalysis and the like. The AgNP can absorb visible light through Surface Plasmon Resonance (SPR), and is often used as a photocatalyst in a photocatalysis process. However, plasmon excitation in AgNP has a short thermionic lifetime, resulting in low catalytic efficiency.
Disclosure of Invention
The invention aims to provide a fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles, which solves the problem of difficult AgNP electron transmission and solves the problem of less exposed active sites through an assembled fan-shaped structure.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of a fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles comprises the following steps:
s1: dissolving silver nitrate in a mixed solution of deionized water and methanol, and uniformly stirring to form a solution a;
dissolving benzimidazole in a mixed solution of deionized water and methanol, and uniformly stirring to form a solution b;
dissolving melamine and polyvinylpyrrolidone into a mixed solution of deionized water and methanol, and uniformly stirring to form a solution d;
s2: pouring the solution b into the solution a, and uniformly stirring to form a solution c; pouring the solution d into the solution c, and uniformly stirring to form a solution e;
s3: heating and stirring the solution e for a period of time, then centrifugally separating and collecting a product, and washing to obtain an Ag precursor;
s4: and calcining the precursor of Ag at high temperature for a period of time to obtain a fan-shaped structure assembled by the carbon-coated silver nanoparticles.
As a preferred technical scheme, the volume ratio of deionized water to methanol in the mixed solution of deionized water and methanol is 1:1.
preferably, in step S2, the volume ratio of the solution b to the solution a is 1:1, the volume ratio of the solution c to the solution d is 2:1.
as a preferred technical solution, the step S3 specifically includes: and heating the solution e to 90 ℃, stirring for 4.5h, then collecting a product through centrifugal separation, and washing the product for several times by using deionized water and industrial alcohol to obtain the precursor of the Ag with uniform size and appearance.
In a preferred embodiment, in step S4, the temperature of the high-temperature calcination is 330 ℃, and the calcination time is 60min.
The invention also provides the photocatalyst with the fan-shaped structure assembled by the uniform carbon-coated silver nanoparticles, which is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the method of the invention takes the silver-based complex as a precursor, and constructs the photocatalyst with a fan-shaped structure assembled by carbon-coated silver nano particles through in-situ calcination. The electron transport capacity and the photocatalytic activity of the silver nanoparticles are improved by coating the silver nanoparticles with carbon;
according to the method, the problem of AgNP thermal electron mass transfer is solved by combining the carbon material and the Ag nano particles and utilizing the strong electron transmission capability of the carbon material, the problem of difficult AgNP electron transmission is solved by the synthesized fan-shaped structure photocatalyst assembled by uniformly coating the silver nano particles with carbon, and the problem of less exposed active sites is solved by the assembled fan-shaped structure.
Drawings
FIG. 1 (a) X-ray powder diffraction pattern (XRD) of Ag-based complexes; (b) low power Scanning Electron Micrographs (SEM) of Ag-based complexes;
FIG. 2 (a) Scanning Electron Micrograph (SEM) after 4.5h reaction at 90 ℃; (b), (c), (d), (e) is the element analysis diagram;
FIG. 3 (a) X-ray powder diffraction pattern (XRD) of the product; (b) Scanning Electron Micrographs (SEM) of the product; (c) Scanning Electron Micrograph (SEM) of the product at magnification; (d) Transmission Electron Micrographs (TEM) of the product;
FIG. 4 (a) hydrogen generation diagram of Ag @ C irradiation for 10 hours; (b) photocurrent response diagram.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Examples
1. The synthesis method of the precursor comprises the following steps:
dissolving silver nitrate in a solution of deionized water and methanol (1), and uniformly stirring to form a solution a; dissolving benzimidazole (0.01 g) in a solution of deionized water and methanol (1), and uniformly stirring to form a solution b; then pouring the solution b into the solution a, and uniformly stirring to form a solution c; dissolving melamine (0.013 g) and polyvinylpyrrolidone (PVP, 0.05 g) in a solution of deionized water and methanol (1; and finally, pouring the solution d into the solution c, stirring uniformly to form a solution e, heating to 90 ℃, and stirring for 4.5 hours. And (3) collecting a product through centrifugal separation, and then washing the product for a plurality of times by using deionized water and industrial alcohol to obtain the precursor of the Ag with uniform size and appearance. Fig. 1 is an XRD (fig. 1 a) and a scanning electron micrograph (fig. 1 b) of the product obtained by solvothermal under the experimental conditions described above. The XRD chart shows that the obtained product is an Ag-based precursor with better crystallinity, and the scanning electron microscope chart shows that the obtained product is an Ag-based complex with a one-dimensional rod-assembled fan-shaped structure. FIG. 2 (a) Scanning Electron Micrograph (SEM) after 4.5h of reaction at 90 ℃; (b) The elemental analysis of FIG. 2 shows that C, N, O and Ag are uniformly distributed in the synthesized fan-shaped precursor.
2. A fan-shaped structure assembled by carbon-coated silver nanoparticles:
calcining the precursor as a template at 330 ℃ for 60min, and thermally decomposing the precursor of Ag to form a fan-shaped structure assembled by carbon-coated silver nanoparticles. Fig. 3 is an XRD (fig. 3 a), a scanning electron micrograph (fig. 3b and 3 c) and a TEM (fig. 3 d) of the product obtained by calcination. The XRD chart indicated that the resultant product was Ag, the scanning electron micrographs (fig. 3b and 3 c) indicated that the resultant product was a fan-like structure assembled with silver nanoparticles, and the TEM chart (fig. 3 d) indicated that there was a layer of amorphous structure on the outside and silver nanoparticles on the inside. FIG. 4 (a) shows that the hydrogen production amount of the Ag @ C catalyst at 10h irradiation is 449.6. Mu. Mol/g, and FIG. 4 (b) shows that the recombination of electrons and holes can be effectively suppressed by photogenerated carriers.
Claims (6)
1. A preparation method of a fan-shaped structure photocatalyst assembled by uniformly coating silver nanoparticles with carbon is characterized by comprising the following steps:
s1: dissolving silver nitrate in a mixed solution of deionized water and methanol to form a solution a;
dissolving benzimidazole in a mixed solution of deionized water and methanol to form a solution b;
dissolving melamine and polyvinylpyrrolidone in a mixed solution of deionized water and methanol to form a solution d;
s2: pouring the solution b into the solution a, and stirring to form a solution c; pouring the solution d into the solution c, and stirring to form a solution e;
s3: heating and stirring the solution e for a period of time, then centrifugally separating and collecting a product, and washing to obtain an Ag precursor;
s4: and calcining the precursor of Ag at high temperature for a period of time to obtain a fan-shaped structure assembled by the carbon-coated silver nanoparticles.
2. The preparation method according to claim 1, wherein the volume ratio of deionized water to methanol in the mixed solution of deionized water and methanol is 1:1.
3. the method according to claim 1, wherein in the step S2, the volume ratio of the solution b to the solution a is 1:1, the volume ratio of the solution c to the solution d is 2:1.
4. the preparation method according to claim 1, wherein the step S3 specifically comprises: and heating the solution e to 90 ℃, stirring for 4.5h, then collecting a product through centrifugal separation, and then washing the product for several times by using deionized water and industrial alcohol to obtain the precursor of the Ag with uniform size and morphology.
5. The method according to claim 1, wherein in the step S4, the high-temperature calcination temperature is 330 ℃ and the calcination time is 60min.
6. A photocatalyst having a fan-like structure assembled with uniform carbon-coated silver nanoparticles prepared by the method of any one of the preceding claims.
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